Manufacture of Alum PDF

THE LIBRARY
OF
THE UNIVERSITY
OF CALIFORNIA
LOS ANGELES
THE MANUFACTURE OF ALUM
AND THE SULPHATES AND
OTHER SALTS OF ALUMINA AND IRON

THE
MANUFACTURE OF ALUM
THEIR USES AND APPLICATIONS AS MORDANTS IN
DYEING AND CALICO PRINTING, AND THEIR OTHER
APPLICATIONS IN THE ARTS, MANUFACTURES, SANITARY
ENGINEERING, AGRICULTURE, AND HORTICULTURE
LUCIEN GESCHWIND
ie Publishers wish it to be distinctly understood that
i5 series of books is supplied on such terms as prohibit

their being sold below the published price.
WITH 195 ILLV
LONDON
SCOTT, GREENWOOD & CO.
19 LUDGATE HILL, E.C.
1901
[The sole right of publishing this work in English rests mth the above Firm.]
D. VAN NOSTRAND COMPANY.

NEW YORK.
THE
MANUFACTURE OF ALUM
THEIR USES AND APPLICATIONS AS MORDANTS IN
DYEING AND CALICO PRINTING, AND THEIR OTHER
APPLICATIONS IN THE ARTS, MANUFACTURES, SANITARY
ENGINEERING, AGRICULTURE, AND HORTICULTURE
LUCIEN GESCHWIND
TRANSLATED FROM THE FRENCH BY CHAS. SALTER
WITH 195 ILLUSTRATIONS
LONDON
SCOTT, GREENWOOD & CO.
19 LUDGATE HILL, E.G.
1901
[The sole right of publishing this work in English rests with the above Firm.]
D. VAN NQSTRAND COMPANY,

NEW YORK.
rr
INTRODUCTION
IN compiling the present work, the author has endeavoured to

somewhat scanty literary data available on the manu-
collect the
facture of the sulphates of alumina and iron, and- combine with

them the results of his own researches, in order to bring before
the reader a complete account of the processes involved in the
treatment of the raw materials employed, namely, bauxite, alunite,
pyritic lignites ;
and of the various applications of the resulting
products.
The work has been divided into four parts :
1. A Theoretical Study of Iron, Aluminium, and their Com-

pounds, chiefly confining the question to the sulphates and the
minerals employed in the operations described in the succeeding
parts of the book. This section, it is hoped, will save the chemist
and manufacturer the considerable trouble often encountered in
seeking for information on theoretical points connected with
practical procedure ; and, furthermore, simplifies the subsequent

sections, in so far as the reader is instructed beforehand in the
composition and origin of the minerals, the reactions employed,

and the characteristics (specific gravity, solubility, etc.) of the
substances used.
2. the Sulphates of Aluminium and Iron.
Manufacture of
Here be found a description of the various methods of manu-
will
facturing aluminium sulphate, the various alums, normal ferrous

and ferric sulphate, and the basic ferric sulphates, more especially
Rouil mordant. Wherever feasible, the costs of production have
been given in detail, and possible improvements in the methods
of manufacture have been suggested. A number of the illustra-
Vi INTRODUCTION
tions used are reduced from original drawings made on the spot,
or lent by the proprietors of the works described.

3. Applications of the Sulphates of Aluminium and Iron. In
this section an attempt has been made to go beyond a mere arid
recapitulation of the uses to which these bodies are put, and to
describe the mode of their employment, in order to save the
reader the trouble of further research.
4. The Analysis of the Iron and Aluminium Compounds: this
part containing, in addition to the usual tests, examples of the

methods of analysing the natural and industrial products, such as
bauxite, aluminium sulphate, aluminium hydroxide, etc.
The work is designed to meet the requirements of chemical
manufacturers, chemical engineers, works managers, and others
engaged in the various chemical industries producing or using

alum, aluminium sulphate, the sulphates of iron, etc.
The author wishes to express his thanks to the following
gentlemen, who have afforded great assistance in the fulfilment of
his task Messrs. Lacarriere (chemical manufacturer, Noyon),
Vivien (St. Quentin), Bernier (Chailvet), Gaillot (Laon Agri-
cultural Station), and Professor Hermant of the Institut Industriel
du Nord, their advice and inforrrfation having proved of great
utility.
L. GESCHWIND.
CONTENTS
PART I
THEORETICAL STUDY OF ALUMINIUM, IRON, AND COMPOUNDS OF

THESE METALS
CHAPTER I
SECS.
1.
2.
Aluminium
Compounds
.........
........
of
Aluminium Minerals
ALUMINIUM AND
Aluminium .
ITS
-
COMPOUNDS
. . . .
PAGE
.10
i
3. 42
CHAPTER II
1.
2.
Iron
Compounds
Iron Ores
..........
......
of Iron
IRON, AND IRON COMPOUNDS
59
.63
3. . . . . . . . .
115
PART II
MANUFACTURE OF ALUMINIUM SULPHATE AND SULPHATES OF IRON
CHAPTER III
MANUFACTURE OF ALUMINIUM SULPHATE AND THE ALUMS

1. Manufacture of Aluminium Sulphate . . . . .
.134
2. Alum Manufacture . . . . . . .
.163
CHAPTER IV
THE MANUFACTURE OF SULPHATES OF IRON
1. Ferrous Sulphate . .
Conjoint Manufacture of Ferrous Sulphate and

. .
Alum ....
. . .
.183
.....
2. 190
A. Treatment of Shales ... .190
.....
. . . .
. Treatment of Pyritic Lignites 193

3. Manufacture of Ordinary Ferric Sulphate 266
4. Manufacture of Basic Ferric Sulphate, or Rottil Mordant . . .
270
vii
viii CONTENTS
PART III
USES OF THE SULPHATES OF ALUMINIUM AND IRON
CHAPTER V
USES OF ALUMINIUM SULPHATE AND ALUMS
.....
SECS. 1-AGE
1. Application to the Art of Dyeing .

283
.
2. Employment in the Manufacture of Pigments 290

3. Various Applications of Aluminium Sulphates .
299
CHAPTER VI
USES AND APPLICATIONS OF FERROUS SULPHATE AND FERRIC SULPHATES

1. Uses of Ferrous Sulphate . . . . . .
.310
2. Applications of Ferric Sulphate . .
33 1
3. Applications of Mixtures of Iron and Aluminium Sulphates . . .
342
PART IV
CHEMICAL CHARACTERISTICS OF IRON AND ALUMINIUM. ANALYSIS OF
VARIOUS ALUMINOUS OR FERRUGINOUS PRODUCTS
CHAPTER VII
ALUMINIUM
1.
2.
Analysing Aluminium Products ......
Chemical Characteristics of the Aluminium Compounds . . .
352
357
CHAPTER VIII
1.
2.
Analytical Characteristics of Iron Salts
Analysis of certain Ferruginous Products
.....
IRON
..... 368
373
TABLE OF ILLUSTRATIONS
FIGS. PAGE
I and 2. The Netto aluminium
do.
process Furnace
Introducing sodium into the cryolite
for preparing
...
....
sodium . .
3
4
....
3.
........
4. do. Converter for producing aluminium 4
The Cowles aluminium process Electrical furnace
......
5. 6
End view
.......
6. do. 6
7. The Heroult aluminium process 7
8. The Minet aluminium process 8
Preparation of aluminium chloride
9. . . . . . .12
10 to 13. Octahedral crystals, various shapes . . . . .28
15.
1 6. Effect of heat
Block of alum
on alum ........
14. Octahedron modified by facets of cube and rhomboidal dodecahedron
.........
Diagram showing relations between cube, octahedron, and dodecahedron
....
.
.
30
31
32
17.
18 to 20. Topaz crystallised
..... . .
36
43
21 and 22. Corundum crystallised
23.
24.
Diaspore crystal
Cymophane ........
........
crystal
.
. . . .
-55
44
45
48
25. Andalusite crystal
26. Oligoclase crystal
27 and 28. Albite crystals

29. Orthose crystal (adular)
........
.......
. . . . . . .
57
57
58
30.
31 and 32. Orthose crystal (maclea)
33 to 35- Ferrous sulphate crystals, most
...
common forms
.58
.58
.92
.....
. . .
361038. Ferro-ferric oxide crystals . . . .

.115
39. Magnetite crystal .116
40. Oligistic iron (haematite) Primitive basal form .
.117
41. ,, ,, Primitive and rhombohedral . .
.117
42. ,, ,, From the Altenberg mines . . .
.117
43. Haematite (Framont) . . . . . . .
.117
44. ,, (St. Gothard) . . . . . .
.117
.117
......
45. ,, (Mont-Dore) . . . . . .
46. ,, II?
47- .
117
48. ,, (Elba) . .
.117
......
(Primitive, based
49. ,, by facets of the exquiaxial rhombohedron) .
117
50. Ilmenite crystal . . . . . . . .118
51. Gcethite crystal .119
52. Magnetic pyrites crystal . 120
53. Pyrrhotine crystal . . . . . . . .120
TABLE OF ILLUSTRATIONS
FIGS.
PAGE
54 to 57. Crystals of pyrites

58. Cubo-dodecahedral pyrites
.
.121
mine 121
59. Pyrites from a Cumberland
. . .
.
6oand6i.
62 to 64. White ...
Crystals of pyrites
pyrites
.
.122
122
65. Marcassite
66. Chalcopyrite
67. Vivianite
... ......
Grouping of crystals
.
known as
"
.
Crete de coq
"
(cockscomb) .
.123
123
124
68. Mispickel
69. Pharmacosiderite . . . .126
70 and 7 1. Spathic iron . .126
I2 7
72 to 74.
...
,,
7 5 and 76. Peridot . .128

77 to 83. Augite 129
....
.
84 to 86. Almandin garnet . .

13
87 to 89. Ilvaite
I
31
Achmite
....... 32
1
90 to 92. . . . .
93. Reverberatory evaporator used in aluminium sulphate manufacture Cross
94.
95.
do.
do.
section
Longitudinal section
Plan of hearth and bed
...
... .
.140
139
140
96. Lixiviation of crude aluminate .
142
97. Carbonating the aluminate .
143
. . .
98. Grinding mill . .146

.147
.....
Face of the millstones
99. . . . . . .
101. Collector ...

100. Mill for grinding and sifting bauxite
102 and 103. Rectangular vat in plan and longitudinal section

. . . .
.
. .148
.151
149
105. Concentrating the liquor

106. Cutting rake .........
104. Cylindro-conical vat, with automatic air-blast agitator
.
.
.
.
.152
.
155
155
......
107. Pulveriser Cross section . . . . . . . 1
56
108. Pulveriser for
109.
no. Hopper
Blade of pulveriser
.........
aluminium sulphate
111. Reverberatory furnace for roasting alunite

. . .
. .
.
.157
.
.176
157
158
....... Transverse
112. ,, ,, ,, ,, ,, . .
176
114. Preparing the mineral

115. Firing the
1
heap ........
113. Section of the strata at Chail vet (Aisne)
....
16. General plan of works for treating pyritic lignite
. . . .
.199
202
202
206
117 to 121. Plan and sections of lixiviation plant
117.
llSand
Plan . .
119. Transverse sections

.
...... . . . . .208
209
......
1 20. . . . .
.
. . .
209
121. General plan showing arrangement of lixiviation tanks, channels,
reservoirs, and tramways 209
122 and 123. Plan and section of the reduction plant . . .
.214
124. Reverberatory evaporating furnace for the reduced liquor . .
.215
125. Double-bed evaporating furnace . . . .
.215
126 to 129. Leaden evaporating pan used at Chailvet
126. View from above showing appearance of the bottom of the 216
pan .
127 and 128. Plan and section showing details of the firegrates and flues .
217
129. Longitudinal section of above . . . . . .218
130. Leaden evaporating pans Continuous system (Chailvet) . . .218
TABLE OF ILLUSTRATIONS XI
FIGS. PAGE
131 and 132. Plan and section of a dressed-stone crystallising vat 220
....
. . .
133 and 134. Details of wooden pump . . . . ... 221
......
135. Longitudinal section of the washing tank (turbine) 222
136. Transverse section of the washing tank (turbine) 222
..".....
. . .
137. Plan of the washing tank (turbine) 223
......
138. Re-crystallising vat Plan 224
139. ,, ,, ...
Longitudinal section . . .
224
140. ,, ,, Cross section 225
Showing the arrangement of the rods destined to serve
141.
142. Mould
,, ,,
(a) collected .....

....
as nuclei for the crystallisation
on distillery waste
. . .
225
226
......
143. ,, (b) formed on re-crystallisation liquor . 226
144. ,, (c) laboratory culture obtained by inoculating (d) on same liquor with
addition of sugar 226
145. ,,
Alum .....
(d) preparation obtained by sowing (b) on gelatinised meat broth .
.231
226
146.
147.
148.
,,
,,
recovery tank Plan
,,
,,
Alum washing and draining tank

......
Cross section
.
.231
232
149.
..... 237
. . . .
150. Alum re-crystallising plant . . .

238
151. ,, ,, Plan of the vat 238
.....
152. Copper syphon . .
239
153. Copper vat with underneath fire . . .
239
Large alum tank Plan 240
....
154. .
I54A. ,, ,, Section . . . . . .
.241
alum to the tank
.....
155. Apparatus for introducing the 241
156. Block
157.
158. Alum
Wicker
mould for alum
Block of alum cut open
mill .........
.....
.....
sieve for drying purified alum
to show
. .
interior
. . . .
.241
242
244
159.
1 60.
161.
162.
Front view of pouring spout of the above
Blowpipe for autogene soldering
.....
Cast-iron pot for melting lead for the plant
.... .
245
248
248
249
...
163. Leaden hydrogen generator for the autogene soldering process . .
249
......
164. Bellows for the autogene soldering process 250
.
165 and 166. Soldered lapped butt joint in leaden sheets . . .

251
167 and 168. Butt joint .
251
169.Scraper for brightening the parts to be soldered . .
252
17010172. Soldering a vertical joint . . .
252
173. Jointing two horizontal pipes . . . .
253
174. Fitting a leaden pipe to a vertical wall, accessible on the rear face
...... 253
. .
175. ,, ,, ,, inaccessible from the back . .

253
176. Bolted loose-flange joint for pipes 254
177. Hot extraction Diagram of a unit of an extraction battery . .
264
178. Manufacture of ferric sulphate (Rohart process)
1
180.
79. Rouil mordant process
,, ,,
Peroxidation vat
Recuperation of the nitrous products
... . .
.
.
267
272
274
181. ,, ,, Recuperation carboys . .
276
182. ,, Treatment of sediment Section of boiling pan .
279
183. ,, ,, ,, ,, ,,
280
184. ,, ,, Section through boiling pan and fireplace 280
185. Indigo dyeing Ferrous sulphate vat . . . . . 3 11
form 3J8
.....
186. Laming purifier for lighting gas Original . . .
187. ,, ,, Present form . . .

3 l8
188. Distributor bell for a set of Laming purifiers 319
Xll TABLE OF ILLUSTRATIONS
FIGS. PAGE
189.
190.
191.
Spraying engine
Mordanting silk
...
Portable spraying apparatus for ferrous sulphate
... ....
. .
.
.
.
326
327
332
192. Washer employed for silk . . .
333
193.
........
Gallery furnaces for the manufacture of Nordhausen sulphuric acid
194. Purification of waste waters
decantation basins
. .
Plan of a series of isolated and independent
......
195. Vertical section of decantation basin
342
346
348
PART I
THEORETICAL STUDY OF ALUMINIUM, IRON, AND

COMPOUNDS OF THESE METALS
CHAPTER I
ALUMINIUM AND ITS COMPOUNDS
I. ALUMINIUM (Al = 27)
i. Preparation in the Laboratory. HISTORICAL. Aluminium

may be prepared in a perfectly pure state in the laboratory by
reacting on purified aluminium bromide with sodium in a

brasqued crucible. Another method is by heating alumina
in presence of borax, carbon, and a little silica, the alumina being
reduced to the metallic state.
The discovery of this metal is generally ascribed to Wohler,
thisrenowned chemist having prepared it, in 1827, as an impure
grey powder, by decomposing aluminium chloride with potassium.
Various ancient authors, however, Petronius Arbiter (Satyricon^
chap, Dio Cassius (R.R., lib. Ivii. c. xxi.), Pliny (Hist, naturalis^
li.),
1. xxxvi. c. Ixvi. 195), mention a workman who discovered a

method of separating from aluminous glass a new metal out of
which he fashioned a cup which he presented to the Emperor
Tiberius. In view of the well-known abundance of boric acid
springs in Italy, it is not impossible that the method consisted in

the employment of boric acid, potash, silica, and carbon, aluminium
being formed as mentioned above.
2 THEORETICAL STUDY OF ALUMINIUM, IRON,
The discovery of aluminium would thus appear to date back
to a much earlier period than is generally believed. (See paper
by Duboin, Rev. gtn. des Sciences, Vol. 9, No. 16, p. 635.) The
credit of having isolated the metal in a pure state and described
its properties belongs to H. St. Claire
Deville (1854) ; and, not
satisfied with this result, the same chemist, after experimenting
largely in collaboration with H. Debray and P. Morin, very

soon afterwards founded the first industrial process for the manu-
facture of aluminium, at the works of Messrs. Rousseau freres at
La Glaciere.
This process, which at the present time is merely of historical

interest, consisted in allowing slightly heated sodium to react on
the vapour of aluminium chloride. Owing to the numerous
difficulties encountered, the inventors had to modify their original
plan b.y replacing the highly deliquescent aluminium chloride by
the double chloride of aluminium and sodium. A fluoride was
afterwards added to serve as a flux, the following proportions
being taken :
Sodium-aluminium chloride
Common salt ... .
....
. . . .
400 grams.
200 ,,
Cryolite 200 ,,
Sodium 75
This mixture, fused at a high temperature in a crucible provided

with an aluminous brasque, yielded aluminium of fairly good
quality.
2. Preparation of Aluminium on a manufacturing scale.
A. CHEMICAL METHODS. At the present time the metallurgy

of aluminium comprises two principal divisions : chemical and
electrical methods. The former includes several processes, all
more or less derived from the classic method of St. Claire

Deville, the most important being
The Castner process, worked at Oldbury, near Birmingham ;
The Netto process, worked by " The Alliance Aluminium

Co." at Wallsend-on-Tyne, near Newcastle ;
The Grabau process.

I. The Castner process. The of this
principal advantages
manner of preparing the sodium. Instead
process reside in the
of employing sodium
carbonate, which requires a very high
AND COMPOUNDS OF THESE METALS 3
temperature for itsdecomposition, caustic soda is used, this body

decomposing at about 800 C, according to the equation
6NaOH + C = 2Na CO + 3H + Na 2 2 3 2 2.
The carbon is introduced in the form of specially prepared iron

carbide.
The double chloride is obtained by treating with chlorine a
mixture of alumina, common salt, and carbon in horizontal
retorts about i 2 feet long, heated by gas. The double chloride
FIGS, i and 2. The Netto process.
A, Caustic soda reservoir tap for emptying same ; e, funnel inlet for caustic soda ;
; r,
c, cover ; C, reducing furnace ; /, stopper, worked by wheel v ; i, clay jacket ; d,

condenser for metallic sodium ; h, oil reservoir ; D, storage for residual Na2 CO3 ;
b, effluent pipe ; , tuyeres ; in, n, o, p, q, flues.
is mixed with
cryolite and the necessary quantity of sodium in a
revolving cylinder, the whole being then rapidly transferred to a

reverberatory gas furnace heated to the requisite degree for the
performance of the reaction.
The quantities employed for a charge are : 1210 Ibs. of double
chloride, purified by fusion with a little powdered aluminium or

sodium ; 605 Ibs. of cryolite, and 149*6 Ibs. of sodium.
A fairly pure metallic aluminium is obtained.
II. The Netto process. In this case the raw material consists
THEORETICAL STUDY OF ALUMINIUM, IRON,
of the double fluoride (cryolite) of aluminium and sodium, instead

of the double chloride of these metals. In preparing the cryolite
the inventor utilises the scoria resulting from the treatment of
this salt with sodium, and consisting mainly of sodium fluoride.
With this object he fuses the said residue with aluminium
sulphate, and extracts sodium sulphate from the mass by lixivi-

ation, leaving the insoluble double fluoride behind. The reaction
is expressed by the equation
A1 2 (S0 4) 3 + 1 2NaF = A1 2 F 6 6NaF + 3Na 2 SO 4
,
.
Is-?
f
FIG. 3. Introducing the FIG. Converter for producing aluminium
4.
by the
sodium into the cryo- action of sodium on cryolite.
lite.
A, Reducing crucible a, charging aperture
; ; B, heat-
A, Crucible ; B, block of ing flue ; g, pipe from gas furnace ; /, air inlet ; P,
sodium suspended from
driving pulley ; e, outlet.
the rod / ; d, perforated
plug.
The natural Greenland cryolite could of course be

used, were
itnot rendered too
expensive by the high rates of freight and
by the monopoly established by the American owners of the
deposits.
The object of the Netto method of
preparing the sodium is
to reduce to a minimum the
formation of sodium carbonate, to
carry out the reaction at a temperature low
enough to permit the
use of cast-iron retorts, and to separate immediately the sodium

and sodium carbonate formed.
Forthis purpose the caustic soda is fed gradually to the
glowing carbon the resulting vapour of sodium escapes as soon

;
as formed and condenses in a lateral pipe situated at the top of

the retort, whilst the sodium carbonate runs away uninterruptedly
at the bottom (Figs, i and 2).
The operation is conducted at a bright red heat. One of
the conditions essential to the success of the sodium treatment
has been elucidated by Netto and Grabau, and that is, not to
leave the sodium in contact with the cryolite any longer than is
absolutely necessary. The arrangement employed by Netto is
designed with a view to effect the immediate reaction of the

sodium on the double fluoride.
The cryolite and the necessary amount of sodium chloride
are fused at red heat in a refractory crucible. As soon as the
mass is in a molten condition a block of sodium is introduced by
means of a plug and a rod (Fig. 3), on which it has previously
been moulded, whereupon the reaction is almost instantaneous.
The apparatus is then tipped so as to discharge the contents into
a cast-iron mould, from which, when cold, the aluminium is taken
out as a solid block. The operation may also be performed in
an apparatus analogous to the Bessemer converter (Fig. 4). The
aluminium obtained is of a high degree of purity.
III. The Grabau process. In this method metallic sodium
is employed to reduce aluminium fluoride, the two being heated
separately in order to obviate the great inconvenience arising
from the corrosion of the vessels by fluorides. The aluminium
fluoride, which is infusible at the temperature of the operation,
is reduced to powder, and in this condition is brought into
contact with the sodium. The reaction is expressed by the
equation
2 A1 2 F 6 + 6Na = 2 Al + A1 2 F 6 , 6NaF,
the cryolite, produced as a residue, tending to solidify on the
walls of the crucible and protect them against the action of the
mass.
Grabau prepares his aluminium fluoride by reacting with
fluor spar on aluminium sulphate, the products being aluminium

fluosilicate and calcium sulphate, according to the equation
A1 2 (S0 4) 3 + 2CaF 2 = A1 2 F 4 SO 4 + 2CaSO 4 .
The fluosilicate is then treated with cryolite
3 A1 2 F 4 S0 4 + A1 2 F6 6NaF = 4A1 2 F 6 + 3Na2 SO 4

,
.
B. ELECTRICAL METHODS. I. The Cowles process. A

mixture of alumina and carbon, with the metal destined to form
FIG. 5. Cowles process. Apparatus employed at the Milton Works.
an alloy with the aluminium, is introduced into an apparatus
arranged in a similar manner to the Siemens crucible (Figs. 5

and 6). Under the influence of a powerful electric current the
carbon reduces the alumina and liberates aluminium, which
immediately forms an alloy with the

metal introduced for that purpose. It
would appear that the thermal effect
of the current alone comes into play
in this process, and a trial made with
an alternating current machine gave
the same yield of aluminium, in the
FIG. 6. Cowles process. End
condition of bronze, as was obtained
view of the apparatus.
by a continuous current.
This process is employed by the " Cowles
Syndicate," whose
works are at Milton near Stoke-on-Trent it is
only suitable for ;
the production of alloys.

II. The He'roult process. This process, which is analogous to
that of Cowles, is worked at Neuhausen near Schaffausen, and at
Froges (Isere). The material employed is either bauxite, free
from silica and iron, or else pure alumina.
The apparatus for treating this material consists of a crucible
AND COMPOUNDS OF THESE METALS
of pressed carbon clamped by iron plates (Fig. 7). It would

appear that the first stage is the fusion of the alumina by the
electric arc, the fused mineral then undergoing electrolysis. The
bottom of the bath is formed by the metal to be alloyed, which
acts as the negative pole. A description of the process is given
by the inventor in a supplement (dated April 15, 1887) to his
original patent of April 23, 1 886, which relates to the electrolysis

of alumina dissolved in molten cryolite.
III. Tlie Minet process. The bath is composed of 70 parts of
sodium chloride and 30 parts of the double silicate of aluminium
and sodium. For a- current of 4000 amperes the weight of the
charge amounts to about
176 Ibs., and a tempera-
ture of about 800 is
high enough to keep the

bath in a sufficiently
liquid state for the normal

conduct of the electro-
lysis.
The apparatus (Fig.
8) is composed of a
parallelepiped metallic
vat, the sides of which

measure 12 to 20 inches
in length according to
FIG. 7. Heroult process.
the intensity of current
employed. In order to enable the vat to resist the action of the

molten fluoride, connection is established between the walls and
the negative electrode by means of a resistance which allows
only fjhr of the current to pass. By this means the sides are
kept covered by a thin deposit of aluminium, which acts as a
protective layer.
electrodes are made of compressed carbon, and imme-
The
diately below the cathode a small crucible is placed to collect
the metal produced. When the current is passed the aluminium
fluoride is decomposed, aluminium collecting at the negative pole,
whilst at the same time an equivalent amount of fluorine is
liberated at the positive pole. The bath is renewed, as decom-

a mixture of alumina and aluminium
position proceeds, by
the liberated
fluoride and the alumina seizes upon a portion of
;
fluorine to form aluminium fluoride,

which thus regenerates the
electrolyte.
The output by this process is 25 grams per
of aluminium
electrical horsepower hour, the cost of the motive power consumed
in I Ib. of the metal being

about 2d.
producing
Properties of Aluminium.
3.
PHYSICAL PROPERTIES. A
in
Aluminium is a dull white metal exhibiting a slight blue tinge
Its sp. gr.
comparison with silver ;
it readily takes a fine polish.
varies between 2-50 and 270,
according to whether it has been
cast or rolled. The specific heat
is 0*2253; fusing point about

600 C; and the metal is capable
of retaining gases by occlusion.
When newly cast, aluminium

is of equal hardness to virgin
silver, but this quality is greatly

increased by rolling, which treat-
ment also imparts elasticity. In
point of malleability the metal is
FIG. 8. The Minet process. comparable with gold and silver,

B, vat ; A, anode ; C, cathode ; R, and in tenacity it occupies a
resistance coil ; D, collecting crucible.
position between zinc and tin,
or, when rolled, is equal in this respect to rolled copper.
Aluminium easy to stamp, and can be forged without
is
difficulty both cold and hot; it is, moreover, highly sonorous.

Its atomic weight is 27, and it is regarded as a trivalent metal.
B. CHEMICAL PROPERTIES. Aluminium must be looked
upon as one of the most unalterable metals. It is unacted upon
by whether moist or dry, and undergoes no change when
air,
fused in the open air, though when heated in a blast furnace it

becomes covered with a thin layer of oxide. When it contains
silicon the metal burns freely. It is readily soluble in hydro-
chloric acid or caustic alkalis, but offers considerable resistance to
and organic acids. Sulphur will

the action of nitric, sulphuric,
not attack aluminium except at very high temperatures and ;
when extraneous metals, such as iron, copper, etc., are present,

these latter become converted into sulphides at temperatures
whereat aluminium does not undergo any change.

It combines readily with chlorine, bromine, and iodine under
the influence of heat, and forms crystalline compounds with boron

and silicon. Carbon, nitrogen, phosphorus, and arsenic have no
effect upon it. With the majority of other metals aluminium
forms interesting alloys.
Water is not decomposed by aluminium, even when the metal
is heated
nearly to the point of fusion.
Aluminium decomposes a very large number of metallic
compounds in solution, by displacing and liberating the metal,

the reaction being greatly facilitated by rendering the solution
alkaline or ammoniacal.
Even in a molten state aluminium is unattacked by potas-
sium nitrate, which, on used for refining the metal.
this account, is
The physical and chemical properties are considerably modi-

fied by the presence of impurities, such as silicon, sodium, etc.
4. Uses of Aluminium. Aluminium is employed for purify-
ing other metals, most of the large steel works in France and
Germany using pure aluminium for this purpose, whilst in
England and the United States ferro - aluminium is utilised
instead.
The resistance offered by this metal to oxidation, and its
general properties, recommend it as a material for cooking

utensils ;
numerous trials have been made, and are in progress,
with reference to its use for military bottles, pannikins, harness
fittings, etc.
Other applications for this metal are the manufacture of keys,

optical, surgical, and physical appliances its sonority renders it
;
suitable for musical instruments and bells, and its lightness for
the metallic fittings of balloons. Aluminium is also employed in
the form of sheet metal in marine construction, and it is likewise

used for making bicycles. The already extensive utility of this
metal will be increased in proportion as improved methods of
IO THEORETICAL STUDY OF ALUMINIUM, IRON,
production enable it to be obtained in a pure state and at low
cost, and its alloys are at present very largely employed.
2. COMPOUNDS OF ALUMINIUM
5. Aluminium Fluorides. A. ANHYDROUS ALUMINIUM

FLUORIDE (A1 2 F6 ). This compound may be prepared by treating
calcined alumina with hydrofluoric acid in excess, the product
being dried and distilled in a tubular carbon retort through which

a current of hydrogen is passed (H. St. Claire Deville).
Another method is by fusing, together a mixture of anhydrous
aluminium sulphate and cryolite, the resulting sodium sulphate
and insoluble aluminium fluoride being separated by lixiviation.
Grabau treats cryolite with a solution of aluminium sulphate,
evaporating the mass to dryness and taking up the residue with
water.
Brunner has shown that this salt may also be obtained by
passing a current of gaseous hydrofluoric acid over alumina heated
to redness in a platinum crucible.
/
Aluminium fluoride crystallises in rhombohedra (88 3O ),
which
are colourless, of low refraction, and frequently grouped into large
agglomerations. These crystals are insoluble in acids, even in
boiling sulphuric acid. Caustic potash solution scarcely affects

them at all, and the only means of attack is by sodium carbonate
at a red heat. When fused with boric acid they furnish crystallised
aluminium borate.
B. HYDRATED ALUMINIUM FLUORIDE (A1 2 F 6 7H 2 O). ,
This prepared by the action of dilute hydrofluosilicic acid on

is
calcined alumina or kaolin. According to St. Claire Deville, a

soluble aluminium silicate (3SiF 4 ,
A1 2 F 6) is first formed, but, on
prolonging the digestion with alumina, silica is deposited and a
neutral liquor containing the salt A1 F 7H
2 6 , 2 O is left behind.
This hydrated fluoride is soluble, and is readily attacked by
acids.
C. FLUO-ALUMINIC ACIDS. Dilute hydrofluosilicic acid is
allowed to react on calcined alumina, care

being taken to preserve
the liquid in a strongly acid state until the
operation is completed.
AND COMPOUNDS OF THESE METALS I I
Strong alcohol being then added, an oily precipitate is formed,

which quickly solidifies and crystallises.
This product is a fluo-aluminic acid, having the formula 3 A1 2 F 6 ,
4 HF, ioH 2 O.
If, instead of treating it with alcohol, the acid liquid is
evaporated, hydrofluoric acid will be liberated, leaving a crystalline

mass which, when washed with boiling water and dried, exhibits
the composition A1 2 F 6 , HF, 5H 2 O.
The existence of these two fluo-aluminic acids, and the great
difference between the anhydrous and the hydrated fluoride, led
St. Claire Deville to consider cryolite (A1 2 F 6 6NaF) as
,
derived from
an undiscovered fluo-aluminic acid, A1 2 F 6 6HF, by
,
the substitu-
tion ofan equivalent quantity of sodium for the hydrogen. The
hydrated aluminium fluoride would then be simply a fluo-aluminate
of aluminium
A1 2 F6 A1 2 F 6
, + i
4 H2 = 2(A1 2 F 6 , ;H 2 O),
the 6 atoms of hydrogen in A1 2 F6 6HF
being replaced by 2,
,
atoms of aluminium. This would accord with what is known as

to the trivalence of the metal.
The fluo-aluminic acids, free from silica, may be volatilised
completely, yielding anhydrous aluminium fluoride, water, and

hydrofluoric acid.
D. DOUBLE FLUORIDE OF ALUMINIUM AND SODIUM
(CRYOLITE) (A1 2 F6 6NaF). This double salt may be prepared
,
by treating a mixture of alumina and sodium carbonate, in suit-

able proportions, with hydrofluoric acid, the liquid being evaporated
and the excess of acid driven off from the residue by calcination.
Another method is to partially saturate a solution of hydro-
fluoric acid with alumina and then add sufficient sodium chloride
to furnish 6 atoms of sodium per 2 atoms of aluminium, where-
upon cryolite is precipitated.
This remarkable compound is met with in nature, the most
important deposits being found on the coast of Greenland. Since
1855 it has been utilised in Denmark and Prussia, under the name
of mineral soda, for soap-making, by treating the finely powdered
mineral with boiling milk of lime, which precipitates calcium
fluoride and leaves in solution an aluminate of sodium with an
excess of caustic soda. Soaps made with this aluminate retain a
very high percentage of water.

At the present time cryolite is used in the manufacture of
aluminium, and as a flux.
6. Aluminium Chlorides. A ANHYDROUS ALUMINIUM

CHLORIDE (A1 2 C1 6 ).
This chloride
prepared by intimately
is
mixing i oo parts of calcined alumina with 40 parts of lampblack

and enough oil to make a stiff paste, the whole being calcined in
a covered crucible at a bright red heat. The resulting solid mass
is broken small pieces, which are placed in a tubulated retort
in
fitted with a porcelain tube reaching to the bottom. The retort

being set in a reverberatory furnace, the porcelain tube is con-
FlG. 9. Preparation of aluminium chloride.
nected with a chlorine generator ;

and in the neck of the retort is
fitted the stem of a funnel, in the bowl of which is luted a gas jar
provided with a delivery tube (Fig. 9).

On heating the retort to redness and passing a current of
chlorine, the aluminium chloride formed distils over and condenses
in thegas jar in the form of a crystalline incrustation, which can
be detached when the operation is completed.
For the preparation of this salt on an industrial scale -St.
Claire Deville replaced the above mixture by alumina and tar,
and employed a gas retort set vertically inan enclosure traversed
by the flame from a furnace, a brick-work condensing chamber
being substituted for the gas jar.
Crude aluminium chloride is
generally yellow in colour, owing
to the presence of the sulphides of chlorine and iron. To purify

the salt the above-named chemist proposed a method of sublima-
tion over metallic iron, the ferric chloride being thereby reduced
to non-volatile ferrous the sulphur chloride is

chloride, whilst
converted into sulphur and ferrous chloride.

Dumas proposed a second sublimation over finely divided
aluminium.
The best results are obtained by the following process, devised
by Weber :
Aluminium chloride and powdered aluminium are introduced

into a tube closed at one end and bent into the shape of a U.
The other end being sealed in the lamp, heat is applied, the
chloride fuses under the pressure of its own vapour and gradually
becomes decolorised in contact with the metal ;
it can then easily
be sublimed into the second branch of the tube. The chloride
purified in this manner takes the form of a colourless transparent
mass composed of hexagonal prisms. Under ordinary atmo-

spheric pressure it readily sublimes without fusing. Nevertheless,
when heated rapidly in large bulk it can be fused and even
raised to ebullition. It fuses rapidly under pressure.
The actual fusing point is between 186 and 190. Towards
400 C. the vapour density very near 9*20, but diminishes to
is
4'6 at about 800. The heat of combination is A1 2 C1 6 = 32 1-96

cal. ;
the heat of solution is Al 2 Cl 6 Aq = 153-69 cal.
Aluminium chloride is a highly deliquescent salt, which com-

bines directly with phosphorus pentachloride to form a compound
with the formula 2PC1 5 A1 2 C1 6 a white mass capable of sublima-
, ,
tion and fusing to a brown mass which boils at about 400.

With phosphorus oxychloride it forms a double salt, A1 2 C1 6 ,
2PO.C1 3 which,
,
an excess of the oxychloride, crystallises in
in
colourless needles which fuse at 165 and volatilise without

decomposition. It is broken up by the action of water.
Aluminium chloride absorbs sulphuretted hydrogen and
furnishes small transparent crystalline lamellae which are in-
stantaneously destroyed by water, H 2 S being disengaged.

When sublimed in a current of phosphuretted hydrogen,
aluminium chloride yields a crystalline product, 3A1 2 C1 6 + 2PH 3 .
Aluminium chloride readily absorbs dry ammonia gas,
sufficientheat being evolved to liquefy the compound, which
corresponds to the formula A1 2 C1 6 3

When distilled in ,
6NH .
hydrogen this product gives off ammonia and becomes converted

into Al 2 Cl a ,
2NH 3.
Sulphur dioxide combines slowly with aluminium

chloride
at the ordinary temperature, and more rapidly towards 50 C.,
furnishing a compound, A1C1 2 ,

SO 2 C1.
In the laboratory, aluminium chloride is largely employed

for synthetical experiments in organic chemistry (Friedel and
Crafts' method).
B. HYDRATED ALUMINIUM CHLORIDE (A1 2 C1 6 i2H 2 O). ,
This salt may be prepared from aluminium sulphate and barium

chloride by double decomposition. The anhydrous chloride
dissolves in water, with evolution of considerable heat, and the
solution, on cooling, deposits crystals in the form of hexagonal
prisms terminating in a rhombohedron (about 138). The

formula is A1 2 C1 6 ,
I2H 2 O. The same result is obtained by
Crystals of better shape are

crystallisation in hydrochloric acid.
produced by heating aluminium hydroxide with concentrated

hydrochloric acid in a sealed tube.
The following table gives the density of various solutions of
aluminium chloride at I
5 C. :
The sp. gr. of the saturated solution (41-13 per cent.) is 1*3536.
These solutions cannot be
evaporated to complete dryness,
because the hydrated chloride is then decomposed, water
and hydrochloric acid being disengaged and aluminium de-
posited. When exposed in vacua over concentrated sulphuric
acid the crystallised hydrated chloride does not part with even a
trace of its water of crystallisation.
C. DOUBLE CHLORIDES OF ALUMINIUM. Aluminium chloride
combines with alkali chlorides to form veritable chlorinated
spinelles, having the general formula 2R.C1, A1 2 C1 6 . These pro-

ducts fuse at about 200 C., and are volatile at red heat ;
when
dissolved in water they furnish a mixture of the two salts, crystal-
lising separately.
The most important of these double chlorides is that of
aluminium and sodium, which is prepared by passing a current of
chlorine through a mixture of alumina and carbon with an addition
of common salt.
It a colourless, crystalline substance, fusing at about 185

is
and volatilising at red heat, and is very hygroscopic, though less

so than aluminium chloride.
D. BASIC CHLORIDES. Liechti and Suida have prepared
solutions corresponding to the following salts :
A1 2 C1 6 ,
A1 2 C15 (OH),
A1 2 C1 4 (OH) 2 ,
A1 2 C1 3 (OH) 3 ,
A1 2 C1 2 (OH) 4 ,
though they did not succeed in isolating any of them. The

solutions are decomposed by heat or by dilution with water.
7. Aluminium Bromide (Al 2 Br6) may be prepared by slowly
pouring bromine over finely divided aluminium, sufficient heat
being evolved during combination to raise the aluminium to
incandescence.
The best method of preparation, however, is by passing
bromine vapour over aluminium in a glass tube heated to
incipient redness. The product, which may be purified by pass-
ing its vapour over aluminium, is colourless, and crystallises in
the form of small brilliant flakes. to a limpid It fuses at 93
mobile liquid boiling at 260; the density in the solid state is
2-54; vapour density, i8'62 (Deville and Troost) heat of forma- ;
tion, Al 2 Br6 = 239-44 cal. ;

heat of solution, Al 2 .Br6 = 170*60 cal.
It is very hygroscopic.
1 6 THEORETICAL STUDY OF ALUMINIUM, IRON,
8. Aluminium Iodide (A1 2 I 6 ). Given a sufficiently high tem-

perature, iodine and aluminium combine directly, with evolution
of sufficient heat to raise the mass to incandescence. The usual
method of preparation is by passing iodine vapour over red-hot
aluminium, the product being purified in the same manner as for
the bromide.
The resulting compound is a colourless solid, crystallisable
by fusion. It melts at 125 and boils at 350, but can only be

distilled in an atmosphere of inert gas, since above
this tempera-
ture explodes when mixed with air, and furnishes alumina

it
and iodine. The double iodide A1 2 I 6 2KI fuses readily, and ,
may be heated much above the fusing point of aluminium iodide

without undergoing any change.
According to Berthelot, the heat of formation of this com-

pound is A1 2 I 6 = 140^7 8 cal., and the heat of solution, A1,I C Aq.
,
= 178 cal. The density in the solid state is 2-63, and the
vapour density at 440 is 27, the theoretical density for A1 2 I 6 =
2 vols., being 28'3. The difference between these last two values
is attributed by Deville and Troost to the instability of this
iodide, which becomes partially decomposed at the temperature

of the experiment.
Aluminium iodide is soluble, at the ordinary temperature,
in 3 times its own weight of carbon disulphide ;
it is also
soluble in alcohol and ether, is deliquescent, and dissolves in
water with evolution of heat.

9. Alumina. A. ALUMINIUM SESQUIOXIDE, or ALUMINA
(A1 2 O 3), is obtained on dehydrating the hydroxide by heat, or
by subjecting ammonium alum to strong calcination.

Pure alumina is a light, white powder, devoid of odour or
flavour ; hygrometric, adherent to the tongue, and very refractory.
In the oxyhydrogen furnace it yields a
very fluid globule, which
on cooling re-crystallises to an extremely hard mass capable of
cutting glass. The heat of formation from its elements is A1 2 O 3
= 196-3 cal.
Calcined alumina is
totally insoluble in water, but if not
heated above dark redness it
capable of re-hydration, heat
is
being evolved. When calcined and re-cooled in a moist

atmosphere it will absorb and tenaciously retain up to 15 per

cent, of its own weight of water.
Its solubility in acids varies with the method of preparation
employed. If calcined very strongly it becomes very slightly

soluble, even in hot concentrated acids. Alkaline solutions also
dissolve it with great difficulty, but it
may be easily converted
into a soluble aluminate with caustic potash or
by calcination
soda (or even with an alkali carbonate) in a silver crucible.
B, ALUMINIUM HYDROXIDE (A1 2 O 3 , sH 2 O). I.
Ordinary
Hydrate. The heat of formation from its elements A1 2 .O 3 3H Q O
,
= I97'8 cal.
The voluminous, gelatinous precipitate obtained on treating

a soluble salt of aluminium by ammonia is readily soluble in
dilute acids and alkalis, and when dried at 100 C. exhibits
the composition A1 2 O 3 , 3H 2 O.
A much denser form of the same hydrate can be prepared,
as a granular precipitate free from iron,
by passing a current of
carbon dioxide through a cold dilute solution of sodium alu-
minate. The hydrate thus obtained is insoluble in acetic acid.
If the precipitate formed by ammonia be boiled for some time
in water it undergoes dehydration and is converted into A1 2 O 3 ,
2H 2 O, which, like calcined alumina, is insoluble in weak acids

and dilute alkalis.
Aluminium hydrate possesses great affinity for organic sub-

stances, a property which accounts for its extensive use in dyeing.
II. Soluble Alumina. Successful attempts have been made

to obtain alumina Walter Crum prepared it
in the soluble form.
by heating a dilute solution of aluminium bi-acetate in a closed
vessel, for ten days and nights, in boiling water.

On then boiling the solution for an hour or two, and re-
placing the water lost by evaporation, all the acetic acid is
driven off and there remains a transparent, insipid solution of

soluble alumina, which becomes gummy when concentrated, and
coagulates to a firm jelly on the addition of a small quantity

of alkali or acid. When evaporated on the water bath it
yields
the hydroxide A1 2 O 3 2H, 2
O.
Soluble alumina was also obtained by Graham by dialysing
1 8 THEORETICAL STUDY OF ALUMINIUM, IRON,
aluminium chloride containing an excess of alumina in solution ;
"
prepared by Crum does not
"
but whereas the metalumina
act as a mordant, the product obtained by Graham possesses
mordanting properties.
For the rest, both varieties are coagulated to a firm jelly
or various salts, a property
by small quantities of acids, alkalis,
utilised in bacteriology for the preparation of certain special
culture media.
C. OCCURRENCE IN NATURE. PREPARATION OF CRYSTAL-
LINE ALUMINA. Alumina in a pure state is somewhat rare in
nature. In the condition of colourless crystals it forms

corundum ;
and when crystalline and coloured by various
oxides it is known under the names of ruby, oriental topaz,
oriental sapphire, amethyst, etc.; whilst, in admixture with ferric
oxide, alumina constitutes emery.

Several natural hydroxides are known. Gibbsite, A1 2 O 3 ,
3H 2 O,corresponds to the ordinary hydrate; diaspore exhibits

the formula A1 2 O 3 H 2 O. Bauxite, another natural hydroxide
,
of variable composition, but approximating most nearly to A1 2 O 3 ,
2H 2 O, is Important deposits are met

particularly abundant.
with in France, particularly near Tarascon.
Corundum was first artificially prepared by Ebelmen, by
heating a mixture of alumina and sodium borate in a porcelain
furnace, the alumina crystallising in proportion as the sodium

borate is volatilised. By the addition of a little chromic oxide
to the mixture, ruby is obtained.
Corundum was also prepared by St. Claire Deville and Caron,
by heating, in a carbon crucible, a fluoride above which is placed
a small platinum crucible containing boric acid. At a high
temperature the fluoride reacts on the boric acid, forming boron
fluorideand a crystallised oxide, which may be coloured by the
addition of some pigmentary oxide.
De Senarmont has obtained a mixture of corundum and dia-
spore by strongly heating a dilute solution of aluminium chloride.

10. Aluminates. Alumina will combine with alkalis, baryta,
etc., to form soluble products, whilst lime yields an insoluble
product. These bodies constitute the aluminates.

A fairly large number of natural aluminates are known,

viz., the spinelle ruby (magnesium aluminate) ; gahnite (zinc
aluminate) ; hercytine (iron aluminate), crystallising in octahedra ;
cymophane (glucinum aluminate), crystallising according to the

right rhomboidal prism system.
The general formula for these aluminates is
RO.A1 2 3
.
Ebelmen reproduced them by heating, in presence of boric

acid, a mixture of alumina with the oxide forming the base of
the desired aluminate. To obtain balas ruby it is sufficient to
add mixture a trace of potassium dichromate.
to the
Cymophane and gahnite have been reproduced by Deville

and Caron, by heating a mixture of the fluorides of aluminium
and glucinum, or zinc, in a carbon crucible containing a small
platinum capsule filled with boric acid.

Stanislas Meunier prepared artificial spinelle by strongly
heating, for several hours, a mixture of cryolite and aluminium
chloride covered with alumina and magnesia in a carbon crucible
brasqued with magnesia.

A. POTASSIUM ALUMINATE (K 2 A1 2 O 4 3H 2 O). This alu- ,
minate may be regarded as derived from the hydroxide

2
A1 2 O 3 ,
H O= R
2 4.
j-0
It is prepared either by dissolving gelatinous alumina in caustic
potash, or by heating a mixture of alumina with an excess of
potash, to the point of fusion in a silver crucible. On evaporat-
ing the solution in vacuo hard and brilliant crystals of potassium
aluminate are obtained, and may be purified by re-crystallisation.
It isa white substance, very soluble in water but insoluble in
alcohol, with a caustic taste and alkaline reaction. In presence
of a large volume of water it undergoes decomposition, alumina

being precipitated.
B. SODIUM ALUMINATE (Na 6 Al 4 O 9 ) may be considered as
derived from the hydroxide
VI 2 A
2A1 2 3 +3H O= H
rt 6 J
9
.
It is prepared in the same way as the potassium salt, by

substituting caustic soda for potash, and is very soluble in
water, the solution gradually becoming covered with a layer

of sodium carbonate when evaporated in an open vessel.
from its use in dyeing, this product is of great

Apart
industrial interest for the preparation of iron-free alumina, which
is utilised manufacture of aluminium and for the pro-
for the
duction of pure aluminium sulphate and alum.

On a manufacturing scale it is prepared by heating to redness
a mixture of i part of Na 2 CO 3 and 2 parts of bauxite free
from silica, the fritted mass being extracted with water. From
this solution the alumina is separated either by the action of
carbon dioxide or by agitation, a small quantity of recently
precipitated alumina being added to facilitate precipitation
(Baeyer process).
According to Cavazzi, the compound Al 2 O 2 (NaO) 2 is obtained
when aluminium is dissolved in caustic alkali.
C. BARIUM ALUMINATE (Al 2 O 4 Ba, 4H 2 O). This salt was
prepared by Deville, by heating to redness a mixture of alumina

and caustic baryta (barium hydroxide). It is soluble in water,
from which it is thrown down as a

crystalline precipitate by alcohol.
Other aluminates of barium, having the formulae
A1 2 O 3
3 BaO, 5H 2 0; A1 2 O 3 BaO, ;H 2 O; A1 2 O 3
, , sBaO, ,
HO2
have been obtained from baryta water and alumina.

D. CALCIUM ALUMINATE. Ebelmen prepared a crystalline
calcium aluminate of the formula Al 2 O 4 Ca. The compounds of
alumina and calcium are insoluble, and some of them appear to
play a part in the hardening of cement.
Many other aluminates are known, but the only compound
of this class really possessing any industrial interest is sodium
aluminate.
ii. Aluminium Sulphide. Aluminium is not attacked by
sulphur except at a very high temperature. On bringing sulphur
into contact with the red-hot metal, combination occurs and is
accompanied by evolution of heat.

Aluminium sulphide may be prepared by passing sulphur
vapour, in a current of hydrogen, over aluminium heated to
redness; and Fremy has obtained it by passing the vapour- of
carbon disulphide over white-hot alumina in a platinum capsule,

carbon oxysulphide being formed at the same time.
Aluminium sulphide is a pale yellow substance, fusible with
difficulty, and setting to a crystalline mass on cooling. In moist

air decomposes, sulphuretted hydrogen being given off; and
it
water decomposes it instantly, with evolution of sulphuretted
hydrogen and deposition of alumina. When heated to redness

and exposed to steam it is also broken up, an extremely hard
residue of crystalline alumina being left.
12. Aluminium Sulphite. Alumina precipitated from its
salts easily dissolves in sulphurous acid, whereas the alumina

of aluminates is insoluble therein.
Aluminium sulphite is very soluble in water, the solution
yielding a gummy mass on evaporation in vacua. Heated
gently, it gives off sulphur dioxide, and, according to Gouggins-
perg, if the heating be continued until the evolution of gas
ceases, a precipitate of SO 3 (A1 2 O 2 )'

/
, 4H O2
is formed.
Another method of preparation is by heating a concentrated
solution of sodium sulphide with aluminium sulphate on cooling, ;
sodium sulphate crystallises out, leaving aluminium sulphite in
solution.
Jacquemart prepared it by passing a current of sulphur

dioxide through a solution of sodium aluminate, .the effect of
which is to throw down a basic aluminium sulphite, sodium
bisulphite remaining dissolved. The precipitate is collected and
dissolved in an excess of sulphurous acid.
Aluminium sulphite has been utilised in the sugar industry,
for purifying the syrup.
13. Aluminium Sulphates. A. NORMAL ANHYDROUS SUL-

PHATE (SO 4) 3 A1 2 This salt is prepared by dehydrating the
.
crystallised sulphate by heat. It is a white substance of sp.
gr., 2710 (Nilson and Petterson) ;

the specific heat is 0-1855;
molecular heat, 63-59 ;
and molecular volume, 126*50. When
heated to redness it parts with
sulphuric its acid, anhydrous
alumina, A1 2 O 3 being ,behind, prolonged exposure to strong
left
heat being, however, required to drive off the final traces of the
aciH, which are somewhat tenaciously retained. All the basic

salts of aluminium obtained by precipitating the sulphate by

behave in the same way.
ammonia, calcium carbonate, etc.,
at red heat,
Hydrogen reduces anhydrous aluminium sulphate
water and sulphur dioxide being liberated, and alumina almost
entirely free from sulphuric acid left. Ammonium chloride
also this sulphate, with the assistance of heat, and

decomposes
gives rise to volatile products.
Whenfused with sulphur the anhydrous sulphate is reduced
to sulphide, with evolution of sulphur dioxide. When treated
several times in succession with acid, in the warm,
hydrochloric
a small portion is converted into aluminium chloride.
The aluminium sulphate varies according to the
solubility of
temperature, Poggiale giving the following values per

100 parts
of water :
Temperature. dissolved. Temperature.

o 31-30 60 59-09
'
10 33-50 7 66 2 3
20 36-15 80 73-I4
30 40-36 90 80-83
40 45-73 100 89-11
5 52-I3
B. ORDINARY ALUMINIUM SULPHATE, (SO 4) 3 A1 2 i8H 2 O, ,

is
a white occurring most frequently in masses resembling fat

salt,
in consistency also as powder, lumps, etc. It is greasy and unctu-

;
ous to the touch, and is deliquescent when an excess of sulphuric

acid is present. It is extremely soluble in water, and crystal-
lises, though with difficulty, in needles or nacreous white scales.

Handsome crystals may be obtained by leaving a concentrated
solution of aluminium sulphate for a considerable time in absolute
quietude in a large uncovered beaker. The crystalline habit is

that of an orthorhombic prism, considerably flattened along g1 ,
with the faces mh l a l scarcely developed at all. When perfectly

free from sulphuric acid the salt is efflorescent.
The flavour is sweet at first, but
astringent afterwards.
Aluminium sulphate is generally regarded as a hydrate
(sp. gr., i'767 at 22) containing 18 molecules of water, but,
according to P. Margueritte Delacharlonny, the proper formula

hydrate should be (SO 4) 3 A1 2 i6H 2 O.
for the typical ,
In solution, aluminium sulphate is acid to litmus paper, and

turns Congo-red blue. It is almost insoluble in alcohol, but dis-
solves readily in hot hydrochloric acid, handsome colourless tablets
being obtained as the solution cools down. Under the influence of

heat it swells up and loses water, a porous mass of low solubility
being left. When heated to redness it leaves an alumina

tenaciously retentive of the final traces of sulphuric acid.
On treating an aqueous solution of aluminium sulphate with
alcohol a precipitate of hard nacreous flakes consisting of
(SO 4 ) 3 A1 2 ,
ioH 2 O is obtained, which when gradually heated parts
with water and sulphuric acid, leaving behind a skeleton of
insoluble alumina retaining the form of the original crystals. On
the other hand, in contact with moist air, the precipitate absorbs
water and is converted into (SO 4 ) 3 A1 2 i8H 2 O.
,
Aluminium sulphate in solution is decomposed by calcium

carbonate, zinc, forming with the first-named reagent calcium
etc.,
sulphate, an insoluble basic aluminium sulphate, and carbon

dioxide, the latter being disengaged. Zinc gives in the warm
an abundant liberation of hydrogen, zinc sulphate, and a sub-
sulphate of aluminium, 3(SO 4 A1 2 O 2 ), 2A1 2 O 3 + 2oH 2 O, being
formed. In the cold the reaction is less rapid, but the mass
gelatinises by degrees, and here again a sub-salt is produced,
represented by the formula 3(SO 4 .A1 2 O 2 )A1 2 O 3 36H 2 O. The ,
same product in a different form is also obtained from the

reaction of calcium carbonate on alum (H. Debray). These
basic salts will be more fully discussed later on.
On heating a concentrated solution of sodium sulphite with
aluminium sulphate and leaving to cool, crystals of sodium
sulphate are obtained, whilst aluminium sulphite remains in
solution (Man/oni).
A concentrated solution of aluminium sulphate forms an
excellent reagent for salts of potassium, ammonium, etc., by pro-
ducing a highly characteristic precipitate of alum.

Aluminium sulphate is found in nature. The commercial
product assumes the form of cakes, blocks, lumps, powder, etc.,
and is more or less dry according to the degree of concentration
before casting. It is opaque and white, the whiteness being more

pronounced as the salt is purer. Ferrous sulphate imparts a
greenish tinge, whilst in presence of ferric sulphate a reddish

coloration appears ;
and aluminium sub-sulphate turns the mass
yellow. When cast in cakes, aluminium sulphate resembles fat
or alabaster in appearance, and after a time the cakes assume
a crystalline texture in the case of the pure salt. The com-
mercial sulphate often contains free sulphuric acid and potash
alum.
Aluminium sulphate is
extremely soluble in water, the figures
given by Poggiale per I oo parts of water being
(SO 4 ),Al,, iSH.,0 (SO 4 ). ( AI., iSH,0
Temperature.
10
20
30
4
50
We are indebted to Reuss for the determination of the density

of solutions of pure aluminium sulphate, and of the commercial
sulphate prepared from alunite ;

the latter invariably contains
potash alum.
The following table gives the density and corresponding
percentage of (SO 4 ) 3 Al a of these solutions at differenttem-
peratures :
C. BASIC ALUMINIUM SULPHATES. Of these a large num-

ber are known, and, while many of them are probably mixtures,
they are for the most part of little importance, though some
possess a certain decided interest in view of their utility in dyeing.
Some of these basic sulphates are soluble in water. If solu-
tions of the normal sulphate are partly neutralised by carbonates

of the alkalis or alkaline earths, by aluminium hydroxide, etc.,
solutions of basic sulphates are obtained, the salts varying in
composition according to the degree of neutralisation.

With sodium bicarbonate, for example, the following sul-
phates may be produced :
(SO 4 ) 3 A1 2 ,
1 8H 2 O + 2CO 3 NaH
- (SO 4) 2 A1 2 O, H 2 O + SO 4 Na + 2CO 2 + 8H,O. 2
1
2[(S0 4 ) 3 A1,, i8H 0] + 6CO 3 NaH 2
= (S0 4 ) 3 A1,, A1 3 3H,0 + 3SO 4 Na 2 +6CO 3 +36H 2 , 2 0.
(SO 4) 3 A1 2 ,
8H O + 4CO 3 NaH
1
2
= SO 4 A1 O 2H O + 2SO Na + 4CO + i8H

2 2, 2 4 2 2 2 O.
The basic aluminium sulphates may be regarded as derived

from sulphuric acid (H 2 SO 4) by the substitution of the oxygen-
ated radicles A1 2 O and A1 2 O 2 for hydrogen, or they may be
considered as the result of a union of two sulphates of the
following types :
3H S0 4 2 . . .
(S0 4) 3 Al 2 <->,
2H 2 SO 4 . . .
(SO 4) 2 (A1 2 O)
(IV)
,
H 2 S0 4 . . . S0 4 (A1 2 2 )".
Again, they may be also regarded as resulting from the

displacement of one or two divalent groups SO 4 in the normal
sulphate (SO 4 ) 3 A1 2 by I or 2 divalent atoms of oxygen.
,
According to Berzelius, a basic sulphate is produced when

an aqueous solution of normal aluminium sulphate is precipitated
by an insufficiency of ammonia. The formula of the washed
and dried precipitate is given as
S0 4 (A1 2 2 )", 9H 2
= (S0 4 , 2 )A1 2 9 H 2 O.
,
This compound is met with in nature in the form of a white
earthy mass (Websterite) of sp. gr. 1705.

According to Bley, when a solution of alum or aluminium
sulphate is treated with a quantity of ammonia insufficient to
throw down the whole of the alumina, and the precipitate is left
to collect for two or three days, a sub-salt corresponding to the
formula
(S0 4 ) 2 A1 2 0, 2A1 2 O 3) 2oH 2
is obtained after filtering and washing.
Alum, precipitated by ammonium carbonate under the same
conditions, gives the same sub-salt, which, however, always retains
i
per cent, of potash.
When, according to the same author, a solution of alum is
treated with potassium hydroxide or carbonate, avoiding an

excess of the reagent, the precipitate, which only collects very
slowly, has the formula

SO 4 A1 2 2,
A1 2 3,
I2H 2 0.
If a solution of aluminium acetate, containing not more than
0*3 per cent, of alumina, is treated with potassium sulphate and
kept at a temperature of 38, there results, according to Walter

Crum, a precipitate of basic sulphate, which settles down gradually
and contains all the alumina in the solution, its formula being
SO 4 A1 2 O 2 A1,O 3)
,
ioH 2 O.
Certain natural products, such as felsobanite, SO 4
A1 2 O 2 ,
A1 2 O 3 ,
ioH 2 O, and paraluminite, SO 4 A1 O 2 2,
A1 2 O 3 , I5H 2 O,
exhibit analogous composition.
A basic sulphate is easily obtained by heating a concen-
trated aqueous solution of aluminium sulphate with aluminium
hydroxide. The resulting salt has, according to Mans, the
following composition :
(SO 4 ) 2 A1 2 O, H 2
O.
It. is encountered in nature, in the anhydrous condition, as
alumiane.
According to Marguerite, when alumina in any desired quan-

tity is dissolved in the neutral sulphate, or the latter is treated
with zinc, or potash- or ammonium alum is heated with care, an
identical product, (SO 4 ) 2 A1 2 O, I2H 2 O, is
always obtained.
When a concentrated solution
sulphate is of aluminium
boiledwith aluminium hydroxide a
gummy mass is obtained,
which contains twice as much alumina, in
proportion to the
AND COMPOUNDS OF THESE METALS 2J
amount of acid, as is present in the neutral sulphate. This

product is soluble in a small volume of water, but, if boiled in
a larger quantity of that liquid, breaks up into normal sulphate,
which remains and a precipitate of more highly basic
in solution,
sulphate, believed by Berzelius to have the composition

2(SO 4 A1 2 2 ) + (SO 4 ) 2 A1 2 O + 3oH 2 O.
On saturating very dilute sulphuric acid with aluminium
hydroxide and setting it aside for some years, Rammelsberg

obtained a crop of transparent, microscopic needles of the above
composition.
In contact with a hot solution of neutral aluminium sulphate,
zinc liberates an abundant volume of hydrogen. By heating a
similar solution with zinc in a platinum capsule Debray obtained
an easily washed granular precipitate, soluble in dilute acids, and
having the formula

3(SO 4 A1,O 2 ), 2A1 2 O 3 2oH 2 O.
, ,
In the cold the reaction is slower. On leaving a cold solu-

tion of aluminium sulphate in contact with zinc and platinum
for eight days the same experimenter obtained a gelatinous
precipitate, which, when washed and dried, consisted of hard
lumps with a vitreous fracture, and exhibiting the composition

3 (S0 4 A1 2 2 ),
A1 2 3 3 6H 2 0.
,
Debray also obtained the same salt, as a crystalline
precipitate, by digesting calcium carbonate with a cold solution

of ordinary alum.
When zinc and platinum are simultaneously introduced in
a cold aqueous solution of alum, the zinc gradually dissolves,
with evolution of hydrogen, and a crystalline precipitate of
5(SO 4 A1 2 O 2 ), 3A1 2 O 3 25H 2 O is formed. Athanesco obtained a

,
basic sulphate, with the formula 2(SO 4 A1 2 O 2), (SO 4) 2 A1 2 O, 9H 2 O,

by heating a 3 per cent, solution of neutral aluminium sulphate
to about 250. This salt crystallised in small, colourless, trans-
parent rhombohedra, greatly resembling cubes.

An
aqueous solution of neutral aluminium sulphate, con-
taining sodium chloride, heated to 130 140 for 2 hours,
furnished with a in-
Bottinger white, pulverulent precipitate,
soluble in water and acetic acid. At red heat it parted with
only 2 molecules of water, and its composition corresponded to

SO 4 A1 O 6H
2 2, 2 O.
The existence of basic sulphates as so many separate

chemical entities has been denied by certain authors. S. U.
Pickering states that he failed to obtain basic sulphates of
constant composition.
14. Alums. A. GENERAL REMARKS. Aluminium easily

forms double salts with metals, the alums being the most
important compounds of this class.
The name alum is given to a remarkable series of bodies,

typified by potash alum, to which alone the generic term was
formerly applied.
The general formula is (SO 4) 3 M 2 SO 4 R 2 24H 2 O.
, ,
All the alums are more or less soluble in water and crystallise
in regular octahedra, though at first sight the octahedron is not
always recognisable in the crystals obtained, since the volume
and the relative dimensions of the facets and edges may vary
considerably according to the conditions under which crystallisa-
tion was effected. Nevertheless, though these conditions may
produce deformations totally modifying the external appearance,
the dihedral angles formed by the intersection of the facets
always remain unchanged. The various shapes assumed by

the octahedron are shown in Figs. 10 to 13.
FIGS. 10 to 13.
The alums
differ from one another
only because the alumina
and potash may be replaced, wholly or*in part, by isomorphous
substances. For example, alumina may be replaced by the
sesquioxides of iron, manganese, chromium, etc., whilst the place
of potash may be filled by soda, ammonia, the oxides of
rubidium, cesium, thallium, etc.
Alums with organic bases have also been prepared, such as
trimethylamine alum, ethylamine alum, methylamine alum, and

amylamine alum ;
and selenic acid, which is
isomorphous with
sulphuric acid, may replace the latter in combination, and thus
also furnish alums.
Furthermore, mixed alums may be prepared by mixing

solutions of different alums together and leaving them to
the formation of crystals being facilitated in some
crystallise,
cases by adding a certain quantity of ordinary alum to the
solution. Thus iron alums with a base of thallium are more
easily obtained as large crystals when part of the ferric oxide
is
replaced by an equivalent quantity of alumina.
A crystal of any alum may be developed in a solution of
some other alum, by reason of the isomorphism of these salts ;
and it is for this reason that a crystal of chrome alum may

be grown in a solution of ordinary alum, and vice versd.
The method of naming these compounds makes them easily
recognisable. If merely the name of the metal or oxide re-
placing potash is given, the alum always contains alumina.

For example :
Sodium alum = (SO 4) 3 A1 2 SO 4 Na 2 + 24H 2 O. ,
Ammonium alum = (SO 4) 3 A1 2 SO 4 (NH 4 ) 2 + 24H 2 O. ,
When only the name

of the metal or oxide taking the place
of the alumina is given, potassium is always the second metal.
For instance: chrome alum = (SO 4 ) 3 Cr2 SO 4 K 2 + 24H
, 2
O.
If the place of the two metals aluminium and potassium is
occupied by isomorphous bodies, the names of both substitutes

are given in speaking of the resulting alum.
Thus: ferro-ammonium alum = (SO 4) 3 Fe 2 ,SO 4 (NH 4) 2 + 24H 2 O.
When the acid is other than sulphuric acid it also is specified.
At present a number of alums are known, among which the
following may be cited :
Ordinary alum . .
(SO 4 ) 3 A1 2 ,
SO 4 K + 24H O. 2 2
Ammonium alum . .
(SO 4) 3 A1 2,
SO (NH 4) + 24H
4 2 2 O.
Sodium alum. . .
(SO 4) 3 A1 2 , SO 4 Na + 24H O. 2 2
Rubidium alum . .
(SO 4) 3 A1 2, SO 4 Ru 2 + 24H O. 2
Cesium alum . . .
(SO 4) 3 A1 2, SO 4 Ce + 24H O. 2 2
Thallium alum . .
(SO 4 ) 3 A1 2
,
SO 4 T1 2 + 24H O. 2
Manganese alum .
(S0 4) 3 Mn 2 SO 4 K 2 + 2 4 H 2 O.
,
Chrome alum (SO 4 ) 3 Cr2) SO 4 K 2 + 2 4 H 2 O.

Iron alum (SO 4 ) 3 Fe 2) S0 4 K 2 + 2 4 H 2 0.
Chrome-ammonium alum. (S0 4 ) 3 Cr 2 S0 4 (NH 4 ) 2 +2 4 H 2 0.
,
Ferro-ammonium alum (S0 4) 3 Fe 2) S0 4 (NH 4 ) 2 +2 4 H 2 0.

Ferro-thallium alum (S0 4) 3 Fe 2) S0 4 T1 2 +2 4 H,0.
Selenium alum (SeO 4) 3 Al 2 SeO 4 K 2 +2 4 H 2 0.
,
FIG. 14. Octahedron modified by facets of the cube and the

rhomboidal dodecahedron.
The organic alums having been already mentioned, need not

be referred to again.
In the same manner that basic sulphates are prepared from
aluminium sulphate, alums may be made to yield double basic
salts, which are, moreover, found in nature, e.g., alunite, loevigite.
Whilst some of these compounds are merely of theoretical

have found extensive application, and form the
interest, others
object of considerable industrial and commercial enterprise. A

description of the principal kinds will now be given.
AND COMPOUNDS OF THESE METALS 3!
B. POTASSIUM (POTASH) ALUM. I. Ordinary Alum (SO 4 ) 3 A1 2 ,
SO K + 24H
4 2 2 O. In the laboratory this salt is prepared
by dissolving and crystallising together equivalent proportions
of pure aluminium sulphate and potassium sulphate. It may be
purified by successive re-crystallisations, provided no other alum,
FIG. 15.
even in small amount, is present ;

otherwise separation is very
difficult, if not quite impossible.
When dissolved, alum exhibits an acid reaction and a sweet
flavour with an astringent after-taste. It crystallises in regular
octahedra, which may be obtained of large size, colourless, and

transparent. The most frequent modification of the crystals is
by facets of the cube and the rhomboidal dodecahedron (Fig. 14),
and such modifications are easily produced.
Fig. I
5 shows the relation between the crystal and the cube,
and dodecahedron.
The solution of ordinary alum can be supersaturated with
ease ;
and alcohol will precipitate the salt from its solutions.
When freshly prepared the crystals are translucent, but

become opaque after a lapse of some days. On exposure to
the air for some considerable time they become milky and
resemble marble or alabaster, by reason of a slight efflorescence,
and more particularly by the formation of a superficial layer of
a sub-salt under the influence of atmospheric ammonia.
According to Poggiale, 100 parts of water dissolve

., . 43 1,., SO 4 K..-i
Temperature. dissolved. Temperature. dissolved.
3-90 60 66-65
IO 70 90-67
20 80 1
34 '47
30 22'IQ 90 209-31
40 30-92 100 357-48
50 44'II
When kept over sulphuric acid in a closed vessel, or heated

to 61, alum loses 18 molecules of water (Graham); and at
92' 5 it melts in its own water

of crystallisation. If the temper-
ature be increased, dehydration
gradually ensues, and the whole
24 molecules of water (45-5 per
cent, of the total weight) are
parted with by degrees.

When heated to redness in
a crucible, alum swells up and

projects far above the mouth of
the vessel (Fig. 1
6). The porous
and friable mass thus obtained
forms the calcined alum employed
FIG. 16. as a caustic. At a bright red
heat alum is
decomposed, sulphur trioxide being given off together
with sulphur dioxide and
oxygen, whilst alumina and potassium
sulphate are left behind. If the temperature be raised still higher,
and the heating prolonged, potassium aluminate will be formed.
On exposing a mixture of 3 parts of calcined alum and

i
part of lampblack to moderate heat, in a crucible, a
pulverulent mass, igniting spontaneously in contact with air

(Homberg's pyrophore), is obtained. This consists of a very
finely divided mixture of alumina, carbon, and potassium
sulphide.
Crystallised anhydrous alum may be prepared by heating
to fusion a mixture of alumina and potassium bisulphate. On
taking up the mass with hot water small hexahedral crystals
of anhydrous alum are obtained (Salm-Horstmar). This product
is soluble, though slowly, in water, the following percentage
solutions being obtained (Poggiale) :
(SO,),A1 2 ,
SO 4 K 2 (SO 4 ).,A1 2 SO 4 K 2
,
Temperature. dissolved. Temperature. dissolved.
2'10 6O 2670
10 4-99 70 35-11
20 774 80 45-66
30 10-94 90 58-68
40 14-88 100 74-53
50 20-90
The density of these solutions is given below :
(S0 4 ),AU,S0 4 K, (SO 4 ) 3 A1 2 ,SO 4 K 2

Sp. gr. +24H..O Sp. gr. + 24 H 2 O
1-0065 l
P er cent - i'O2i8 4 per cent.-
I'OIIO 2 ,, i -0269 5 , ,
1-0166 3 ,, 1-0320 6 ,,
We have already seen that alum crystallises in octahedra ;
but there is a variety met with in commerce (Roman alum) as
cubical crystals, and this kind was formerly preferred to all
others by reason of its freedom from soluble iron salts. It is
prepared from alunite, and only differs from ordinary alum in

containing a slight excess of alumina (Leblanc).
A crystal of ordinary octahedral alum, if cut in the shape
of a cube and placed in a solution of alum rendered basic by
a little ammonia, will continue to grow, still retaining the cubical
form; but if octahedral facets have been cut on the cube they
will gradually disappear and the crystal will again become
cubical. The converse, however, occurs if a solution of ordinary
alum be employed.
3
De Hauer obtained hemihedral alum by cutting tetrahedron

facets on a crystal of cubical alum and leaving it to grow in a
solution of basic alum.
Ordinary alum may give rise to basic double sulphates,
erroneously termed basic alum.

II. Alunite. If caustic potash, soda, ammonia, or an alkali
carbonate be added to a solution of alum a precipitate will be
formed, which will re-dissolve 'on agitation, provided a slight
excess of reagent has not been employed in the case of ammonia

or the alkali carbonates. The originally acid reaction of the
liquid will have become neutral, and on evaporating the solution
at the ordinary temperature a crystalline incrustation, having the
formula
SO 4 A1 2 2, (SO 4) 2 A1 2 0, SO 4 K 2 , 3 HO
2
will be obtained.
When evaporated at 40 the formula of the precipitate will
be s(S0 4 A1 2 2 ), SO 4 K 2 6H 2 O.
, ,
According to A. Mitscherlich, when a mixture of 3 grams of

aluminium sulphate, I
gram of potassium alum, and 10 c.c. of
water is heated to 230, rhombohedral crystals, with angles
measuring 91*30 and 88'3O, and exhibiting the composition of
be formed.
alunite, will
Natural alunite is a very important mineral.
III. Larvigite. On boiling a concentrated solution of alum
along with zinc, in a platinum capsule, hydrogen liberated, and is
a crystalline product, having the formula 3(SO 4 2 O 2), SO 4 K 2>

A1
9H 2 O, is obtained. This is Icevigite, and, according to Debray,
the precipitate is almost insoluble in concentrated hydrochloric
acid and nitric acid, but soluble in a mixture of equal parts, by
weight, of water and sulphuric acid.
The same salt, but readily soluble in acids, has been
obtained by Riffault by treating a solution of alum with
caustic potash, avoiding any excess of the reagent and the ;
same worker also prepared it by boiling aluminium hydroxide

in alum solution.
Walter Crum prepares Irevigite by heating a solution of alum

with aluminium hydroxide or insoluble aluminium bi-acetate.
Mitscherlich has prepared it by heating a solution of ordinary

alum to 230 in a sealed tube. It was this author who bestowed
the name of loevigite on the precipitate obtained by him, which

gave the following composition :
3(S0 4 A1 2 2 ), S0 4 K 2, 9 H 3 0.
He also prepared it
by heating potassium sulphate with
aluminium sub-sulphate.
Loevigite differs from alunite solely in that it contains a
slightly higher percentage of water, which, however, it loses more
readily when heated, and is further distinguishable from alunite
by furnishing potassium sulphate, instead of alum, when subse-

quently taken up with water.
IV. Roman Alum. This body, which has already been
briefly referred to, only differs from ordinary alum by contain-
ing a slight excess of alumina and by crystallising in cubes.
For a long time it constituted a very important industrial
product, superior in many instances to ordinary alum by its
freedom from soluble compounds of iron, and was prepared

from alunite. It may easily be reproduced by adding a
little ammonia or an alkali carbonate to a solution of ordinary
alum heated to 30 or 40, cubical alum crystallising out as
the liquor cools down. When heated beyond 50 solutions
of cubical alum deposit a little aluminium sub-sulphate, and
the liquor on crystallising out will then furnish octahedral
alum solely.
C. AMMONIUM ALUM. I. Ordinary variety (SO 4) 3 A1 2 ,
SO 4 (NH 4) 2 24H 2 O. This salt

,
is used industrially in place of
ordinary alum, and serves almost every purpose fulfilled by the
latter. Both salts are produced in turn by alum manufacturers,
the most weighty considerations influencing their production
being the relative market price of the crystallising reagents,
potassium sulphate and ammonium sulphate at the present ;
time the latter (" sulphate of ammonia ") being the cheaper, the
balance is in favour of ammonium alum.
Great similarity exists between these two alums, both in
appearance, crystalline habit (Fig. 1

7), and solubility.
When heated, ammonium alum melts and swells up like
potassium alum ; and, like the latter, is also slightly efflorescent.
Strongly heated, it leaves behind a residue of pure alumina.

The temperature
required to render
this decomposition
complete is much
higher than that
necessary to secure
the volatilisation of
ammonium sulphate ;
consequently, if
FIG. 17. Block of alum.
alum coated with
ammonium sulphate be heated carefully, the latter can be
volatilised without affecting the composition of the alum.
'The sp. gr. of ammonium alum is 1*631.
The dehydrated alum is slightly less soluble in water than
ordinary ammonium alum, 100 parts of water taking up (accord-
ing to Poggiale)
(SO 4 ),AI,, SO 4 (NH 4 ) 2 + 24 H.,O
Temperature. dissolved. (SO 4 ).1 A1 2 SO 4 (XH 4 )
,
o 5-22 2-63
10 9-16 4-50
20 13-66 6'57
3 I9-29 9-05
40 27-27 12-35
50 36-51 15-90
60 51-29 21-09
70 7I-97 26-95
80 103-08 35 '19
90 187-82 50-30
100 421-90 70-83
The densities of ammonium alum solutions at 17-5 are

below, with the
given corresponding percentages of the dis-
solved salt :
(S0 4 ).,A1 2 , SO(NH 4 ) S (SO 4 ) S A1,,

Sp.gr. 24 H 2 O. Sp. gr. 24 H.,O.
4
i -0060 1
per cent. I-O2OO 4 per cent.
1-0109 2 ,, 1-0255 5 ,,
1-0156 3 I-0305 6
According to Mulder, the saturated solution boils at iiO'6,

and contains 2077 parts of alum,
expressed as anhydrous alum.
II. Basic Sa/ts Just as, in the case of potassium alum,
alunite and loevigite are obtained, ammonium alum will also
yield basic double salts.

When ammpnia is added to a cold solution of alum there
ensues a precipitate which re-dissolves on agitation, provided
there is no excess of ammonia, the solution then containing
the salt
(S0 4 ) 2 A1 2 0, S0 4 (NH 4 ) 2 ,
which crystallises with difficulty.
According to Riffault, the addition of ammonia to a boiling

solution of alum, until the precipitate becomes permanent, results
in the formation of an ammoniacal loevigite,
3(S0 4 A1 2 ,
2 ), S0 4 (NH 4 )2, 9 H 2 0.
By keeping a mixture of ammonium sulphate, aluminium

sulphate, and water at 190, an alunite
3(S0 4 A1 2 O 2 ), SO 4 (NH 4 ) 2
, ,
6H 2 O,
analogous to potassium alunite, is obtained.

Ammonium alum is found to a small extent in nature.
D. SODIUM ALUM, (SO 4 )3 A1 2 , SO 4 Na + 24H 2 2 O, may be

prepared by crystallising a solution containing equivalent
quantities of aluminium sulphate and sodium sulphate. It has
the same crystalline form as ordinary alum, but is very efflor-
escent, the crystals turning to powder at the end of a few
days.
According to Buignet, the sp. gr. of sodium alum is i'$6?.
It is
very soluble in water, 100 parts of water at 16 taking up
1 1 o
parts of the salt. For this reason sodium alum cannot be
separated, on a manufacturing scale, from sulphate of iron, and
therefore ferruginous materials are unsuited for the preparation of
this alum.
Solutions of sodium alum are very easy to supersaturate.
If a solution of this salt be concentrated by evaporation to a
point at which it begins to solidify on cooling, it will be found

that large crystals form on the addition of a little water, the
entire mass crystallising from the surface downwards. The
change is facilitated by stirring.
Sodium alum is insoluble in alcohol. It occurs in nature as

mendozite.
15. Aluminium Dithionate is obtained by decomposing

barium dithionate with aluminium sulphate, but is for the most
.
part decomposed during the evaporation of the solution.
1 6. Aluminium Nitride (A1 2 N 2). This body occurs in the
crystalline form as short orthorhombic prisms with dihedral

apices. In the amorphous condition it is pale yellow, while the
crystals are translucent and of a honey-yellow colour.
was obtained by Mallet in various experiments, wherein

It
aluminium was raised to a high temperature in a carbon crucible.

The surface of the metal exhibited yellow crystalline particles,
which were liberated, by dilute hydrochloric acid, along with
an amorphous mass of the same colour. The nitrogen was
evidently derived from the air traversing the crucible walls.
The nitride was always accompanied by a little crystalline

alumina.
To obtain a sufficient quantity for examination, Mallet heated
aluminium to a very high temperature with dry sodium car-
bonate, in a carbon or lime crucible contained in a second

crucible of graphite, the space between the two vessels being
packed with lampblack.
When calcined in contact with air this body slowly yields up
its nitrogen, and the aluminium oxidises. In presence of moist
air decomposes spontaneously, alumina being formed and
it
hydrogen evolved. The amorphous nitride is less stable than the

crystalline form.
17. Aluminium Nitrate (Al 2 (NO3) ti ,
2H 2 O) is obtained by
dissolving aluminium hydroxide in nitric acid. The solution is
evaporated, care being taken that the liquid contains an excess

of acid and, on re-cooling, large crystals are
;
deposited, which
contain 1 5 molecules of water. When crystallised in concen-
trated nitric acid, only 2 molecules of water are retained.
Aluminium nitrate is a very deliquescent salt. At about 140
it
decomposes into alumina and nitric acid and this property ;
has been utilised in analysis for the separation of aluminium

from calcium and magnesium.
The crystals of aluminium nitrate melt at y2 8

-
to a colour-
less liquid, which solidifies on re-cooling, the mass having a
crystalline texture. They are soluble in water, nitric acid, or
alcohol.
1 8. Aluminium Phosphates. These are three in number,
derived from
PO 4 H 3 . . .
Orthophosphoric acid,
P O H
2 7 4 . . .
Fyrophosphoric
'
PO H 3 .
Metaphosphoric
. .
A. ALUMINIUM ORTHOPHOSPHATE, (PO 4) 2 A1 2 . This salt is
prepared by precipitating a neutral solution of alumina with

ordinary sodium phosphate, and comes down as a white gelatinous
substance, which, when dried in the air, retains 9 molecules of
water (Rammelsberg). According to the results obtained by
different workers, the content of water varies and does not
appear to be very constant.
The salt prepared as above is soluble in caustic potash, but
insoluble in acetic acid. This property, which is shared by
ferric phosphate, enables these two to be easily separated from
the phosphates of lime, magnesia, etc.
When
phosphoric acid is added to a concentrated solution of
sodium aluminate until the reaction is acid, and the mixture is
then heated to 250 under pressure, the salt (PO 4) 2 A1 2 is obtained
as hexagonal prisms, of sp. gr. 2-59, infusible at red heat, insoluble
in HC1, HNO 3)
and soluble (though with difficulty) in concen-
trated H SO2 4 .
By heating dissolved alumina in phosphoric acid,
Hautefeuille and Margottet obtained
At 100, the salt A1 2 O 3 3P 2 O 5
, ,
6H 2 O, crystallising in colour-
less prisms ;
At 150 to 200, the salt A1 2 O 3 3P 2 O 5 4H 2 O, in needles; , ,
Above 200, the salt A1 2 O 3 3P 2 O 5 crystallising in regular , ,
tetrahedra.
According to Rammelsberg, the addition of ammonia to an

acid solution containing aluminium phosphate results in the
formation of a basic salt,
3 ), 3 (P 2 5 ), i8H 2 0, 4(A1 2
which phosphate, combined with the aluminium fluoride, forms
the native mineral wavellite, the composition of which is given by

Berthier as
A1 2 F6( [(A1 2 3 ) 4 (P 2 5) 3 ] 3 36H 2 0.
, ,
Onboiling a mixture of dissolved aluminium sulphate and
ordinary ammonium phosphate in presence of a little sulphuric

acid, there results, according to Millot, an acid phosphate,
2(PO 4 ) 3 A1 2 H 3 + i;H 2 O.
This compound, when treated by phosphoric acid in suitable
amount, furnishes a residue which, when washed and analysed,

yields values corresponding to the formula
(P0 4) 4 A1 2 H 6 5 H 2 0.
,
By precipitating with ammonia an acid solution of one of
the foregoing phosphates, avoiding an excess of the reagent,

Millot obtained a basic phosphate,
2(PO 4) 2 A1 2 A1 2 O 3
, ,
8H 2 0.
B. ALUMINIUM PYROPHOSPHATE is obtained as a white
amorphous precipitate soluble in mineral sodium pyro-

acids,
phosphate solution, ammonia, etc., by neutralising sodium pyro-

phosphate with aluminium chloride solution.
It may also be prepared, this time as very fine clinorhombic
crystals, by treating aluminium metaphosphate with fused meta-

phosphoric acid containing a certain quantity of tribasic silver
phosphate (Hautefeuille and Margottet).
C. ALUMINIUM METAPHOSPHATE. Hautefeuille and Mar-
gottet obtained this salt by treating alumina with fused meta-
phosphoric acid. On treating the mass with boiling water,
aluminium metaphosphate is obtained in the form of cubic
crystals exhibiting modifications tending towards the octahedron,

rhomboid dodecahedron, or trioctahedron. Nevertheless, when
this method of preparation adopted, the crystals are for the
is
most part badly formed, being softened by the temperature

necessary for fusing the metaphosphoric acid. Fine, large
crystals, free from silver, may, however, be obtained by adding to
the mass a small quantity of triargentic phosphate, which
imparts fluidity to the metaphosphoric acid.
If the proportion of triargentic
phosphate is at all large, and
particularly when 2 parts of alumina are added to a mixture
AND COMPOUNDS OF THESE METALS 4!
of 4 to 6 parts of metaphosphoric acid and 8 parts of tri-
argentic phosphate ;
or if crystals of aluminium metaphosphate
be treated with about 3 times their own weight of triargentic
nitrate, the crystals obtained are colourless, perfectly trans-
parent, double energetically on polarised light,

refracting, act
and are derived from an orthorhombic prism. Their formula is
2A1.0* Ag 2 0, 4 PA-
A slight excess of
metaphosphoric acid gives rise to clino-
rhombic crystals of aluminium pyrophosphate, whilst an excess of
triargentic phosphate produces pointed octahedra, apparently
derived from a clinorhombic prism, and corresponding to the
formula 2A1 2 O 3 3 P , A-
Aluminium phosphate occurs in nature, most frequently as a
double phosphate (wavellite, amblygonite, childrenite, turquoise).
19. Aluminium Arsenite. This salt may be obtained by
precipitating aluminium sulphate with barium arsenite and con-

centrating the nitrate at first by gentle heat, and afterwards
over sulphuric acid. It crystallises in fine rhombohedral octa-

hedra. On
concentrating the solution of these crystals, at 70,
arsenious acid is formed, a basic arsenite remaining in solution.
20. Aluminium Arsenates. Coloriano obtained the arsenate
(As5 O 4 )2 A1 2 as
,
lenticular crystals, by heating a solution of
trisodic arsenate and aluminium sulphate to 200. The "neutral
"
arsenate of Berzelius, (As 2 O T ) 3 Al 4 was the pyro-arsenate.
,
Prob-
ably this salt is hydrated and corresponds to
It is insoluble, but there is a very soluble acid salt which
cannot be crystallised, and probably corresponds to the formula
21. Aluminium Silicates. In nature these silicates occur

in considerable quantities, and constitute diosthene, the felspars,
kaolins, clays, etc. Fuller details of these rocks will be given in
dealing with aluminium minerals. Double silicates of this metal

are also easily produced, and are in fact the most frequent form
of occurrence.
By exposing an intimate mixture of 4 parts kaolin and 3

parts common salt to a cherry-red heat, Gorgeu obtained a double
silicate of aluminium and sodium, 2SiO.,, A1 2 O 3 Na 2 O. The ,
same author also prepared the double silicate of aluminium and

potassium, 2SiO 2 A1 2 O 3 , ,
K 2 O, by heating I
part of kaolin with
2 parts of potassium iodide in a covered platinum crucible for
2 hours. The resulting salt is amorphous, insoluble in water,
and retains 2 per cent, of iodide.
These double silicates are soluble in hydrochloric acid and

dilute nitric acid, but insoluble in alkalis or carbonates ;
and are
infusible, or nearly so, at a bright-red heat.
When i
part of kaolin, 2SiO 2 A1 2 O 3
, ,
2H 2 O, and 13 parts
of sodium carbonate are heated together, it will be found that
carbon dioxide is evolved at a cherry-red heat, and again when
the temperature approaches orange-red heat. Consequently there
are two successive reactions, and these give rise to different
silicates, the first corresponding to the formula

3 Si0 2 ,
2A1 2 3) 3 NaO,
whilst the second approximates to
SiO 2 A10 3 Na 2 0.
, ,
The action of fused caustic soda on kaolin" is very rapid.
3. ALUMINIUM MINERALS
Aluminium is met with

very abundantly in nature, in the
form of numerous compounds, the most important of which
belong to the silicate series of minerals.
Many of these compounds, whether silicates, oxides,

hydroxides, or sulphates, etc., have found extensive application,
and are utilised by the jeweller and in various industries. The

most interesting of these bodies will now be examined.
22. Minerals containing Fluorine. A. FLUELLITE. White,
vitreous, crystalline incrustations, found on Stenno-Gwyn quartz
(Cornwall), and consisting of aluminium fluoride. This mineral
belongs to the third degree of hardness, and crystallises in ortho-
rhombic octahedra a'a' = 109 6' and 82 12'.
B. TOPAZ, SiO 4 (Al 2 F 2 ), (syn. :

Chrysolite, physalite, pyro-
physalite, pycnite).
Occurs as honey-yellow, brownish, reddish, bluish, or colour-
less crystals in gneiss and granite, associated with tourmaline,
mica, or emerald ; frequently also with apatite, fluorine, cassiderite,

etc. ;
or in talc rocks or mica schist
The principal deposits are in the Ural and Brazil.
Topaz is slightly attacked by H SO2 4, hydrofluoric acid being

liberated. In the blast furnace it parts with silicon fluoride,
without fusing. Tested with cobalt nitrate, it gives the reaction
for alumina.
The hardness of these crystals is 8, the sp. gr. 3^4 to 3'6,
and the crystalline form that of orthorhombic prisms. See Figs.
I 8, 19, 20.
FIGS. 18, 19, and 20. Topaz.
C. CRYOLITE is a double fluoride of aluminium and sodium,

A1 2 F 6 6NaF.,
It is found as fragile, whitish, crystalline masses
cleaving in three rectangular directions, and occurs in Greenland

and the Ural.
Sulphuric acid decomposes cryolite, liberating HF. It is
very fusible; has a sp. gr., 2'9 to 3-7 ; hardness, 2'5 ;

and
crystallises in the anorthic system.
23. Anhydrous Aluminium Oxide Minerals (A1 2 O 3).

A. CORUNDUM. This mineral is a pure, crystalline sesquioxide
of aluminium, colourless, and crystallising in the rhombohedric
system. The primitive rhombohedron (86'4) is, however, rare,
and the mineral is mostly found in basal hexagonal prisms d-â^
frequently terminating in pyramids.

The hardness is 9 ;
the sp. gr. ranges from 3-9 to 4-2 ;
refractive power, 0^73 9. It exhibits double refraction at one
negative axis.
Corundum is unacted on by acids and is infusible in the
blast furnace.Owing to its hardness and high re-
fractive power, it forms a highly precious stone for
the jeweller.
In addition to the colourless variety, corundums
are met with containing traces of the oxides of iron,
chromium, or titanium, and forming coloured gems,

each of which has its distinctive name.
Tinged with red by traces of chromium oxide,

it is more valuable
constitutes the oriental ruby, which
than the diamond. The finest specimens come from
Ceylon, India, and China.
Coloured blue, forms the sapphire, varying in shape from
it
dark to very light blue, and less valuable than the ruby.
The green corundum, or emerald, is very rare, and is found

in Ceylon.
The oriental topaz is yellow corundum. It is of lower value

than the preceding gems.
Violet corundum, or oriental amethyst, is somewhat rare.
A considerable quantity of corundum is found in France,

in the extinct volcanoes of Auvergne ;
but the
mineral is of no value, the crystals being devoid
of transparence.
Emery is a mixture of corundum and ferric
oxide, the latter often attaining 30 per cent. It is
a dark coloured mineral, two types of which are

met with the compact and the granular fre-
FIG. 22.
quently containing quartz, chlorite, etc.
Corundum.
Emery is found in beds or stratified deposits
among gneiss rocks and mica schists, in Saxony, China, India,
and, above all, in Asia Minor, the first deposit having been found
in the latter region at the ancient city of
Gumuch-Dagh, near
Magnesia.
On account of its hardness this mineral is employed for
polishing hard substances, metals, etc.

24. Aluminium Hydroxide Minerals. A. DIASPORE (A1 2 O 3 ,
H 2 O). Diaspora is generally found with corundum in dolomite,
chloritic schists, etc.; and has been discovered in gneiss at
Bournac (Haute-Loire). It crystallises in the orthorhombic

/
system; generally as orthorhombic
prisms (;;/;;/. I2947 ),
truncated at g l
,
and terminating in a octahedron b^b^= 151 34'.
The line of cleavage is along g^ or, less frequently, m. Degree
of hardness, 6'5 to 7 ; sp. gr., y2 to 3'5 ;
colour
white or yellowish white. It is transparent, and
exhibits a very brilliant, conchoidal fracture.
Heated in a sealed tube, diaspore decrepitates
violently, and forms white, pearly scales. At a high

temperature water is liberated. Tested with cobalt
nitrate, it gives a fine blue coloration. In its
FIG. 23.
ordinary state it is unacted upon by acids, but loses Diaspore.
its resistance when calcined.
B. BAUXITE (A1 2 O 3 2H 2 O). ,
This mineral is sometimes
compact, sometimes oolitic, and occurs as concretionary rounded
grains or as earthy masses. The colour is variable :
white, grey,
brown,
yellow, red, hard,
etc., and the mass
and more is brittle,
and more tinged with red as the content of ferric oxide increases.
The following table gives the results yielded by different varieties
of this mineral on analysis (Pommier) :

46 THEORETICAL STUDY' OF ALUMINIUM, IRON,
Other samples analysed at the Ecole des Mines gave
It is thus evident that bauxite is a mineral of extremely vari-

able composition. Only the purest kinds are utilised industrially,
since, for the manufacture of aluminium sulphate in particular,
freedom from iron is essential
(as far as possible) ;
and it is on
this account that consumers lay down a maximum percentage
of ferric oxide, which must not be exceeded in the goods
supplied by sellers. According to Lacarriere, the bauxite

treated in his works at Noyon contains on an average
The permissible maximum of ferric oxide is fixed at 3 per
cent., and the minimum content of alumina at 60 per cent.

Bauxite was discovered by Berthier, at Baux near Aries, in
the form of grains disseminated in compact chalk it is also found;
at Revest near Toulon, at Allauch (Var), etc.

Far from being of restricted accidental occurrence, bauxite
forms numerous isolated deposits in the cretaceous
system, about
a line drawn from Tarascon to Antibes, for a distance of over
90 miles. It has been discovered and worked by Auge, of Mont-
pelier, at Villevayrac (Herault), and other deposits are known to

exist in Senegal, Calabria, Ireland, Austria, etc.
The mineral is extracted by open workings, or underground
headings, the ground being broken and the bauxite mined by
blasting. The crude product is hand-picked and pulverised before

being used.
Among the numerous applications to which the bauxite is put
are : the manufacture of sodium aluminate, pure alumina, alu-
minium, aluminium sulphate, alums, etc.

25. Aluminates. These minerals belong to the group of
spinels, the general formula of which is 2

O4 MR ;
M = Mg, or
Fe, Zn, Mn; and R = Al, Fe, Mn, Cr, Ti, etc. They usually
crystallise in cubes.
A. SPINEL RUBY (balas ruby) (MgAl 2 O 4 ). This occurs in'
more or less modified octahedra. The fracture is conchoidal the ;
lustre vitreous ;
colour variable, but generally red ; sp. gr. varies
between 3*5 and 3'S ; hardness, 8. It is infusible in the blowpipe
flame ; only slightly soluble in borax ;
soluble in sodium-ammonium
phosphate.
When containing variable quantities of ferric oxide, spinel
ruby is generally black, and is known as ceylanite, pleonaste, cJiloro-
spinel, etc. Associated with chrome, it is yellow or greenish

yellow, and is then termed picotite.
Red, rose, and violet spinels are employed by the jeweller, but
are held in less esteem than the oriental ruby.
Spinels are found in crystalline chalk rocks, gneiss, and

serpentine, and are often associated with the oriental ruby.
Pleonaste is found in the cipolines situated in the gneiss of
Mercus and Arignac, to the north of Tarascon ;
and also as
grains disseminated in herzolite, near Montpelier.

Gahnite is a zinciferous spinel.
B. (G1A1 2 O 4), (syn. Chrysoberyl oriental chry-
CYMOPHANE :
;
solite). A
glucinum aluminate crystallising in the orthorhombic
prism system, generally in the form of tabular crystals of hex-
agonal shape (Fig. 24).
Cymophane is greenish white, verging on grey, in colour ;
trichroic, opalescent, and non-transparent; sp. gr., 375; degree

of hardness, 8' 5.
A green variety, found in Ceylon, is
known as cat's - eye, on account of its
peculiar sheen.
Cymophane is found in granite, gneiss,
FIG. 24. Cymophane. m i ca sc hist, etc.
26. Sulphatic Minerals. A. ALUNOGEN (AU(SO 4) 3 , i8H 2 O),

(syn. : Feather alum, halotrichite, etc.).
Alunogen is monoclinic, and constitutes fibrous or scaly

masses found in solfatara. It is translucent and very soluble ;
the degree of hardness is 1-5 to 2, and the sp. gr. i'6 to i'S.
It has been found in the bitumen deposits at Chamalieres.

B. ALUMIANE consists of anhydrous aluminium sulphate, and
has been found in the Sierra Almagrera mines. It is white, and
occurs as a vitreous mass or in microscopic crystals. The degree
of hardness is 2 to 3, and the sp. gr. 270 to 278.
C. WEBSTERITE, (syn. :
Aluminite, hallite, etc.) (SO 4 (A1 2 O,),
9H 2 O).
This mineral is a hydrated sub-sulphate of aluminium,
occurring as kidney-shaped earthy masses, dull white in colour,

tender, soft to the touch, and biting to the palate. It is soluble
in acids, gives off water when heated, and produces a fine blue
colour in the cobalt nitrate test.
Websterite is met with in the lower tertiary formation, as
New- Haven, etc.
veins or nodules in plastic clay, at Auteuil, Halle,
D. ALUMS. Potassium alum occurs as an efflorescence, or
as fibrous masses, in aluminous schists sodium alum, as fibrous ;
crusts in the sulphur springs of Naples, Milo, etc. ;

ammonium
alum, in lignite, at Tschermig (Bohemia), and in the crater of
Mt. Etna.
E. ALUNITE, (syn. : Alkaline sub-sulphate of- alumina, alum
stone, etc.) (K 2 O, 3A1 2 O 3 4SO 3 ,

6H 2 O). There are four separate
,
types of this mineral : the compact, the porphyroid, the earthy,

and the breccial.
Alunite is a rock of whitish, greyish, yellowish, or reddish
colour, found at La Tolfa near Civita Vecchia at Montioni in ;
the Duchy of Piombino ;

at Mursaly, Munkact, and Tokay in
Hungary; in the islands of Milo, Argentine, and Nipoglio

(Grecian Archipelago) Puy-de-Sancy and Madriat (Auvergne)
;
at ;
Samsoun in Asia Minor, and in Australia.

It is sometimes met with crystallised in rhombohedra, but
more frequently as a light greyish rock, as hard as quartz and

with an average sp. gr.
= 2-5.
In the blowpipe flame alunite decrepitates but declines to fuse ;
it gives off water in a closed tube. The degree of hardness is 3-5

to 4; sp. gr., 2 '6 to 2*75. It is soluble in H SO
2 4,
and is partly
soluble in water after calcination.
At La Tolfa the mineral occurs in limited deposits in the
midst of reddish argillaceous schists of the Jurassic epoch.
The deposit at Madriat is about 1 5 square kilometres
(6 square miles) in area, to the south-east of the Mt. Dore
range (Issoir district), and occurs, disseminated in the form of
balls, kidney-shaped masses, etc., in blood-red clays of the lower
tertiary formation.
The composition of alunite is exceedingly variable, the
following analyses (Pommier) showing the percentage constitution

of the Madriat mineral :
Vauquelin gives the following analysis of Mt. Dore alunite :
Silica 28-40
Sulphuric acid 27-03
Alumina . 31-80
Potash . 579
Ferrous oxide 1-44
Water . 372
Loss i '82
According to Pommier, La Tolfa alunite consists of:
Further analyses by different chemists give the following
composition of alunites from various sources :
*
Including organic matter.
t Magnesia, 0*55 ; lime, 0*28 ; baryta, 0*44 ; organic matter, 0*47.
*
Magnesia, 3-21 lime, 07.
;
t Including 0-13 of barium and unestimated matters.

t Lime, 0-56; magnesia, 0*41 ; magnesium sulphate, 0-9 ; magnesium chloride, 0-03 ;
potassium silicate, 0*31.

The following analyses of the same mineral are given by

Vivien (i), Cordier (2), and Klaproth (3).
For the sake of comparison the mean composition of crude

La Tolfaalunite, treated for aluminium sulphate, is given below :
Potassium sulphate 14-00

Alumina 28-00
Sulphur trioxide . 20-00
Ferric oxide . 2'OO
Alunite is worked on a large scale for the manufacture of

alum and aluminium sulphate, for which purpose it was utilised
as far back as the fifteenth century.
F. LOEWIGITE is also a hydrated sulphate of alumina and

potash, SO 4 K 3(SO 2 ,
4 A1 2 O 2 ), 9H 2 O,
and is found in rounded masses,
resembling compact alunite, at Zabrze (Silesia) and La Tolfa.
Before the blowpipe it exhibits the same characteristics as
alunite. The degree of hardness is 3 to 4 the sp. gr., 2'6 ; ;
fracture, conchoidal.
27. Phosphatic Minerals, A WAVELLITE, (PO 4) 2 , (A1.OH) S ,
4|H 2
O. Wavellite crystallises according to the orthorhombic
system, the crystals being frequently acicular and grouped in
radial, spherical, or hemispherical masses. Occasionally they

occur as small greenish prisms. The colour is variable :
grey,
green, yellow, etc. Cleavage is easy, and the fracture is im-
perfectly conchoidal; degree of hardness, 3-5 to 4; sp. gr., 2-32

to 2-34.
Before the blowpipe wavellite swells up, and gives the

aluminium reaction with cobalt nitrate. It is soluble in acids
and caustic potash, and contains fluorine.
Occurrence, In the fissures of Devonshire clay shales ;

in
the brown haematite contained in Jurassic chalk at Amberg

(Bavaria) ;
in stanniferous veins at Montebras (Creuse), at Saint-
Girons (Ariege) ;
and in America.
B. TURQUOISE, (PO 4)A1 2 (OH) 3 H 2 O. Turquoise exhibits a
microcrystalline structure and a conchoidal or irregular fracture ;
the colour is azure blue, apple green, etc., and the lustre faintly
vitreous. Degree of hardness, 6 ; sp. gr., 2

-
6 to 2 '8. The
powdered mineral is white or greenish, and cupric oxide is
present to the extent of 2 to 5 per cent.

Turquoise is infusible before the blowpipe, to the flame of
which it imparts a green tinge. Heated in a closed tube, it
decrepitates, gives off water, and becomes black or brown. It
is soluble in acids; and, in presence of sodium ammonium

phosphate, furnishes a copper-red bead when heated in the
reducing flame.
Turquoise is used by the jeweller, the most highly esteemed
kind coming from Nichapour in Persia, where it is found in
veins over a clay schist. It has also been found at Holsnitz
(Saxony), Mt. Sinai, Suez, and Simorre (Gers).
28. Silicates. Alumina occurs as a constituent of a large
number of multiple silicates, the most important mineral of this
class being the clays and felspars.
A. CLAYS. This term is applied to a large number of
amorphous substances, derived from the decomposition of other
minerals and bearing a number of distinctive names.
The clays are all hydrated aluminium silicates, more or less
pure, and attackable by acids ;

and are divided into four classes :
I. Clays proper, or potters' clays, prepared by sedimentation.

II. Kaolins, produced by the decomposition, in situ, of
felspathic rocks.
III. Smectic clays, and clays produced by chemical decom-
position.
IV. Boles and ochres.
I. Clays properly so called. The sp. gr. of these bodies varies
between 17 and 27. They form white, grey, yellow, or black
masses, exhibiting an earthy fracture, biting to the tongue, and
mixing with water to a plastic paste. On exposure to dry air
they lose a portion of their moisture, and undergo considerable

shrinkage; the whole of the water is given off on calcination,
the shrinkage increasing with the temperature. Heated to
whiteness, they become sufficiently hard to stand fire.
These clays are acted upon to some extent by boiling hot

hydrochloric and nitric acids, and more extensively by sulphuric
acid. They are infusible before the blowpipe.
The subjoined analyses by Berthier represent typical
examples of these clays :
Dreux clay. Forges clay.

Silica 50-60
Alumina 35 '20 24*00
Ferric oxide 0-40 traces
Water
Marl is clay containing 20 to 25 per cent, of chalk.

II. Kaolin is a very pure clay resulting from the decom-
position of felspar, and is usually mixed with fragments of

the parent rock, mica, quartz, etc., from which it is purified by
levigation.
Pure kaolin is white, unctuous to the touch, and has a

sp. gr. of 2-21 to attacked by hot sulphuric acid,
2-26. It is
but is infusible, or nearly so, before the blowpipe.
Amphigene and emerald may become converted into

kaolin.
The preceding table gives the composition of kaolins from

various sources.
III. Smectic Clays. These constitute beds intercalated among
oolithic and cretaceous rocks. They are translucid at the edges ;
white, brown, or variegated; biting to the tongue; mix with

water to form a short paste ;
and absorb fats. They are
attacked by acids, and fuse to greyish enamel before the

a
blowpipe. The sp. gr. varies between \"j and 2-4.

" "
The fossil flour of the Chinese '
is white and earthy,
exhibiting an aromatic odour; it contains 0*002 per cent, of
nitrogen, and is said to possess alimentary properties.
Halloysite is a compact clay, with translucent edges and a
waxy sheen ;
it is of various colours, and is met with in veins
and deposits.
This clay dissolves to a jelly in acids, infusible before the
blowpipe, and has a sp. gr., 1^92 to 2' 12.

Lithomarge is somewhat similar to halloysite.
Allophane is a variety usually occupying irregular cavities

in beds of limonite and chessylite.
The composition of these clays is shown in the following
table :
IV. Boles and ochres are argillaceous substances containing

a large proportion of ferric oxide, and exhibiting an earthy
fracture. They are opaque, brown, red, or yellow ; biting to the
tongue, and crumbling in water.
Boles and ochres are partly attacked by acids ;
the sp. gr.
varies between 1-6 and 2-5, and the degree of hardness from
i
'5 to 2. Certain of these bodies are employed as pigments,
either in the raw state or when calcined, e.g., sienna, umber,
and sinope.
The composition of two of them is given below :
Alumina
Silica
....
....
Sasebuhl Bole.
20*90
41-90
Amberg Ochre.
14-21
33-23
Ferric oxide . . . 12-20 3776
Magnesia
Water ....
. . . . ...
24-90 J
i"38
3'24
Other bodies that must also be included in this group are

the unctuous, canary yellow, known ashydrated silicate
nontronite, from Nontron (Dordogne), Montmort, and Autun

(Saone - et -
Loire), as well as the chromiferous clays : chrome
ochre (from around Creusot), which imparts a green colour to
triassic arkose rocks, and wolkouskoite, a pigmentary earth
found in .the province of Perm (Russia).
The clays are employed in the production of ceramic ware,
porcelain, etc. ;
the more aluminous kinds, especially kaolin, are
largely utilised for the manufacture of aluminium sulphate.
B. ANDALUSITE (syn. :
Apyrous felspar) is an aluminium
silicate, Al 2 SiO 5 = Al 2 O 3 SiO 2 ,
found in almost square rhomboidal
prisms, covered, and even penetrated, by mica
and disthene, and occurs in crystalline schists.
Andalusite is opaque, and grey or rosy in

colour; a transparent, greenish
-
yellow, poly-
chroic variety is met with in Brazil.
It is unattacked by acids; infusible before

the blowpipe the degree of hardness is 7-5
;
and FlG ;
' 2 5- -Andalusite.
the sp. gr., 3- 1 6 to 3-20. The crystals belong to the ortho-

rhombic prism system.
C. FELSPARS. The felspars occupy an important place
among the constituents of the eruptive rocks. They are colour-
less or white, and only assume a greenish or rose coloration when
they have undergone alteration ; they are often transparent.
The distinctive characteristic of the felspars consists in the
existence of two planes of cleavage, at an angle of 87 to 90.

The degree of hardness is 6 to 7, and the sp. gr. 2'4 to 2 '8.
All felspars are silicates of aluminium and an alkali metal,
such as potassium or sodium, or an alkaline earth, e.g., lime
and occasionally barium. The proportion of the oxygen com-
bined with the alumina is always as 3 : i

compared with that
attached to the other bases. As for the oxygen in the silica,
its proportion is essentially characteristic of the different kinds

of felspar.
The entire series of felspars may be regarded as polysilicates,
each member of which differs from its preceding neighbour by
one additional molecule of silica.
The following table gives a classification of the felspars in

the order of their increasing richness in silica :
Ratio of Oxygen.
RO A1 2 O., SiO 2
Anorthite :
3 :
4
Labradorite :
3 : 6
Andesine :
3 = 8
Oligoclase 3 : 10
Albite . :
3 : 12
I. Anorthite (Si 2 O 8 Al 2 Ca). The only occurrence of this felspar

as decided crystals is in the volcanic rocks in certain localities,
such as the ejected blocks of Somma, the lavas of Iceland, in Java,
etc. In France it is met with as laminar masses in certain
galbros (St. Clement, Puy -de -

Dome), pyroxerite (Roguedon,
Morbihan), or diorite (Corsican orbicular diorite). Some varieties
are rose or rosy grey in colour.

This felspar is completely attacked by acids, a deposit of
silica being left. Before the blowpipe it fuses to a vesicular
glass. The degree of hardness is 6 the sp. gr., 2*69 to 2*75 and ; ;
the crystals belong to the anorthic prism type, mt= 120 30';
pm =111 40' ; // = 114 7'.
Labradorite (Si 3 O 10 Al 2 Ca) is but very rarely met with in

II.
the form of crystals, being generally found as white lamellar

masses in diorites, diabases, euphotides, norites, etc. The finest
specimens come from Labrador, where they form a rock with

hypersthene and amphibole.
The crystalline form of labradorite is the anorthic prism,
;;// = i 2 T 3 7' ; pm = i i o .5
o' ; -pa = 98 5 8'. Hydrochloric acid
attacks it with difficulty. Before the blowpipe it fuses quickly to
a colourless glass. The sp; gr. is 2*67 to 2-76.
III. Andesine (Si 4 O 12 Al 2 R) (R = Ca or Na 2 ).
This substance
forms milk-white crystals in Esterel blue porphyry (dacite), and

laminar masses in Autun gneiss. The crystalline form is that of
the anorthic prism, mt = 120; pg^ = 86 I o' ; pt = 1 1
5.
It is imperfectly attacked by acids, and is somewhat infusible
before the blowpipe, the edges alone melting to a milky glass.
IV. Oligoclase (Si 5 O 14 Al Na2 2)
is
rarely met with in the
state of crystals, being generally found as white or greenish
laminar masses, in granite, syenite, porphyry,
basalt, etc.
It fuses with difficulty before the blow-
pipe, and is almost unacted upon by acids.

The degree of hardness is 6; sp. gr., 2^63 to
273; and the crystalline form that of the
anorthic prism, mt = I 20 1 2' ; ^=120 FIG. 26. Oligoclase.
pg = 86
l
24'; pt= 114 40'; 10'.
V. Albite (Si 6 O 16 Al 2 Na 2 ). This felspar occurs as milky-white

crystals with vitreous lustre, and nearly always macleated. The
maclea known as albite exhibits the
appearance of a characteristic trough-
like depression formed by the juxta-
position of two faces (/) sloping in
opposite directions.
Albite frequently occurs as veins
in granite, gneiss, diorite, etc. It is
unattacked by acids, and fuses to a

vesicular glass before the blowpipe, FIGS. 27 and 28. Albite.
the flame acquiring a yellow tinge, The degree of hardness

varies from 6 to 6-5, and the sp. gr. between 2-54 and 2-64.
The crystalline form is that of the anorthic prism, mt=i2O
47'; pm= 1 10 50' //= 1 14 52'; pg = 86 24'.
l
;
VI. Orthose (Si 6 O 16 Al 2 K 2 ) is frequently met with as simple or

macleated crystals in granites and microgranulites. The most
general form of maclea is that kno\vn as Karlsbad, wherein two
crystals are joined along their plane of symmetry, the one crystal
I 80 about the vertical
being fixed, whilst the second is turned
edge of the prism.
Orthose is often encountered in flesh-coloured, rose-red, or
58 THEORETICAL STUDY OF ALUMINIUM, IRON, ETC.
white laminar or granular masses, and constitutes an essential

element of granite, pegmatite, syenite, gneiss, porphyry, etc.
Occasionally crystals of albite are found deposited regularly
on those of orthose, or vice versA. The orthose of volcanic rocks
is always transparent.
FIG. 29. FIG. 30. FIG. 31. FIG. 32.

Orthose (adular). Orthose. Orthose maclea. Orthose maclea.
In common with other felspars, orthose readily undergoes
decomposition, potassium silicate being dissolved out by water,

and kaolin left as the final product.
Orthose is unattacked by acids, and is fused, with difficulty,
to a vesicular glass. The degree of hardness is 6 to 6-5, and the
sp. gr. 2'44 to 2*62. The crystalline form is that of the clino-
rhombic prism, mm 1 1 8 48' ; pa
1
=129 40'.
The felspars are largely utilised in the ceramic industry and
for porcelain, and some are employed for the preparation of alum.
CHAPTER II
IRON, AND IRON COMPOUNDS
i. IRON (Fe= 56)
29. Preparation in the Laboratory. The preparation of pure

iron in the laboratory will alone be entered into here the ;
reader desirous of studying the metallurgy of this metal being

referred to special works on the subject, wherein a full description
is given of the numerous and interesting methods for extracting
iron from its ores, and refining and converting the metal into the
various products required for use in the industrial arts. In the
present work it is our purpose to mention that the

sufficient for
basis of the metallurgy of iron is the reduction of the various oxide
ores, by means of carbon, in special forms of apparatus.

To obtain chemically pure iron in the laboratory, the purest
commercial form of iron, namely piano wire, may be treated with
ferric oxide and a flux, such as glass, in a refractory crucible
exposed to the heat of a blast furnace. In this manner a silver-

white bead of metal is obtained.
It is, however, always more convenient to reduce the oxide or
chloride of iron by means of hydrogen. By calcining anhydrous
ferrous chloride (which can easily be obtained pure) in a current
of pure hydrogen, HC1 is liberated and pure iron left behind as
cubic crystals.
When effected at a high temperature the reduction of ferric
oxide in hydrogen yields very finely divided metallic iron. At a
lower temperature the product forms a very finely divided mass,
shown by Moissan to consist of ferrous oxide. This is the pro-
duct known by the name of pyrophoric iron.
Again, pure iron may be easily prepared by the action of

heat on precipitated ferrous oxalate, C 2 O 4 Fe = Fe+ 2CO 2 .
30. Properties of Iron. A. PHYSICAL PROPERTIES. Iron

is bluish grey in colour and of metallic lustre, with a slight
metallic odour and taste. It is highly tenacious, an iron wire
i mm. in diameter requiring a force of *5 5 kilos to produce
rupture. The fracture is granular, and the brilliancy and fineness

of grain of the metal are
in proportion to its purity. When
chilled it becomes
brittle, but regains its properties on re-heating.
It is malleable and ductile, and may be forged with ease whether
cold or hot. The mean sp. gr. is 7'8, but varies according to the
method of preparation employed. Thus the sp. gr. of cast iron
is 7*5, that of wrought iron being 7*4 to 7-9. The melting point
is about 1500, but before this point is reached the metal be-
comes soft enough for two surfaces to unite by welding. It is
the hardest of the metals in general use, but is marked by glass.

Its conductive capacity for heat is represented by 119, compared
with silver =1000; and its electrical conductivity at 20 C. =
14*44, that of silver at o being taken as 1000.
Molten iron crystallises in cubes or octahedra, on which
account it becomes brittle. Hammering whilst hot prevents
it assuming a crystalline structure ; nevertheless, it regains this
condition by degrees if, after being hammered, it is subjected to
repeated vibration.
Iron is
magnetic, but loses this property towards 800 C. It
is attracted by the magnet, and itself behaves as a magnet so long

as contact is maintained, but ceases to act as such when removed.
Steel, on the other hand, can be permanently magnetised.
At a red heat iron is permeable by gases, notably by
hydrogen, and absorbs them in considerable quantity. It always
contains about 12 times its own volume of gas, which it
gradually loses when heated

in a vacuum. The proportion of
gas is much
higher in the case of electrolytic iron.
With 2 to 5 per cent, of carbon, iron forms cast iron, melting
at about 1250; but when the
proportion of carbon is lower,
namely 07 to 2 per cent., it becomes steel, the fusing point of
which is about 1
400 C.
B. CHEMICAL PROPERTIES. Iron is unalterable in dry air at

the ordinary temperature, but at red heat it absorbs oxygen, and
is converted into the black, or magnetic, oxide, Fe3 O 4 . This
combustion goes on very briskly in pure oxygen. In moist air
iron undergoes slow oxidation, though only after a considerable
time, the metal becoming coated with a layer of hydroxide,

known as rust. Once formed, this hydroxide constitutes, with
the metal, a voltaic couple, in consequence of which the
oxidation proceeds more rapidly. In order to protect the metal
from this attack it is customary to cover it with a layer of
paint, or preferably zinc (galvanised iron), tin (tinned iron),
enamel, etc.
At a red heat iron decomposes water, liberating the hydrogen,

and itself becoming converted into Fe 3 O 4 .
Iron unites with a large number of elements. With metals it
forms alloys ;
the metalloids of the chlorine group attack it at
the ordinary temperature, and at a high temperature it combines
with sulphur, a somewhat fusible sulphide being produced.
Iron decomposes ammonia at red heat, and forms an iron
nitride, Fe5 N 2 . A large number of dilute acids are also decom-
posed by iron, with evolution of hydrogen and formation of the
corresponding iron salt.
Under the influence of heat, concentrated sulphuric acid is
decomposed by sulphur dioxide being liberated.

iron, Concen-
trated fuming nitric acid, however, not only does not attack iron,
but also renders the metal proof against the action of weaker acid.
In this state the iron is said to have become passive. According
to some authorities, this condition is attributable to the formation
of a stratum of condensed nitrogen dioxide at the surface of the
metal as a kind of gaseous sheath. Others, however, regard this
explanation as erroneous, and ascribe the passivity of the iron to
a deposit of ferro-ferric oxide, which protects the metal from
ulterior attack. Nevertheless, this condition of passivity is
merely apparent, since in course of time passive iron dissolves,

without any liberation of gas.
However this may be, if the iron rendered passive by
immersion in concentrated acid is afterwards placed in weak acid
and touched with a copper wire, the passivity disappears and the
metal is attacked energetically.
Very dilute nitric acid dissolves iron without any liberation
of gas. In this case the nascent hydrogen produced is converted,
by the excess of nitric acid, into ammonia, which remains in
solution as ammonium nitrate.
Carbon dioxide in aqueous solution reacts upon iron, forming

iron carbonate and hydrogen.
The heat of combination of iron with oxygen, and the
halogens, has been determined by Berthelot, who gives the
following values :
Oxygen. Chlorine. Bromine. Iodine.
34,100 cal. 4i,ioocal. 35,000 cal. 20,000 cal.
In the case of carbon the combination is endothermic, and the

reaction is consequently comparable to solution. With manganese
heat is disengaged.
C. ATOMICITY OF IRON. Iron is capable of entering into
combination in several states of basicity, and gives rise to two
perfectly distinct series of compounds, corresponding to two
different valencies for the metal. In the one set the iron plays
the part of a diatomic element, and is represented by the symbol
Fe" =56, known by the name of ferrosum whilst in the other ;
case the metal acts as a hexatomic element (Fe2 ) VI = ferricum.

There is no need to dilate upon the diatomicity of ferrous
iron, this condition being sufficiently proved by the existence of
ferrous chloride, Fe"Cl 2 wherein the metal
,
is combined with 2
atoms of the monovalent element chlorine. To this series of
compounds the term ferrous compounds is applied.

So far as ferricum, (Fe 2 ) VI =ii2, is concerned, this form
represents a double atom of iron. It may be asked why the
doubling of the iron atom should be regarded as necessary, and

whether it would not be simpler to consider ferricum as trivalent
Fe" =56.
1
And, in fact, the analysis of ferric chloride gives
corresponding to Fe Cl 3 = 162*5.
IH
figures Nevertheless, an
examination of the vapour density of this compound as com-
pared with hydrogen, namely 164-4 (Deville and Troost), leads to
the conclusion that the molecular weight is 325, which corre-
VI IU
spends to the formula Fe2 Cl 6 and not Fe Cl 3 ,
In fact, the cal- .
culated vapour density works out to 162' 5, a value approximating

to that determined by Deville and Troost. One is therefore
compelled to acknowledge the existence of the double atom of

VI
iron, Fe.2 constituting a hexatomic couple.
,
Once established,
this can be explained in other ways.
fact For instance, in iron
pyrites or iron disulphide the metal seems to play the part of a
tetratomic element. This, however, is merely hypothetical, since
the tetravalence of iron could only be established by the existence
of a compound of I atom of the metal with 4 atoms of a
monovalent element. Nevertheless, if we admit this tetravalence,
\ve can equally acknowledge the possibility of one such atom of
iron coalescing with a similar one to form the hexavalent group
IV v VI
(Fe Fe' ) .
This is equivalent to supposing that the diatomic iron of ferrous

chloride, become tetravalent under the influence of an excess of
chlorine, exchanges with itself the two valencies corresponding to

the 4th atom of chlorine of each of the 2 molecules of the tetra-
chloride, which is therefore not formed. Ferric chloride is therefore

Fe lv
]
FeCl 3 FeCl 3 = =Fe 2 Cl 6 .
|
[Cl 6
Fe IV J
2. COMPOUNDS OF IRON
31. Fluorides of Iron. A. FERROUS FLUORIDES. I. Fer-

rous Fluoride(FeF 2 ). This
prepared bysalt is the action of iron
on HF, and forms small white crystals, slightly soluble in water,
but more freely so in an excess of acid.
In hydrofluoric acid, sp. gr. 1*07, iron dissolves slowly, form-
ing at the end of several days a green solution which, on evapora-

tion, furnishes green prisms, adhering firmly to the walls of the
basin and corresponding to the formula

FeF 2 ,
8 HO.
At a high temperature this salt melts in its own water of
crystallisation, and subsequently dries to a white saline mass if
air has been excluded during the operation. On exposure to the

air, HF is liberated and a mixture of ferric oxide and ferric
fluoride is left. On adding nitric acid to a solution of ferrous
fluoride a colourless liquid is formed, which, when concentrated,

yields a white crystalline mass composed of a mixture of ferric
nitrate and ferric fluoride.
II. Ferro-potassic Fluoride (K 2 FeF 4 ) is soluble, and crystallises

in greenish granular crystals.
III. Ferrous Fluosilicate (FeF 2 SiF4) ,
is
prepared by dissolving
iron in hydrofluosilicic acid. It is very soluble, and crystallises
with difficulty in bluish-green, regular hexagonal prisms.
B. FERRIC FLUORIDES. I. Ferric Fluoride (Fe 2 F6 ). To
prepare this compound, calcined ferric oxide is treated with an
excess of HF. The mixture, which heats spontaneously, is then
placed in a large platinum crucible, the lower portion of which
is raised to a white heat. The fused mass is of a reddish colour,
probably due to contained ferric oxide.

Ferric fluoride is isomorphous with aluminium fluoride, and is
just as volatile, though not so fusible, as the latter.

Hydrated ferric fluoride is obtained by oxidising ferrous
fluoride with nitric acid in presence of HF, the resulting solution
being easy to crystallise. It may also be prepared by dissolving

ferric hydrate in hydrofluoric acid.
Ferric fluoride forms colourless or yellowish crystals, only

slightly soluble in water, and insoluble in alcohol, their com-
position being Fe 2 F 6 , 9H 2
O. At 100 C. it parts with one-third of
its water and becomes Fe 2 F 6 ,
6H O 2 ;
and on being dehydrated
completely, by the application of greater heat, it liberates hydro-
fluoric acid concurrently with water.
Ferric fluoride exhibits the remarkable property of not under-
going complete decomposition under the influence of alkalis.

Thus an addition of ammonia gives a yellow precipitate, from
which caustic potash removes a small quantity of hydrofluoric
acid, but not the whole.
This salt exhibits a constant composition, which corresponds
to the formula
II. Ferri-potassium Fluorides. The salt Fe.2 F 6 6KF

,
is formed
in presence of an excess of potassium fluoride, whereas if ferric
fluoride be in excess the resulting compound is Fe 2 F 6 /J.KF. ,
Both these salts, which are crystalline and soluble, were described
by Berzelius.
III. Ferri-sodium Fluoride. The formula of this salt is
Fe 2 F 6 4NaF +
,
H 2 O, and it is prepared by mixing solutions
of ferric chloride and sodium fluoride, a precipitate, soluble in
an excess of ferric chloride, being formed. On adding alcohol
to the solution the salt
Fe 2 F 6 4 NaF,
,
HO 2
is thrown down as yellow flakes.
The iron in this compound cannot be detected by potassium

thiocyanate ;
and moreover, the same reagent, when coloured red
by a ferric salt, is decolorised on the addition of an alkali
fluoride, in consequence of the formation of a compound of

similar type to the above.
IV. Ferri- ammonium Fluoride (Fe 2 F 6 ,

6NH 4 F). This salt
was described by Marignac. It is but sparingly soluble in
water, and crystallises in small, very lustrous regular octahedra,

which do not lose in weight at 1 00 C.
V. Ferric Fluosilicate is obtained by dissolving ferric hydrate

in hydrofluosilicic acid.
32. Chlorides of Iron. A. FERROUS CHLORIDES.

1. Ferrous Chloride (FeCl 2 ). This is prepared by passing a
gas over red hot iron.
current of acid -
dry hydrochloric
Hydrogen is liberated, and crystalline needles of ferrous chloride
sublime in the cold parts of the apparatus. Another method
is to heat sal ammoniac with iron filings,
(ammonium chloride)
ferrous chloride being left behind as a residue.
When ferric chloride is carefully heated in a current of
hydrogen, well formed crystals of ferrous chloride are obtained.

Ferrous chloride is a white, slightly yellowish salt, volatile,
readily soluble in water and also soluble in alcohol.
Whenheated in a current of hydrogen it furnishes HC1,

and cubical crystals of iron are left. In a current of oxygen
it forms ferric chloride, chlorine being liberated.
5
Hydrated ferrous chloride (FeCL, 4H 2 O) is prepared by dis-
solving the anhydrous chloride in water, or by acting on iron
with hydrochloric acid. By this means a green solution is

obtained which, on concentration, furnishes the hydrated chloride
in the form of bulky green crystals, derived from the clinorhombic
prism.
Ferrous chloride is less soluble in HC1 than in water, so
that, when a current of HC1 gas is passed through the aqueous
solution of this salt, crystals are deposited. If anhydrous ferrous
chloride be dissolved in hot concentrated hydrochloric acid, and
the solution left to crystallise, fine transparent needles corre-
sponding to the formula FeCl 2 2H 2 O are obtained. ,
When strongly heated, FeCl 2 4H 2 O melts in its water of ,
be continued, gradually loses its

crystallisation, and, if the heating
moisture, a white residue being finally left, provided air has been
excluded during the operation. In contact with air, however,
ferric chloride is formed, which is carried away by the liberated
water vapour, and leaves behind a green fusible mass. This

yields up ferrous chloride to water, and a residue of ferrous
oxide, rapidly oxidising in the air, is left.
Ferrous chloride solution absorbs nitrogen dioxide to a

much greater extent than the dry salt; and the alcoholic
solution absorbs a still larger quantity of this oxide.
Gaseous ammonia reacts at a red heat on ferrous chloride,
with formation of ferric nitride, Fe5 N 2 . In the cold, ferrous
chloride absorbs NH 3 and forms FeCl 2 ,
6NH 3. Ferrous chloride
is insoluble in ether.
II. Ferro-potassium Chloride (FeCl 2 2KC1). ,
Ferrous chloride
and potassium chloride readily crystallise together, to furnish the
compound FeCl 2 2KC1, when a mixture containing in solution
,
suitable proportions of these two salts is left to cool.

III. Ferro-ammonium Chloride resembles the foregoing salt,
and is
prepared in the same manner.
IV. Intermediate Ferrous Chloride. Hensgen prepared the
chloride Fe 3 CL, 5H 2 O, in fine pale green needles, by dissolving
ferrous sulphate in HC1, and saturating the mixture with gaseous
hydrochloric acid in contact with air.
V. Ferro -ferric Chloride. According to Lefort, the com-

pound Fe 3 Cl 4 ,
i 8 HO
2
is obtained when a solution of ferro-ferric
oxide in HC1 is evaporated over f^SO^ and CaO, the latter
substance being employed to absorb the excess of HC1.
B. FERRIC CHLORIDE. I. Anhydrous Ferric Chloride
(Fe 2 Cl 6 = 325). This

prepared by passing a current of
salt is
dry chlorine over red-hot iron. We have seen that, to obtain

ferrous chloride, iron is treated with HC1 ;
and these two
methods are general. When any metal forms two compounds
with chlorine, the one containing the smaller proportion of that
element is obtained by the action of HC1, the richer by the
action of chlorine.
When sublimed, ferric chloride assumes the form of tabular
hexagonal crystals, dark red in colour with a greenish reflection.
The vapour density of this body is i62'5, Deville and Troost
having found the value 164-4 compared with H = I.
Ferric chloride is soluble in water, with evolution of heat,
different hydrates being formed. Franz has compiled the
following table, showing the density of the aqueous solutions
of this salt at I7'5C:
soluble in alcohol and ether, but the solutions are

It is also
reacts
unstable, and on exposure to light liberate chlorine (which
on the solvent) and furnish ferrous chloride.
At a red heat, ferric chloride is decomposed by steam,
hydrochloric acid and ferric oxide being formed. This reaction,
which can also be effected in a closed vessel, was utilised by

SeYiarmont for the production of crystalline ferric oxide. When
treated in oxygen it is converted into ferric oxide, chlorine being
liberated.
Anhydrous ferric chloride readily combines with a number

of different substances. With ammonia it forms a red mass,
Fe 2 Cl e ,
2NH 3 ,
soluble in water and easily decomposed by heat.
With phosphorus pentachloride it gives a brown, fusible mass,

corresponding to the formula Fe 2 Cl 6 2PC1 5 and with nitroxyl , ;
chloride yields a dark, deliquescent mass, Fe 2 Cl 6 2NOC1.

,
II. Hydrated Ferric Chloride may be prepared by the action

of water on the anhydrous chloride ;
or by treating a solution of
ferrous chloride with chlorine; or again, by acting on ferrous
chloride with nitric acid or nitrohydrochloric acid.

When ferric hydrate is acted on by HC1, a solution of
ferric chloride containing an excess of dissolved ferric hydrate
is obtained.
On concentration, the solution of ferric chloride deposits
rhombohedral plates of a handsome yellow colour, containing
6 or 4 molecules of water Fe 2 Cl 6 6H 2 O or Fe2 Cl c 4H 2 O.
:
, ,
The first of these salts melts at 31, and the second at 35'5C.
On slowly evaporating a dilute solution of ferric chloride, the
firstcrystals formed respond to the formula Fe 2 Cl 6 I2H 2 O. ,
According to A. Vogel, dissolved ferric chloride is to a small]

extent volatilised below boiling point. With ether this volatilisa-
tion takes place at about 30 C.
On heating a solution of this salt, diluted to such an extent
as to be almost colourless, assumes a deep coloration beyond
it
27 C., without parting with hydrochloric acid. Its properties, how-

ever, will be found to have undergone considerable modification,
the precipitate formed with potassium
ferrocyanide being now
only of a pale bluish-white shade, whilst saline solutions throw
down a precipitate of modified ferric hydrate. When dialysed, .
the solution divides into soluble hydrate and

hydrochloric acid.
If, after the modified ferric hydrate has been
precipitated by
sodium chloride, it is left at rest for 24 hours before filtering, it
will no longer dissolve in water.

Under the influence of heat the solution issplit up into free

" "
hydrochloric acid and the colloid hydrate of Graham.
The more dilute the solution of ferric chloride, the more
readily is it dissociated under the influence of heat ;
the products
vary according to the temperature, duration of heating, and con-

centration of the solution under examination. Thus a 40 per cent.
solution is not decomposed below 100 C. A 32 per cent, solu-
tion furnishes a yellow oxychloride at I2OC., and brown ferric
oxide at 140 C. An 80 per cent, solution yields an oxychloride

of variable composition at 1 1 o C. ;
whilst a 40 per cent, solution
gradually deepens in colour up to 90 C., and then furnishes an

oxychloride. Before precipitation occurs these solutions contain
"
Graham's colloid hydrate," which can be separated by means of
NaCl.
If the heat has not been too great or too prolonged, the solu-
tions containing between 4 and 32 per cent, of ferric chloride
will regain their original condition on cooling. This reversion

is more gradual in the case of I to 4 per cent, solutions, and in-
complete in solutions below I

per cent, strength.
Solutions containing TV per cent, of Fe 2 Cl 6 decompose when
exposed to light, even at 5 per cent, solutions are
or 6 C., but
stable under the same conditions at the ordinary temperature.
The decomposition of these solutions is attended by an alteration,

though slight, in their specific gravity.
When a solution of Fe 2 Cl 6 is heated for some time at 1 00 C.
the soluble hydrated oxide is converted into a form insoluble in
weak acids, but dissolving in water to a solution which is trans-
parent by transmitted light, but turbid when viewed by reflected
light. Heated to 250 to 300 under pressure, the anhydrous

oxide is formed.
In solution in alcohol, even when diluted, Fe 2 Cl 6 does not
undergo any appreciable dissociation.
When an acid solution of this salt is subjected to electrolysis,
ferrous chloride is obtained at the negative pole, whilst chlorine

collects at the positive pole.
On treating pure neutral Fe 2 Cl 6 with sodium sulphite solution

in equal molecular proportions, a very intense, but transitory,
7O THEORETICAL STUDY OF ALUMINIUM, IRON,
blood-red coloration is immediately produced, which is attributed
by Buignet to the formation of a sulphite of ferric oxide.

Ferric chloride is reduced by most reducing agents : nascent
hydrogen, metals, etc. Even platinum is somewhat readily

attacked by Fe 2 Cl 6 probably by the chlorine, which, according to
,
Personne, is always liberated when a sufficiently strong solution

of this salt is heated to boiling.
Sulphuretted hydrogen, sulphur dioxide, and stannous chloride

also reduce Fe2 Cl 6 .
On agitating a solution of this salt with ether, the latter
assumes a yellow colour and extracts the Fe.2 Cl 6 from the

water.
Ferric chloride is largely used as a haemostatic, and may be
administered internally without risk. It has been recommended
in the treatment of croup, and is used for purifying waste
waters.
III. Compounds with other Chlorides. According to Hensgen,
the salt Fe2 Cl 6 2NH 4 C1, 2H 2 O is formed when ferro-ammonium
,
sulphate is treated with HC1 in contact with air.
Fe 2 Cl 6 forms with PtCl 4 a compound (Fe2 Cl 6 2PtCl 4 24H 2 O)

, ,
which crystallises in deliquescent clinorhombic prisms, and parts

with ioH 2 O at iooC.
IV. Oxychlorides of Iron. These compounds are numerous,
and are divided into 2 series, namely soluble and insoluble oxy-
chlorides, corresponding respectively to compounds of the soluble
or insoluble hydrate with Fe 2 Cl 6 .
When left for some time, solutions of ferric chloride gradually

deposit a yellow-brown powder, Fe 2 Cl 6 6Fe2 O 3
, , 9H 2 O, which on
gentle calcination in air is converted into Fe2 Cl 6 3Fe 2 O 3 , ,
H 2 O.
If a concentrated solution of ferrous chloride be oxidised by
means of the theoretical quantity of nitric acid in presence of an
insufficiency ofHC1, the solution being heated to 100 C. and the
nitric added by degrees, a very brisk reaction is set up
acid ;
the liquid, which was initially black, becomes

yellow and turbid,
and yields on nitration a yellow precipitate remarkable for the
tenacity with which it retains chlorine. This precipitate is in-
soluble in water, sparingly soluble in HC1, and varies in com-
AND COMPOUNDS OF THESE METALS 7 1
position according to the proportions of ingredients taken. When

the amount of HC1 employed is about one-third of that theoreti-
cally necessary to form Fe2 Cl 6 the precipitate consists of

,
Fe 2 CI 6 i2Fe2 O 3)
,
and on digestion with water is transformed into the still more

basic oxychloride
Fe 2 Cl 6 i;Fe2 , 3.
When digested for 24 hours with ammonia the composition

becomes
Fe 2 Cl 6) !44Fe 2 3,
and after boiling with NH 3

still retains o 85 per
-
cent, of Fe2 Cl 6 .
The majority of the oxychlorides are prepared by dissolving
freshly precipitated ferric hydrate in a solution of Fe2 Cl 6 . At

first, solution goes on rapidly, but when a certain point is reached
the operation slackens and the liquid sets to a dark coloured
jelly, which is soluble in water and contains

Fe 2 Cl C) !2Fe 2 3.
By the addition of water a further quantity of hydrate can be
brought into solution, the liquid then containing Fe 2 Cl 6 2oFe 2 O 3 ,
according to Bechamp,' or even Fe 2 Cl 6 23H 2 O according to ,
Ordway.
The oxychlorides Fe 2 Cl 6 5Fe 2 O 3 to Fe 2 Cl 6 ioH 2 O may
, ,
be dried without losing their solubility, whereas the others are
thereby rendered insoluble. These solutions exhibit an acid re-

action, and are precipitable by the addition of a salt or HC1.
They are also precipitated by 3

NH
and then furnish hydrate
,
ferric
free from chlorine, whereas the insoluble oxychlorides, even when

boiled for a long time with 3 always
NH
retain a little chlorine.
,
This fact is ascribed by Bechamp to a difference of molecular

condition.
By digesting freshly precipitated chromium hydrate with a

solution of Fe 2 Cl 6 for several months, Be"champ obtained a soluble
compound of ferric chloride and chromium oxide, Fe2 Cl 6 4Cr2 O 3 ,
.
The oxychlorides of iron have been principally investigated by

Bechamp and Ordway.
33. Chlorates of Iron. A. FERROUS CHLORATE (ClO 3) 2 Fe.
This salt is prepared from barium chlorate and ferrous sulphate
by double decomposition. Its solution is split up, by boiling, into

chlorine and ferric chlorate.
B. FERRIC CHLORATE (ClO 3) 6 Fe 2 VI In addition to the pre-
.
ceding reaction, this salt may also be formed by the action of

chlorine on ferrous hydrate suspended in water, a yellowish-red
liquid being thereby obtained.

C. FERROUS PERCHLORATE, (ClO 4 ) 2 Fe, may be prepared by
dissolving iron in perchloric acid, or by double decomposition.
It crystallises in small greenish, deliquescent crystals containing
6H 2 O. The solution oxidises on exposure to air, and deposits a
basic ferric perchlorate. It decomposes above 100 C.
D. FERRIC PERCHLORATE (ClO 4 ) 6 Fe 2 VI . This has only been

obtained in a state of solution.
34. Bromides of Iron. A. FERROUS BROMIDE (FeBr 2 ) is
obtained by treating an excess of iron with bromine. In the
anhydrous condition it forms a light yellow, fusible, lamellar mass

dissolving in water to a greenish solution, from which crystals of
FeBr2 are deposited on concentration. Under the influence of
air this solution throws down an insoluble yellow oxybromide.
B. FERRIC BROMIDES. I. Ferric Bromide (Fe 2 Br6 ). This
salt is when iron is treated with an excess of
obtained in solution
bromide ;
and in the anhydrous condition by treating hot iron
with bromine vapour, the ferric bromide subliming in the latter
case as dark red scales.
II. Oxybromides are formed under the same conditions as the
oxychlorides.
Bechamp obtained Fe2 Br6 i4Fe 2 O 3
, by dissolving ferric
hydrate in a solution of ferric bromide.

Like the oxychlorides, the solutions of the oxybromides are
deep red, and possess considerable tinctorial power.
35. Bromates of Iron. A. FERROUS BROMATE (BrO 3 Fe).
To prepare this salt, ferrous carbonate is dissolved in bromic acid,
the bromate crystallising in regular octahedra when the solution
is evaporated in vacua. It is of low stability, and continually
manifests a tendency to decompose, with formation of a ferric
sub-salt.
B. FERRIC BROMATE (BrO 3 ) 6 Fe 2

VI
.
Freshly precipitated
ferric hydrate will dissolve in dilute bromic acid to form ferric

bromate. The solution refuses to crystallise, and readily decom-
poses with formation of a basic salt.
36. Iodides of Iron. A. FERROUS IODIDE (FeI 2 ). When a

mixture of iron filings and iodine is rapidly heated to redness, and
a further addition of iodine made on the attainment of that tem-
perature, a fused mass containing periodide is obtained, which

suddenly liberates iodine at a particular stage of cooling, and
leaves a grey lamellar mass of ferrous iodide.
Another method of preparation is by gradually adding iodine
to iron filings under water, a paler green, readily oxidisable solu-
tion being obtained, which can only be concentrated in a current
of hydrogen. Under these conditions a deposit of FeI 2 4-H 2 ,

O
(sp. gr. 2-873) is formed. In a pure anhydrous state this salt
is white and pulverulent. When heated in the air it loses iodine
and leaves a magnetic residue on exposure to moist ;
air it turns
greenish, and assumes a crystalline texture.

B. FERRIC IODIDE (Fe 2 I 6 ) is prepared by treating ferric
hydrate with hydriodic acid, or by acting on iron with an excess

of iodine. It forms a brown, uncrystallisable solution.
37. lodates of Iron. A. FERROUS IODATE, (IO 3 ) 2 Fe, is a

slightly soluble light red by double decom-
precipitate, obtained
position.
B. FERRIC IODATE (IO 3 ) 6 Fe 2 VI . Obtained in the form of a
yellow precipitate by heating a mixture of ferrous chloride and an
alkali iodide in presence of an excess of nitric acid.
C. FERRIC PERIODATE (I 2 O 13 Fe 2,
2 1 H 2 O).
This salt may be
obtained, as a brown-yellow precipitate, from periodic acid and

ferric hydrate ;
but not by double decomposition, because in the
latter event it is transformed into the iodate.
38. Oxides of Iron. A. IRON SUB-OXIDE. According to
Marchand, this is the product formed when iron wire is fused in
the oxyhydrogen blowpipe flame. It is a fusible, malleable, black
oxide, soluble with some difficulty in HC1 and H SO2 4.
Marchand
found it to contain a constant proportion of 679 per cent, of
oxygen. According to Dusart, a sub-oxide of iron is also formed

when ferric oxide is reduced by hydrogen; but Moissan, who
has carefully investigated this reduction, is unable to confirm the
alleged result.
B. FERROUS OXIDE. I. Anhydrous Ferrous Oxide (FeO).
This oxide was prepared by Debray by passing a mixture of

equal volumes of carbon monoxide and carbon dioxide over red-
hot ferric oxide.
It is also obtained as a crystalline, black, lustrous, magnetic
substance when carbon dioxide is reduced by means of metallic

iron. On calcination in air, or in a current of steam, this
anhydrous oxide is converted into magnetic oxide, Fe 3 O 4 .
A
pyrophoric ferrous oxide capable of decomposing water is
obtained by heating the oxalate to 500 C. in a current of hydro-
gen. At 350 C. ferro-ferric oxide is produced, and metallic iron

atbetween 500 and 700 C.
II. Ferrous Hydrate. When a ferrous salt is precipitated by
a base, white flakes of ferrous hydrate are formed. This com-
pound is
very unstable in air, and cannot be washed and dried
without undergoing alteration.
Ferrous hydrate is slightly soluble in water, the solution
exhibiting a pronounced ferruginous taste, an alkaline reaction,

and a tendency to soon become turbid on exposure to the air.
When treated with KHO at boiling temperature this hydrate

turns black, the magnetic oxide being formed, and hydrogen
liberated.
C. FERRO-FERRIC OXIDE, or MAGNETIC OXIDE OF IRON.

I. Anhydrous Ferro-ferric Oxide (FeÂ, FeO = Fe2 vl Fe"O 4 = Fe 3 O 4 ).
The crude formula employed for this oxide is Fe 3 O 4 but
,
it may
be regarded as a combination of ferric oxide with ferrous oxide,
i.e. as a ferrite of ferrous oxide. Again, it may be considered as
an intermediate oxide between FeO and Fe 2 O 3 and for this ,
reason will not be described among the ferrites.
Fe3 O 4 is found in terrestrial rocks, either in the amorphous

state or crystallised in octahedra, and occurs in meteorites. It
forms the best iron ore, is characterised

by magnetic properties, its
and constitutes the natural loadstone met with very abundantly

in Sweden and Norway, where it occurs in
compact masses
endowed with a metallic lustre, and of sp. gr. 5*09.
This oxide may be produced under various conditions, e.g., by

the combustion of iron in an excess of oxygen ; or, as a dense
black powder, by fusing ferrous chloride with dry sodium car-
bonate at a low temperature. It is also obtained by roasting
iron in the air, by the action of boiling water on ferrous hydrate,
by the action of iron filings on ferric hydrate in boiling water.

In both the last-named cases hydrogen is liberated.
According to Deville, ferro-ferric oxide is obtained as octa-

hedral crystals mixed with chloride, when a current of HC1 is
passed slowly over ferrous oxide. It has also been prepared
by Sidot, as octahedral crystals, by heating colcothar to a very

high temperature for 2 hours.
Moissan has prepared two allotropic modifications of this
oxide: the one by heating ferric oxide to about 350 to 400 C.
in a current of hydrogen or carbon monoxide, or by heating
ferro-ferric hydrate or ferrous carbonate to about 300 C. the ;
second modification being obtained by reactions carried on at a
high temperature, such as the combustion of iron in oxygen.

The first-named type is black, highly magnetic, susceptible to
the action of HNO 3, and exhibits a sp. gr.
= 4'86, whilst the
other, though black and magnetic, is impervious to this acid, and

is of higher density, namely 5 to 5'io.
II. Ferro-ferric Hydrate is prepared by precipitating an equi-

molecular solution of ferrous sulphate and ferric sulphate by NH 3.
The solution is poured into the reagent, since, if the converse

method be adopted, a mixture (but not the compound) of ferrous
hydrate and ferric hydrate will be thrown down. Ferro-ferric
hydrate is of a dark green colour, and yields a black powder on

desiccation.
III. These comprise a number of oxides

Intermediate Oxides.
richer in FeO
than the magnetic oxide, and formed when iron is
heated to redness in presence of air.
Authorities are not agreed as to the composition of the mem-
bers of this series. Berthier obtained Fe 2 O 3 4FeO, and Mosander
,
6FeO, Fe 2 O 3 ; and, according to the latter, the various figures
given by different authors are due to the formation of successive

layers of oxides, of different constitution, on the surface of iron
heated to redness in the air. These oxides, however, cannot be

regarded as definite chemical entities.
IV. Oxide (Fe 2 O 3 pFeO). ,

This product was found by O.
Veelker on a n'atural magnetic oxide from Prevali in Carinthia.
D. FERRIC OXIDE. I. Anhydrous Ferric Oxide, (syn. :
Sesqui-
oxide, or peroxide, of iron) (Fe 2 O 3 ). When iron, or its magnetic
oxide, is calcined for a considerable time in the air, Fe 2 O 3 is
produced. A
simpler method, however, is to calcine the ferric
hydrate obtained on precipitating a ferric salt by an alkali. It is
also readily obtained by calcining nitrates or sulphates of iron ;
and last-named process is adopted on an industrial scale for

this
the manufacture of Nordhausen sulphuric acid and colcothar, or

commercial ferric oxide,
Fe 2 3 + 3 S0 3 ,
If the iron sulphate be mixed with common salt, the Fe 2 O 3

formed on calcination is in the condition of nearly black crystalline
fibres.
Iron sulphide also furnishes Fe2 O 3 when calcined.
Crystallised may be obtained by decomposing

ferric oxide
ferric chloride by means of lime at red heat (Daubree). When
ferric oxide is fused with borax before the blowpipe flame, and
the resulting greyish-green mass is dissolved in hot nitric acid,
Fe 2 O 3 is left in the condition of orange-coloured rhomboidal
prisms with 5 or 6 facets.
In colour ferric oxide is a more or less dark red, sometimes
nearly black, hygroscopic, and very hard. It is employed for
polishing metals, glass, etc. On prolonged exposure to white

heat it is converted into Fe 2 O 3 FeO. ,
It is not magnetic, though,
according to Malaguti, a magnetic anhydrous ferric oxide does
exist.
Ferric oxide is obtained by calcining organic ferrous salts in

air, ferrous carbonate oxidised spontaneously by exposure to air,
etc. Magnetic ferric oxide is produced by deflagrating ferro-
ferric oxide with KC1O 3 .
When heated towards 300 C., ferric oxide resembles finely

divided amorphous phosphorus in colour ;
whilst under the same
conditions magnetic ferric oxide is a light brick-red. This latter
oxide also differs from the ordinary form in point of density and
specific heat : thus ordinary ferric oxide has an average sp. gr. of
4-784 C., whereas that of the magnetic form is 4-686.

at 15 In
both cases the density is increased to 5-144 by strong calcination,
but the magnetic oxide is thereby rendered inert. The specific
heat of the non-magnetic oxide is 0*1794; that of the magnetic
oxide is 0*1863; and by strong calcination (destroying the
magnetic property of the latter oxide) these values are modified

to 0-1730-0-1734.
The oxide obtained from meteoric iron is also magnetic, a
property shown by Smith to be attributable to the presence of a

small quantity of nickel and cobalt.
On exposure to red heat, ordinary ferric oxide undergoes
incandescence and becomes of a brighter red colour, harder, and
more difficult to dissolve in acids. It is insoluble in HNO 3, the
best solvent being a mixture of 8 parts of H SO 2 4 and 3 parts
of water. The specific heat of the oxide is lowered by calci-
nation.
Ferric oxide is reduced by carbon, hydrogen, etc., and is
converted by SO, into ferrous oxide, which unites with the
sulphuric acid formed. It is attacked by phosphorus penta-

chloride ;
and ammonia reduces it to the state of metallic iron
containing nitrogen. On the other hand, it is not reduced by

stannous chloride, even at boiling heat.
Ferric oxide is an energetic oxidising agent, and its power
is, so to speak, illimitable, because of its recuperative capacity in
contact with air, afterparting with oxygen to oxidisable sub-
stances, the Fe2 O 3 thus reconstituted being again in a position to
give up a further quantity of oxygen.

It is on this account that, in course of time, nails embedded
in wood damage the portions in their immediate vicinity ;
and
fabrics spotted with rust quickly fall in holes.
P. Thenard ascribes an important role in nature to ferric
oxide, and considers that it oxidises organic matter, the nitrogen

of which it converts into nitrates.
Ferric oxide is very extensively found in nature, and consti-
tutes the most abundant ore of iron. For industrial purposes it
is used, under the name of colcothar, as a polishing material for

metals and glass as a pigment for decolorising syrups in the
; ;
sugar refinery, and it also enters into the composition of enamels

and glazes in the ceramic industry.
II. Ferric Hydrates. Several of these are known, but their
investigation is a somewhat difficult matter, and their exact

formula hard to define.
An examination of the various natural ferric hydrates may
serve as a starting-point or basis for the study of these products.
Turgite, or Hydrohaematite, consists of 2Fe 2 O 3 ,

HO 2 ; gcetJdte
is Fe 2 O 3 ,
HO2 ; limonite, 2Fe2 O 3 , 3H O; 2
and the brown mineral
of Huttenrode (Murray), Fe2 O 3 ,
2 H 2 O.
If a dilute solution of ferric chloride be precipitated by NH 3,
and the precipitate dried over sulphuric acid after washing with
alcohol and ether in succession, the mass will exhibit at the end
of 2 months' storage the same composition as Huttenrode ore,
namely Fe 2 O 3 ,
2H 2 O.
The precipitate obtained by treating ferric chloride with an
alkali is probably the hydrate Fe 2 O 3 , 3H 2 O. This compound
dissolves readily in acetic acid, and the resulting solution gives
a precipitate of Prussian blue with potassium ferrocyanide. It
readily parts with water. When dried in vacua it becomes

2Fe2 O 3 , 3H 2 O, and therefore corresponds to limonite. Heated
to 100 under water for several minutes it again undergoes de-
hydration and then becomes Fe 2 O 3 2 O, analogous
to gcethite. ,
H
If the boiling be prolonged, more and more of the water of
hydration is set free, and the whole is lost on heating in a sealed

tube to a temperature approaching 1 60 C. (de Senarmont).
Another method of preparing the hydrate Fe2 O 3 H 2 O is by ,
precipitating a boiling solution of ferrous carbonate by a mixture

of sodium carbonate and sodium hypochlorite. In the cold the
reaction is more protracted, and the precipitate contains Fe 2 O 3 ,
2H 2 0.
A compound, with the formula 3 Fe 9 O 3 , 5 H 9 O, is obtained
by adding basic ferric sulphate to caustic potash in a state of

fusion. H. Brunck and C. Graebe found Fe 2 O 3 ,
HO 2
in the
product of the action of caustic soda on a cast-iron boiler. This

substance occurred as a friable mass composed of lustrous
lamellae,of sp. gr. 2-91, unaffected by cold H 2 SO 4 or HNO 3 ,
and but slowly soluble in cold HC1.

These various hydrates are of different shades of colour,
ranging from yellow to dark brown. D. Tommasi classifies
them, according to the ease with which they give up their water,
into
(1) The broivn hydrates obtained on precipitating ferric salts by
an alkali.
(2) TJie yellow hydrates resulting- from the oxidation of ferrous

or ferro-ferric hydrates, and of ferrous carbonate.
Those of the first class are more easily dehydrated than the
others, and furnish a brown anhydrous oxide, of sp. gr. 5'ii,

readily soluble in acids. The oxide from those of the second
class is red, of sp. gr. 3*95, and "only sparingly soluble in acids.
On gently heating the hydrate obtained by precipitating

ferric chloride by ammonia, so as to drive off all the water, and
then applying stronger heat, the mass suddenly becomes incan-
descent, without alteration of weight, and leaves an anhydrous

oxide more indifferent than if prepared at a lower temperature.
If ordinary ferric hydrate be heated to iooC. for 7 or 8
hours, it acquires properties differing from those it originally
possessed. At the end of several minutes the composition has

altered H 2 O, as we have already seen. The
and become Fe.2 O 3 ,
colour, too,has changed from ochre -yellow to brick -red; and
boiling concentrated nitric acid only dissolves it by degrees,

nor is it dissolved by HC1, except by boiling or prolonged
digestion. No longer does it give a precipitate of Prussian

blue with acetic acid and potassium ferrocyanide and when ;
heated to redness it no longer becomes incandescent, but behaves

as though already calcined.
When dried, this modified hydrate is pulverulent, whereas the
ordinary hydrate yields hard, brittle fragments.
The following facts, investigated by Pean de St. Gilles,
Scheurer-Kestner, and Graham, also tend to prove the exist-

ence of a modified form of ordinary ferric hydrate.
8o THEORETICAL STUDY OF ALUMINIUM, IRON,
If ferric acetate be prepared in the cold, from the precipitated
hydrate and acetic acid, a more or less reddish liquid, presenting

all the characteristic of the ferric salts, is obtained. On boiling
this liquid the colour suddenly becomes 4 or 5 times more
intense, and concurrently a powerful odour of acetic acid is
noticeable, without any precipitation occurring. If the heating

be carried on in sealed tubes at about 1 00 C., on the water
bath, the liquid will be found progressively modified, at the
end of several hours, the colour becoming a lighter red without
any alteration in intensity. Viewed by reflected light it appears
turbid, but is still perfectly limpid and homogeneous by transmitted
light ;
it has, however, entirely lost the usual taste of iron salts,
and now exhibits only that of acetic acid ;
a Prussian blue
precipitate is no longer formed with potassium ferrocyanide, and

no increase in the depth of colour is produced by potassium
thiocyanate. On the other hand, the addition of a trace of H 2 S
or of an alkali salt precipitates the whole of the ferric hydrate
present, in the form of a red deposit insoluble in acids and ;
this hydrate, when dried on a sheet of glass, forms small blackish-

brown lustrous plates, soluble in pure water, and furnishing a
liquid which is turbid by reflected light but transparent by

transmitted light, highly coloured and devoid of any appreciable
flavour. This liquid may be precipitated anew by concentrated
HC1, HNO 2,
etc.
The same result is obtained from ferric nitrate ;

and in the
case of this salt Scheurer-Kestner observed that light produces
the same effects as heat.
These phenomena are evidently of the same order as those

occurring when solutions of ferric chloride are exposed to the
influence of heat.
The resulting liquids can no longer be regarded as solutions
of ferric salts acetates, nitrates, chlorides, etc. but one is com-
;
pelled to look upon them as acid solutions of modified ferric
hydrate, or as emulsions of this hydrate in dilute acids, the latter

acting mechanically and separating the particles of hydrate into
an extremely fine state of division.
On saturating ferric chloride with ferric hydrate and dialysing

the resulting red liquid, the latter parts with almost the whole of
its acid and leaves behind in the dialyser a deep blood-red liquid,
highly charged with ferric hydrate, which can be concentrated, to

a certain degree, by boiling without becoming coagulated.
This solution may be coagulated in the cold by adding a
trace of H SO
2 4, by an alkali, and by a large number of salts ;
but no turbidity produced byis 3 HC1, or alcohol. HNO ,
The coagulum forms a dark red jelly, which though insoluble

in water is readily dissolved by dilute acids. It constitutes the
"
colloid hydrate" of Graham.
When the liquid obtained by dialysis evaporated in vacua it
is
leaves the hydrate 2Fe 2 O 3 , 3H O 2 (Magnier de la Source), whilst

the modified hydrate seems to always contain Fe2 O 3 ,
H 2 O.
Freshly precipitated ferric hydrate is employed as an antidote
to arsenious acid.
39. Ferrites. This name is applied to compounds of ferric
oxide with various protoxides, the ferro - ferric oxide already

described being a typical example. Most of these compounds
are magnetic.
A. POTASSIUM FERRITE. Fremy prepared this body by

heating to redness a mixture of i
part of iron with 2 parts of
potassium nitrate, and Mitscherlich obtained it by calcining
ferri-potassium oxalate. It is yellowish green, and is decom-
posed by water, which extracts the alkali.
B. SODIUM FERRITE is prepared by the same reactions as
the potassium compound, and possesses the same properties.
C. CALCIUM FERRITE, Fe 2 O 3 (CaO) 4 . This has been obtained
by the precipitation of a mixture of i molecule of Fe 2 Cl 6 and

4 molecules of CaCl 2 by caustic potash. The precipitate, yellow
at first, gradually becomes white if carefully preserved from con-
tact with air ;
otherwise it is decomposed by atmospheric carbon
dioxide. When boiled it turns white immediately. This ferrite
is a light, perfectly white powder, insoluble, decomposed by weak

acids (even by CO 2 ).
Neither water nor sugar solution is able to
extract the lime.

List obtained the compound CaO, Fe 2 O 3 on precipitating a
neutral solution of Fe 2 Cl 6 by lime water, and drying and calcining
the resulting deposit. This product is brown, friable, and

magnetic.
J. Percy has prepared a calcium ferrite in voluminous
crystals of metallic lustre, and with a sp. gr.
= 4/693, by heat-
ing to whiteness, and afterwards slowly cooling, a mixture of

ferric oxide and lime.
D. BARIUM FERRITE. A brown, friable, magnetic body, of
the formula BaO, Fe 2 O 3 ,
was obtained by List by the same
method as for calcium ferrite.
E. MAGNESIUM FERRITE is obtained in a similar way from

milk of (calcined) magnesia, and forms a brown precipitate,
which on calcination agglomerates in highly magnetic, fritted,
cannel-brown fragments. When dried over H 2 SO 4 this pre-
cipitate corresponds to the formula Fe2 O 3 4-H 2 O.
,
ZINC FERRITE. According to Ebelmen, the compound

F.
2O3
ZnO, Fe is obtained by heating to whiteness, for several
days, a mixture of
1
part ferric oxide,
2 parts zinc oxide,
2 parts boric acid.
When treated with cold dilute HC1 the mass parts with
zinc borate, and there remains a black powder crystallised in j
regular octahedra and composed of zinc ferrite, which is soluble

in boiling, concentrated HC1.
G. MANGANESE FERRITE. This is a brown-black pre-
cipitate obtained by treating with caustic potash a mixture of

equal molecular proportions of manganese and ferric chloride.
H. COPPER FERRITE (CuO, Fe 2 O 3 5H 2 O) is prepared in the ,
same manner, and forms a dirty yellow, voluminous 'precipitate,

which turns blackish brown on calcination.
40. Ferric Acid. Ferric anhydride, discovered by Fremy,
has the composition FeO 3 ;
but neither this body nor its hydrate,
ferric acid, FeO 4 H 2 ,
is known in a free state, though some of
its salts have been prepared, among them being K FeO2 4,

which
is analogous to K MnO4
2 .
When attempts are made to set ferric acid at liberty it
decomposes as follows :
4 H 2 Fe04 = 2Fe 2 3 + 4H O + 3O2 2 .

De Mollins confirmed the accuracy of the formula FeO 3 by

the analytical results obtained with barium ferrate, namely, from
the quantity of iodine liberated by that salt from potassium
iodide, according to the equation
2FeO 4 Ba+8KI+ I6HC1
= 2BaCl 2 + 8KC1 + 2FeCl 2 + 8H 2 O + 4l 2
41. Ferrates. A. POTASSIUM FERRATE (FeO 4 K 2 ). There
are several methods of preparing this salt :
(1) Dry Method. Five grams of pure iron filings are placed
in a Hessian embedded in live coals, and when the
crucible
metal is red-hot an addition is made of 10 grams of powdered
saltpetre, previously freed from moisture by fusing. A brisk

reaction immediately ensues, and, after leaving the covered
crucible to cool down, a violet-red mass, very rich in potassium
ferrate, is obtained.
The same product may also be prepared by the action of
\
saltpetre on iron oxide.

(2) Wet Method. A current of chlorine passed through a
is
solution of 30 parts of caustic potash in 50 parts of water, in

presence of i
part of freshly precipitated ferric hydrate. An
excess of potash is maintained throughout the reaction by suitable
additions of this reagent. Finally, a black powder (potassium
ferrate) is obtained, which is insoluble in potash but should
dissolve completely in water to form a rose-coloured solution.
Potassium ferrate may also be formed under various other
conditions : forexample, when potassium peroxide is treated with
ferric oxide ; by the action of an electric current on a solution of
caustic potash contained in a cast-iron vessel (Poggendorf) by ;
saturating caustic potash solution with iodine and calcining the

saline residue in an iron crucible ;
etc.
Potassium ferrate is fairly stable when in the solid form or in
concentrated solutions, but decomposes very quickly when diluted

with water, oxygen being liberated and Fe2 O 3 deposited. The
concentrated solution will stand boiling, especially when it con-
tains a mineral salt ;
the addition of an acid, however, produces
immediate decomposition, and ammoniacal salts or reducing
agents
"^^11 LO convert the
V^WJ ferric acid into ferric hydrate.
Potassium ferrate is exceedingly soluble in water, the solution
exhibiting a handsome red or violet- red coloration.
B. SODIUM FERRATE is easily prepared by the wet method,
by passing a current of chlorine through a concentrated solution

of caustic soda containing ferric hydrate in suspension. It is
soluble in water.
C. AMMONIUM FERRATE does not appear to exist, since the
ferrates are immediately decomposed by NH 3 , nitrogen being
liberated and a precipitate of Fe 2 O 3 produced
2 K FeO + 2NH = N + Fe O3 + 4 KHO + H
2 4 3 2 2 2 O.
D. BARIUM FERRATE (BaFeOJ. This compound is pre-
pared by double decomposition, by precipitating potassium ferrate

with barium nitrate or barium chloride, an insoluble precipitate of
a handsome purple-red colour being formed.
It is much more stable than the alkali ferrates, and is but
slightly affected by organic substances. Powerful acids expel
oxygen and form the corresponding barium and ferric salts.
With acetic acid it gives a handsome red solution, which is
decolorised on heating.
The ferrates of calcium and strontium are also insoluble, and
are obtained by the double decomposition method.
42. Sulphides of Iron. These compounds, which are more
numerous than the oxides, will now be dealt with in succession,
commencing with those containing least sulphur.
A. IRON SUB-SULPHIDE (Fe8 S). This substance, described
by Arfvedson, is formed on the reduction of basic

sulphate ferric
by hydrogen. a dull dark grey powder, which dissolves

It is
in acids, with evolution of 4 and i 2 S.

H H
B. IRON SUB-SULPHIDE (Fe 2 S).This sulphide has been pre-
pared by reducing anhydrous ferrous sulphate by hydrogen. In
the initial stage SO 2 and H O are obtained, and subsequently H
2 2 S.'
The reaction may be explained by one or other of the

following equations :
(1) 2SO 4 Fe + 9 H 2 = Fe 2 S + H 2 S + 8H 2 O.
(2) 4 SO 4 Fe + 5 H 2 = 2 Fe 2 S + H 2 S + SO 2 + 4H 2 O.
i 1
When treated with H 2 S in the warm, this sulphide, like the
preceding one, is converted into magnetic pyrites.

C. FERROUS SULPHIDE (FeS) is obtained

by mixing together
60 parts of iron filings and 40 parts of sulphur with sufficient
hot water to form a paste (Lemery's volcano), combination being
attended by evolution of heat. The resulting sulphide is readily
oxidised.
Crystalline FeS is obtained by the action of H 2 S on ferro-
ferric oxide, HO2 and H S being liberated.

2 If stronger heat
is applied sulphur is evolved, and black or yellow hexagonal

crystals are left (Sidot). On heating 56 parts of iron with 32
parts of sulphur, a porous, black, somewhat fusible mass is
obtained, the principal use of which is for preparing H 2S

in the
laboratory.
FeS may also be prepared by the wet method by pre-
cipitating a ferrous salt with an alkali sulphide
S0 Fe + Na
4 2 S = FeS + SO 4 Na 2,
or with a bisulphide
SO 4 Fe + 2NaHS = FeS + H 2 S + SO 4 Na 2.
When ferric salts are employed, FeS is also formed, but in

this case sulphur is deposited
(SO 4 ) 3 Fe 2 + 3Na 2 S = 3SO,Na 2 + 2 FeS + S.
The higher sulphides of iron when heated to bright redness
!
part with sulphur, a residue of FeS being left.

The precipitated sulphide, FeS, is black, insoluble in water,
but dissolves in acids without yielding any deposit of sulphur or
disengaging free hydrogen ;

it is also soluble in alkalis. This
sulphide is readily oxidised, and turns grey in consequence of the

liberation of part of its sulphur ;
at the same time, ferrous
sulphate and ferric oxide are formed

6FeS + ;O 2 = 2SO 4
Fe + 2Fe 2 O 3 + 2S 2 .
Ferrous sulphide prepared by the dry method is fusible, -
brittle, and undecomposable by even white heat, or by hydrogen,
carbon, etc. If, however, lime, earthy carbonates or silicates are
present, it is decomposed by carbon.

In contact with nitric acid, FeS liberates NO, and yields
Fe 2 O 3 and H.SO,.
Ferrous sulphide is comparatively rare in nature.
D. MAGNETIC PYRITES (Fe 7 S 8). This pyrites may be
regarded as a saline sulphide formed by the union of the
sesquisulphide or the bisulphide of iron with ferrous sulphide

FeS 2) 6FeS, or Fe 2 S 3 sFeS. ,
It is obtained artificially by calcining the bisulphide, or by

treating iron at white heat with sulphur ;
or again, by dropping
sulphur into a red-hot crucible charged with iron turnings.
There is also another sulphide, Fe 3 S 4 corresponding to the ,
" "
magnetic oxide Fe 3 O 4 and to which the name
, magnetic pyrites
is better applicable than to Fe 7 S 8 .
According to Rammelsberg, a sulphide with the formula Fe 5 S 6

can be prepared by bringing incandescent iron into contact with
sulphur.
E. IRON SESQUISULPHIDE (Fe2 S 3). This sulphide is formed
by heating to dark redness a mixture of sulphur and ferrous

sulphide and also 'by passing a current of H 2 S over Fe 2 O 3
;
heated to about 100 C.

In the anhydrous condition it is unalterable by air, is of
a yellowish-grey colour with a green or greyish tinge, and is
partially soluble in acids.

It occurs in nature, frequently in association with copper as
coppery pyrites, CuS, Fe 2 S 3 and sometimes as 3CuS, Fe 2 S 3

,
.
F. IRON BISULPHIDE, (syn. : Iron pyrites) (FeS 2 ). This,

the most important sulphide of iron, may be produced artificially
by gently heating iron with an excess of sulphur. Wohler has

obtained it, in the form of octahedral crystals, by heating a
mixture of ferric oxide, sulphur, and sal ammoniac on the sand
bath ;
and it may also be prepared by the action of sulphuretted
hydrogen on ferric oxide, ferro-ferric oxide, or ferrous carbonate,

at a temperature between 100 C. and dark red heat. Below
1 00 C. the product mainly consists of sesquisulphide, and above
red heat of magnetic pyrites.
When heated in the air the bisulphide gives off sulphur
dioxide and leaves behind ferrous sulphate or a basic ferric
sulphate, if the temperature is high enough to effect the de-

composition of the ferrous sulphate.
If heated in a current of phosphuretted hydrogen to a
temperature below that at which sulphur is liberated spontaneously,

the bisulphide yields iron phosphide, sulphur and sulphuretted

hydrogen being disengaged.
This sulphide is very abundant in nature, and constitutes
ordinary or martial pyrites, which occurs in two allotropic

modifications.
(1) Cubical-Pyrites is of a brassy-yellow colour, with a sp. gr. =

4
f
8 to 5'2. It gives off sparks when struck against steel.
(2) Prismatic Pyrites. This form, which is less common,

is white, and of sp. gr. 4' 74. Wohler mentions that these two
densities exhibit the same mutual ratio as those of octahedral
and prismatic sulphur (2'o66 and i'962).
G. IRON PERSULPHIDE (FeS 3). Like ferric anhydride, this
sulphide has not yet been isolated, though it is known in a state
of soluble combination with potassium sulphide, the compound

being prepared by passing H 2 S through a solution of potassium
ferrate.
43. Nitrosulphides of Iron. These salts, discovered by

Roussin, constitute a remarkable group of substances, in which
the contained iron cannot be detected by any of the usual
reagents, as is also the case with the ferrocyanides.
The nature of these compounds is still the subject of con-
troversy ;
and the researches of Porczinsky, Rosenberg, Pawel,
and Demel have increased the complexity of the question by the
varying formulae arrived at by these authors, according to the
methods of preparation employed. According to Roussin, if two
one of ammonium bisulphide, the other of potassium
solutions,
nitrite, be mixed together and treated with ferric chloride or

ferric sulphate, added drop by drop with continual agitation, on
heating to ebullition the blackish precipitate is re-dissolved. On
nitration after boiling, the very dark coloured filtrate obtained
deposits, on cooling, a large quantity of black crystals, whilst

sulphur is left on the filter. The reaction is equally well defined
when is no longer any
ferrous sulphate is employed, but there
deposit of sulphur a slight excess of alkali sulphide has
;
and if
been taken, the precipitate re-dissolves almost completely.
Porczinsky works in a slightly different manner, by adding

ammonium bisulphide to a solution of ferrous sulphate saturated
with nitrogen dioxide, heating to 1 00 C., filtering, and evapor-

ating the filtered liquid.
Demel proceeds by adding I c.c. of ammonium bisulphide
solution to 20 grams of potassium nitrite dissolved in 300 c.c. of
boiling water. Ebullition having been continued for several
minutes, a solution of 33 grams of ferrous sulphate in 200 c.c. of

water is added.
Pawel adds 10 grams of sodium sulphide, dissolved in 300 c.c.
of water, to a boiling solution of 40 grams of potassium nitrite in

600 c.c. of water. He then introduces 70 grams of ferrous sul-
phate dissolved in 300 c.c. of water, heats to 70 to 80 C. for half
an hour, and leaves to cool after filtration.
The crystals deposited when the cooling down has been

gradual are usually very well formed and sometimes attain
i to 2 cm. in length. They are very heavy, easy to wash, and
sparingly soluble in cold water, but more readily so in hot ; very

soluble in alcohol, glacial acetic acid, amyl alcohol, and slightly
soluble in petroleum spirit and in turpentine. In ordinary ether
they are soluble in all proportions, and are instantly liquefied by

contact with the vapour of this solvent, but are totally insoluble
in CS 2 .
The crystals are of a very dark colour, with a metallic lustre, and
greatly resemble iodine. Their tinctorial power is very consider-

able, and the flavour is styptic at
subsequently becoming bitter.
first,
Provided they have been deposited from a slightly alkaline

liquor, they are unalterable on exposure to air. Decomposition
does not ensue on heating, until the temperature reaches 115 to
I40C.
Concentrated sulphuric, nitric, and hydrochloric acids attack
them briskly at the ordinary temperature and ammonia pre-
;
cipitates them from their solutions, as do also (NH 4 ) 2 S,

H 2 S,
and
the ferro- and ferri -cyanides ; tannins, however, have no action.
With black precipitate of sulphide and ferric
silver nitrate a
sulphide is formed, nitrogen dioxide being liberated but gold ;
chloride is reduced to the metallic state.
The formulae ascribed by different authors to the compounds

obtained, by methods differing but slightly one from another, are
AXD COMPOUNDS OF THESE METALS 89
Thus Roussin "

very dissimilar. styles his product iron dinitro-
sulphide," and assigns it the following composition :
Fe s S 5 H.(NO) 4 = Fe 2 S 5 (NO) 3 .H 2 S.FeS.NO.

That obtained by Porczinsky is credited with being
Fe 3 S 3 (NO) 4 2H 2 O = FeS, Fe2 S 2 (NO) 4 + 2H 2 O.
,
Rosenberg's nitrosulphide corresponds to the formula

Fe6 S 5 (NO) 10) 4 H 2 ;
whilst Pawel gives the symbol as

Fe 7 S 5 (NO) 12 H 2 .
Demel has described the ammonium compound of the nitro-

sulphide obtained by himself, and considers it as a nitrated amide
of the composition
F
Fe2 S 2 (N0 2 ) 2 (NH 2 ) 2 =
F
N0 2
Caustic potash and soda have no action on iron dinitrosul-
phide in the cold ; but, on prolonged ebullition, ammonia is

liberated, and a red crystalline deposit of ferric hydrate, Fe 2 H 2 O 4 ,
is formed, leaving a less highly coloured liquid, which, when con-

centrated over sulphuric acid, furnishes voluminous black crystals
arranged like a series of hoppers.

The crystals obtained by the action of caustic soda have
"
received from Roussin the name of sulphuretted nitrosulphide of
"
iron and sodium (nitrosulfure sulfure de fer et de sodium}, and
consist of
Fe 2 S 3 (NO) 2 3Na 2 S-f

, aq.
Porczinsky gives to this compound, when dried at 1 00 C,

the formula
Na 2 S, Fe,S 2 (NO) 4 ;
whilst,according to Rosenberg, the formula of the crystals

should be
Fe s S 9 (NO) 18 Na 8 +2 4 H 2 0;
or, according to Pawel,
Fe 10 S 10 (NO) 18 Na 10 +27H 2 0.
The crystals are soluble in water or alcohol, but insoluble
in
ether. When dissolved and heated with lead nitrate they yield a
reddish precipitate soluble in caustic potash ;

whilst zinc sulphate
gives a brown precipitate containing zinc, sulphur, iron, and

nitrogen dioxide. Ferric chloride gives a black precipitate, but
none is produced by tannin, sulphuretted hydrogen, and potas-
sium ferrocyanide whilst the ferricyanide gives a precipitate of

;
Prussian blue.
When treated with acids, in the cold, the solution yields a
flocculent reddish precipitate, which readily parts with sulphuretted
hydrogen, and which exhibits the composition Fe2 S 3 (NO) 2 4H 2 S. ,
"
Roussin terms this substance " sulphuretted nitrosulphide of iron
(nitrosulfure sulfure de fer).
If a boiling solution of the above-named crystals be treated
with dilute acid, H 2 S is disengaged, and a dense black deposit,
insoluble in water, alcohol, or ether, is formed containing
Fe 2 S 3 (NO) 2 ,
i.e. iron nitrosulphide. This is a very inflammable
substance, and decomposes gradually in the dry state. With

sodium sulphide it gives large crystals, red by transmitted light,
black by reflection, soluble in water, alcohol, or ether, but in-
soluble in carbon disulphide or chloroform ;
the composition is
represented by Fe 2 S 3 (NO) 2 ,
Na 2 S, H 2 O. On treating a solution of
this salt with an acid, iron nitrosulphide is reconstituted.
The iron nitrosulphide compounds may be compared to
the nitrocyanides, into which, moreover, they can be converted

under the influence of mercury cyanide or potassium cyanide.
Conversely, the nitrocyanides may be transformed into nitrosul-
phides by the acid of sulphuretted hydrogen or an alkali
sulphide.
44. Sulphites of Iron. A. FERROUS SULPHITE (SO 3 F,3H 2 O).
When iron is dissolved by sulphurous acid, out of contact with
air, a liquid is obtained containing both SO 3 Fe and S 2 O 3 Fe, from
which, on evaporation in vacua, ferrous sulphite separates out in
the form of greenish needles containing 3H 2 O. This sulphite
oxidises readily in presence of moist air it is sparingly soluble ;
in cold water, the

solubility increasing in presence of SO 2.
B. FERRIC SULPHITE, (SO 3)3 Fe, is unknown in the solid
state, and the solution is very unstable.

When ferric hydrate is dissolved in sulphurous acid the
liquid acquires a red colour at first, but afterwards becomes
rapidly decolorised in consequence of the formation of ferrous
sulphate
(SO 3 ) 3 Fe2 = SO 4 Fe + SO 3 Fe + SO 2 .
Solutions of ferric sulphite yield, on boiling, an insoluble

ochreous powder of basic sulphite
(Fe 2 3) 3 S0 ;H
2) 2 0.
If alcohol be added, instead of boiling the solution, a basic

sulphite is also thrown down.
45. Ferrous Hyposulphite (S 2 O 3 Fe) is obtained as a residue

in the preparation of ferrous sulphite, or by double decomposition
between barium hyposulphite and ferrous sulphate; or again, by
digesting sulphur with ferrous sulphite. It takes the form of
small greenish needles soluble in alcohol.
46. Thiosulphates of Iron. A. FERROUS THIOSULPHATE

(S 2 O 6 Fe, 5 H 2 O).
This
by double decomposition
is obtained
between barium thiosulphate and ferrous sulphate, the filtered
liquid yielding, on spontaneous evaporation, small greenish
prisms, oxidising on exposure to air and soluble in water.
B. FERRIC THIOSULPHATE (S 2 O 6 ) 3 Fe2 . When thiosulphuric

acid is treated with ferric hydrate a basic thiosulphate is obtained
as a brown-red powder.
The thiosulphate (S 2 O 6 ) 3 Fe 2 is obtained, as a red solution, by
double decomposition.
47. Ferrous Tetrathionate (S 4 O 6 Fe) is a very unstable salt,
readily decomposing into ferrous sulphate, sulphuric acid, and

sulphur. It is prepared by adding ferrous hyposulphite, drop by
drop, to a solution of Fe2 Cl 6
Fe 2 Cl 6 + 2S 2 O 3 Fe = 3FeCl 2 + S 4 O 6 Fe.
48. Sulphates of Iron. A. FERROUS SULPHATES. I. Nor-
mal Ferrous Sulphate (SO 4 Fe, 7H 2 O). This substance, which is
still known as green vitriol, green copperas, etc., is one of the
most important salts of iron.
It is prepared, on a manufacturing scale, by the action of

sulphuric acid on iron, by oxidising pyrites, pyritic shales, etc.
The product is, however, impure, being contaminated with copper,

tin, zinc, manganese, alumina, magnesia, lime, silica, sulphuric
acid, organic matter, etc.
In the laboratory, ferrous sulphate is prepared by treating an
excess of iron with pure H SO
2 4, or by repeatedly re-crystallising
the commercial salt.
FIGS. 33, 34, and 35. The forms most commonly assumed by ferrous sulphate.
Ferrous sulphate crystallises in the oblique prismatic system,

rhomboidal -
as crystals of a bluish green colour, containing
7H 2 O. They exhibit a disagreeable styptic flavour, and a

sp. gr.
= 1-884.
This salt is soluble in water, 100 parts of crystals dis-
solving
At 10 C. in 164 parts of water. At 60 C. in 38 parts of water,

,, 15 143 ii 90 ,, 27
24 87 ,, 100 ,, 30
,,43 66
The density of various solutions of this salt at 17-2 C. is
given in the subjoined table (R. Jagnaux) :

According to Gerlach, the density of ferrous solutions at I

5 C.
is as follows :
Ferrous sulphate is almost insoluble in strong alcohol, and

entirely so in glacial acetic acid, though soluble to the extent of
about 3 grams per litre in 50 alcohol.
On heating, the crystallised salt melts in its own water, and

afterwards gradually suffers dehydration. At 1 00 C. it parts
with 6 molecules of water, but the final molecule is not driven off
until nearly 300 C. is attained. This seventh molecule of water
seems to play a different part to the rest, since it is more difficult
to eliminate. This it is also which proves the existence of double
salts, such as
(S0 4) 2 K 2 Fe, 6H 2 O,
isomorphous with SO 4 Fe, 7H 2 O, and which may be regarded as
derived from the latter by the substitution of I mol. of K 2 SO 4 for
i mol. of water.
At red heat, ferrous sulphate splits up into SO 2, SO 3,
and
Fe 2 3
2SO 4 Fe = Fe2 O 3 + SO 3 + SO 2 .
In the crystallised state, ferrous sulphate is somewhat unstable,
oxidising on exposure to the air, and turning yellow, with forma-

tion of an external ochreous layer of basic ferrous sulphate con-
taining (SO 4) 3 Fe2 5Fe2 O 3

,
or (Fe 2 O 3 ) 2 SO 3 This oxidised salt is the
.
one employed in the manufacture of Nordhausen sulphuric acid.

To preserve ferrous sulphate unaltered in the laboratory, the
addition of glucose or gum, to the mother liquor from which the
crystals are to be deposited, has been proposed. For the same

purpose Welborn recommends that a fragment of camphor wrapped
in paper should be kept with the crystals ;
the keeping properties
are also improved by their containing a little free sulphuric acid,
as also by their being stored in a perfectly dry state and in a dry
atmosphere.
In solution also, ferrous sulphate is oxidised by exposure to

the air, and becomes turbid, depositing basic salts. It may,
however, be preserved indefinitely by an addition of sulphuric acid
and exposure to sunlight.
When a solution of ferrous sulphate is exposed to the air it
deposits an ochreous powder, (Fe 2 O 3) 2 SO3, 3H 2 O. The solution
then contains, in addition to ferrous sulphate, normal ferric sul-
phate, (SO 4) 3 Fe 2 and a

,
basic sulphate,(SO 4 ) 3 Fe2 Fe 2 O 3 The ,
.
composition of the precipitate, however, is by no means constant,

but varies according to the strength of the solution, duration of
exposure to air, etc.
On adding water, a new precipitate of varying composition is
thrown down, leaving a ferro-ferric sulphate in solution.
Dissolved ferrous sulphate readily absorbs nitrogen dioxide,

the liquid then becoming a dark blackish brown. On evaporating
the solution in vacuo, NO
disengaged is heat be applied, nitrous
;
if
oxide is liberated and ferric sulphate formed. When heated to

boiling, the solution suddenly decomposes after a while, with con-
siderable effervescence, reddish fumes being evolved if a slight
excess of nitric acid be present. Treated by alkalis in the warm,
ammonia is formed ;
and when heated with absolute alcohol until
the precipitate ceases to re-dissolve, very unstable brown crystals
are obtained on cooling down the mixture out of contact with air.
With an excess of alcohol a more stable brown precipitate is
produced.
Ferrous sulphate is affected by all oxidising agents, nitric acid
converting it into ferric sulphate. Chlorine also acts as an oxidiser,
without any formation of basic salts taking place
6S0 4 Fe + 3C1 2 = Fe 2 Cl c + 2(SO 4 ) 3 Fe 2 .
Crystallised ferrous sulphate dissolves in 400 molecules of
water, 4510 calories being absorbed per molecule of the salt.

In the normal state, ferrous sulphate contains 7 molecules of
water and is isomorphous with the magnesium series ;
but under
certain conditions it parts with varying proportions of its water of
crystallisation, and furnishes hydrates containing I, 2, 3, 4, etc.,
molecules of water, or the anhydrous salt.

II. Anhydrous Ferrous Sulphate (SO 4 Fe). This salt is a
greyish-white powder, obtained by exposing the hydrated sul-
phate to a temperature of about 300 C. When brought into
contact with water it becomes hydrated, and recovers its green
colour.
Ferrous Sulphate with I Molecule of Water of hydration

III.
(SO 4 Fe, 2 O)
H
is obtained
by heating the ordinary hydrated salt
to about 140 C. It loses its water towards 300 C.
IV. Ferrous Sulphate with 2 Molecules of Water (SO 4 Fe,

2H 2 O). According to Bonsdorff, this salt is obtained by treating
a saturated solution of ferrous sulphate with sulphuric acid, added
by degrees so as not to unduly raise the temperature until the
density of the liquid has attained 1*33. On allowing the solution

to evaporate, crystals of sulphate containing 4H O 2
are formed at
first, whilst the final crop of crystals exhibits the formula SO 4 Fe,
2H 2
O.
V. Hydrated Sulphate with 3 Molecules of Water (SO 4 Fe,
3H 2 O). When ferrous sulphate is crystallised in HC1 the salt
SO 4 Fe, 3H 2 O is obtained on cooling. It may also be prepared,
as a white incrustation, by evaporating a solution of SO 4 Fe,
7H 2 O, strongly acidified by 2 SO 4 H .
VI. Hydrated Sulphate with 4 Molecules of Water (SO 4 Fe,

4H 2 O). According to Regnault, this hydrate is formed when a
solution of ferrous sulphate is
crystallised at 80 C.
The author has found this salt, mixed with a little basic
ferricsulphate, aluminium
sulphate, calcium sulphate, etc., as
an accidental evaporation product of the liquors employed
in the manufacture of alum and ferrous sulphate from pyritic
lignites. He has also obtained it in the laboratory by sub-

jecting a concentrated solution of ferrous sulphate, slightly
acidified with H SO
2 4 to prolonged boiling, the water being
replaced as evaporated. It forms a dense, greenish-white
crystalline powder, which becomes re-hydrated on contact with

water, and sets like plaster of Paris. It crystallises in the mono-
clinic system.
VII. Hydrated Sulphate with 5 Molecules of Water (SO 4 Fe,
5H 2 O). This salt, which crystallises in triclinic crystals, has
been prepared by Marignac by evaporating an acidified solution

of ferrous sulphate in vacua.The crystals first formed contain
7H O, followed by those containing 5H 2 O, and finally by a crop
having only 4 molecules of water.
VIII. Hydrated Sulphate with 6 Molecules of Water (SO 4 Fe,
6H 2 O) is obtained by crystallising ferrous sulphate in hydro-
chloric acid through which a current of gaseous HC1 is being
passed. Owing to the action of the air the sulphate is partially
converted into chloride, Fe 2 Cl 4 ,
which crystallises out. The
mother liquor deposits tabular crystals of SO 4 Fe, 6H 2 O.
IX. Ferrous AnJiydrostdpJiate (S 2 O 7 Fe). This is a hygro-
scopic white powder, which comes down on the addition
of 9H SO9 4
to i volume of aqueous solution of ferrous
sulphate.
X. Acid Ferrous Siilphate. BonsdorfT claims to have obtained,
in the preparation of the hydrated sulphate containing 2H 2 O, an
acid sulphate containing
Ferrous oxide 28*38 per cent.

Sulphuric acid . . . .
45 -42 , ,
Water 25-97 ,,
XL Ferro-potassium Sulphate, (SO 4 ) 2 K 2 Fe, 6H 2 O, is obtained
by dissolving iron in potassium bisulphate. forms greenish

It
clinorhombic prisms, of sp. gr. 2-189. In presence of an excess

of H
2 SO 4) crystals
with 4H 2 O are obtained ;
at 60 C. the crystals
formed contain 2H 2 O.
XII. Ferro-sodium Sulphate is less stable than the foregoing
compound. It is prepared by crystallising the mixture of the

two sulphates at over 3 5 C., the resulting crystals being clino-
rhombic and containing 4H 2 O.
XIII. Ferro - ammonium Sulphate. To prepare this salt,
equivalent proportions of the two sulphates are crystallised

together; the resulting crystals have the formula (SO 4) 2 (NH 4 ) 2 Fe,
6H 2 O. They are voluminous, of a pale green colour, sp. gr.
1-813, and less subject than ferrous sulphate to alteration on
exposure to the air.
The conjoint action of concentrated hydrochloric acid and air

converts this salt into ferri-ammonium chloride.
The density of various solutions of ferro-ammonium sulphate

is given in the following table :
Ferrous sulphate forms other double salts, notably with the
sulphates of zinc, copper, etc., as well as with the sulphates
isomorphous with aluminium sulphate. These bodies are, how-

ever, frequently regarded as simple mixtures.
XIV. Ferrous Sulphate and Zinc Sulphate. The two salts
crystallise together, and if the mixture contains at least I 5 per

cent, of ferrous sulphate the crystals resemble those of that salt.
If, on the other hand, zinc sulphate predominates, the crystals are
modified accordingly, and take the form assumed by this sulphate.
XV. Ferrous Sulphate and Copper Sulphate. When ferrous
sulphate predominates the crystals take the ferrous sulphate form,

and contain 7 H 2 O in the contrary event they resemble those of
;
copper sulphate, and contain 5H 2 O.

XVI. Ferro-ferric Sulphates. Ferrous sulphate and ferric
sulphate form between them certain well defined double

salts.
When a cold solution containing 3 molecules of ferrous
sulphate and 2 molecules of ferric sulphate is treated with con-

centrated sulphuric acid an unstable precipitate containing
(SO 4 ) 9 Fe3 (Fe 2 ) 2) 4H O2
is formed.
On two sulphates with 5 or 6 times
diluting a solution of the
its weight of water, the temperature rises by 25, and, on re-
cooling, long pale green prisms corresponding to
S0 Fe + 6[(S0 Fe + ioH 2 O
4 4) 3 2]
are deposited.
When a concentrated solution of the two sulphates is treated

with a large excess of 2 SO 4
H
and cooled down after heating to
,
about 200 C., it furnishes rose-coloured hexagonal crystals of an

acid ferro-ferric sulphate containing
(S0 4) 3 Fe 2 S0 4 Fe, 2H 2 SO 4
,
.
7
B. FERRIC SULPHATES. I. Normal Ferric Sulphate, (SO 4 ) 3 F 2 ,
may be prepared by dissolving ferric hydrate in sulphuric acid, or
by gradually adding to a solution containing nitric and sulphuric

acids a quantity of ferrous sulphate corresponding to 2 molecules
per each molecule of H SO

2 4
6(SO 4 Fe, 7H 2 0)+ sH 2 SO 4 + 2HNO 3

- 3 [(S0 4 ) 3 Fe 2 ] + 2NO + 46H 2 O.
On evaporating to dryness, to drive off the excess of HNO 3, a
yellowish-white residue of normal ferric sulphate is left. This
product is insoluble in HC1, but dissolves slowly in water and

becomes hydrated. Iron and analogous metals reduce it to the
condition of ferrous sulphate, with evolution of hydrogen, and it is
broken up by heat into SO 3 and Fe 2 O 3 .
When boiled, "ferric sulphate solution

is partially decomposed
and throws down a basic hydrated salt. Alkali carbonates pre-

cipitate a body which re- dissolves, with effervescence, on agitation,
the highly coloured liquid then gradually depositing a yellow
precipitate of basic sulphate.

When alcohol is added to a solution of ferric sulphate con-
taining a potassium carbonate, normal sulphate remains in

little
solution, and an unstable reddish-yellow saline mass of a complex
ferri-potassium sulphate is thrown down. This decomposes after

a while, yielding an insoluble basic ferric sulphate.
Hydrated ferric sulphate is of a dark brown colour, and
normally contains 9H 2 O, in which state it is found native in

Chili. A hydrated sulphate containing ioH 2 O has been ob-
tained in the form of nacreous rhomboidal lamellae, by peroxidis-
ing. ferrous sulphate with HNO 3 and boiling with an excess of
sulphuric acid.
Ferric sulphate is extremely soluble in water, the density of
its solutions, measured at 1 7* 5 C., being given in the following

table.
Several basic ferric sulphates are known, and the general

method adopted for their preparation by the action of oxidising
is
agents on ferrous sulphate in the same way as for the normal
sulphate. In treating of the valency of iron it was admitted that

the double hexatomic molecule (Fe 2 ) results from the junction of

2 atoms Fe playing the part of a tetravalent body, and that,
may be regarded as Cl 3 Fe FeCl 3
consequently, ferric chloride .
Now, normal ferric sulphate has the formula (SO 4 ) 3 Fe2 and
,
the
basic sulphates may be considered as this normal salt, wherein
i or 2 divalent atoms of oxygen have replaced I or 2 divalent
groups SO^.
Density. (S0 4 ) 3 Fe 2 .
1-0170 32 per cent.

I -0340 34
36
1-0684 38
I -0854 40
1042 42
1
1
230 44
I42O 46
1624 48
1826 5
2066 52
2 3 06 54
2559 56 ,;
2825 58
3090 60
2SO 3 = (S0 4 )
(Fe 2 O 3
:
II. Basic Ferric Sulphate ,

O
The body is obtained from the normal sulphate by partial
neutralisation with calcium carbonate until the resulting pre-
cipitate becomes permanent. The filtered liquid then contains in
solution
-
Fe 2 j ((so A,
r\
Itmay by digesting normal ferric sulphate

also be prepared
with ferric hydrate, the resulting red liquid yielding, on desicca-
tion,an uncrystallisable gummy mass. This salt decomposes on

the solution being diluted or boiled, an insoluble basic salt being
thrown down and normal sulphate left in solution.
O. Meister described a hydrate of this body deposited as

clinorhombic crystals from a mordant used in dyeing. They
were but sparingly soluble in the cold, and decomposed when
boiled. The formula was 2SO 3 Fe 2 O 3 I5H 2 O, and
, ,
12 out of
the 15 molecules of water were eliminated at 100 C.

basic sulphate
According to S. Umfreville Pickering, the only
of well denned composition obtained by the action of water on
.fi., u. o. un.
IOO THEORETICAL STUDY OF ALUMINIUM, IRON,
the normal sulphate is 2SO 3 Fe O 3, 2

. This sulphate forms double
salts with the alkali sulphates, for which its affinity is greater
than the normal sulphate, since it displaces the latter from the
alums.
S ^5
III. Basic Sulphate (5SO 3 , 3Fe 2 O 3 = (Fe 9) 3
(^ ).
This
I O4
compound is prepared by regulating the action of 3 on a HNO
mixture of ferrous sulphate and H 2 SO 4 a fresh addition of ferrous ,
sulphate being made as soon as the evolution of nitrous fumes

has ceased. The resulting dark red solution is unstable in pre-
sence of water, which breaks it up into normal sulphate and the
basic salt.
IV. Basic Sulphate (Fe2 O 3) 2 (SO 3) 5 = (Fe ) 2 2

^S^ 5
. A dark
solution of this salt is produced by gradually adding boiling

ferrous sulphate to a mixture containing 3 and H 2 SO 4 in HNO
suitable proportions ;
a little sub-salt separates during the opera-
tion. Asimilar solution of basic ferric sulphate (known in France
as " Rouil"\ largely employed as a mordant in dyeing, and the

manufacture of which will be examined in detail later on, is pre-
pared on a large scale in the same way, so as to obtain the same

S
ratio of Fe and SO 4 as in (Fe 2 ) 2
[(
4
\
4
V. Basic Sulphate (Fe 2 )J _ . This is obtained, as a red
U I 2
flocculent precipitate, by boiling a solution of ferri-potassium
sub-sulphate ;
it contains 3 H 2 O.
4
VI. Sulphate, (Fe 2 )J ~ ,
is formed by the action of air on
ferrous sulphate, or by an incomplete precipitation of ferric
sulphate with an alkali. Another way is by heating a dilute

solution of normal sulphate. The precipitate is red, turning
yellow on desiccation, and brown when anhydrous. This sub-
salt is employed for painting on
porcelain.
4
VII. Sulphate (Fe2 ) 4 | .
According to Anthon, this salt
I un
is produced by precipitating the normal sulphate with barium
AND COMPOUNDS OF THESE METALS IOI
acetate, barium sulphate being formed along with yellowish

flakes which can be separated by levigation.
4
VIII. Sulphate, (Fe 2) 7 j^ ,
has been found at Modum
[^20
(Norway) as a hydrated brown mass.
IX. Sulphate (F%Vp r\ - ^ n analysing a deposit of

U9 (
ochre-yellow basic salt produced in the manufacture of the above-

named basic mordant (Rouil\ the author obtained the following
proportions of ferric oxide and sulphur trioxide, after washing
and desiccation in air :
Found. Calculated.
S0 3 . . .
37-80 37-38
Fe2 O 3 . .
43-20 43-62
8roo
which correspond to the formula
C. DOUBLE SALTS. I. Ferri- ammonium Alum (iron alum),
(SO 4) 3 Fe 2) SO (NH
4 4) 2 , 24H 2 O. Cubo- octahedral crystals, or
octahedra, of iron alum (sp. gr. 1-712), are obtained by allowing

a mixture of ammonium sulphate and normal ferric sulphate to
crystallise from aqueous solution.
II. Ferri-potassium Alum may be prepared by crystallising a
mixture of the component sulphates, or by adding 3

to a HNO
solution containing 2 molecules of ferrous sulphate, I molecule
of potassium sulphate, and I molecule of H SO Also by treat-
2 4.
ing a mixture of KNO 3

and SO 4 Fe, 7 H O with H SO crystals of
2 2 4,
iron alum are obtained. take the form of regular octahedra,

They
are often of considerable bulk, and are of an amethyst-violet shade.
The following table gives the densities of solutions of this

alum, measured at 17-5 C.
IO2 THEORETICAL STUDY OF ALUMINIUM, IRON,
III. Various Double Salts. Double basic salts, such as
2(S0 4 2 ), K Fe 2 3
,
2S0 3 6H 2 O,
,
2(SO 4 (NH 4 ) 2 ), Fe 2 O 2SO 3 6H 2 O,

3) ,
5(S0 4 K 2 ), (Fe 2 3) 3
, (SO 3) 2iH 2 O,7,
may be obtained either by the action of ammonia on ammoniacal

or potassic iron alum, or by calcining these alums.
The salt SO 4 K 2, 4Fe 2 O 3 SO 3 9H 2 O has been found as
, ,
ochreous masses in Bohemian lignites and pale yellow masses;
of the corresponding sodium salt are met with in the aluminous

schists of Modum
(Norway).
A large number of double ferric salts, both of normal and
acid character, resulting from the union of 2 sesquisulphates,
have been brought to our knowledge by Etard. In order to
prepare them, he dissolves these sesquisulphates in a large

excess of H SO
2 4, and applies heat, accompanied by agitation,
until a precipitate is formed. This is collected on
glass wool
and washed with cold sulphuric acid, followed by glacial acetic
acid.
Ferri-aluminium sulphate occurs as microscopic, white, hex-
agonal lamellae, which are insoluble in water, and are gradually

decomposed thereby. The formula of this salt is (Al 2 )(SO 4) 6 Fe 2 ,
H SO
2 4, and may be represented by
/so,
/S0 \ 4
SO H 4 Al, -S0 - 4 Fe 2 -SO 4 H.
When heated, it is converted into the crystalline, colourless,

neutral salt (Al 2)(SO 4) 6 (Fe2 ).
The ferro-chromium compound (Fe 2)(SO 4) 6 (Cr2) is also known.
The acid compound (Fe 2 )(SO 4) 6 (Cr2), H 2 SO 4 is crystalline, yellow,
and insoluble.
The ferri-manganese compound (Mn 2 )(SO 4 ) 6 (Fe2 ) is crystalline,
of a handsome green colour, and is decomposed by hydrochloric
acid, chlorine being liberated.

49. Ferric Selenide (Fe 2 S 3) is obtained by passing selenium
vapour over red-hot iron, and fusing the product with an excess of
03
selenium and borax. This body has a metallic appearance, the
sp. gr. is 6' 3 8 ;

it is fusible, and decomposes in air.
50. Selenites of Iron. A. FERROUS SELENITE. The
method of preparation is by double decomposition.
The product forms a white precipitate, turning grey and
afterwards yellow when left exposed to the air.
B. FERRIC SELENITE, (SeO 3) 3 (Fe 2), is a white powder (yellow
after desiccation) obtained by double decomposition (Muspratt).
When heated it parts with water, and at a higher temperature
selenious anhydride is driven off, Fe 2 O 3 being left.
When iron is dissolved in an excess of selenious acid in
presence of HNO 3
a liquid is obtained which crystallises, on cool-
ing, in small, pistachio-green lamellae, consisting of (SeO 3 ) 3 Fe 2 ,
3Se0 2 .
On treating these salts with ammonia a yellow basic salt,
which passes through filter paper, is obtained.
51. Seleniates of Iron. A. FERROUS SELENIATE (SeO 4 Fe,

7H 2 O).
This salt is prepared by dissolving iron in dilute
selenic acid, hydrogen being liberated and a compound left which
at o crystallises like ferrous sulphate. At a higher temperature
it
crystallises like copper sulphate. It readily parts with its
water, and becomes opaque.

B. FERRIC SELENIATE, (SeO 4 ) 3 Fe 2 ,
is prepared by double
decomposition. It resembles ferric sulphate, and, like the latter,
furnishes basic salts.
52. Tellurites of Iron. A. FERROUS TELLURITE. Light

flakes, yellowish-grey in colour, obtained by double decomposition.
B. FERRIC TELLURITE. Pale yellow precipitate of low
stability, soluble in an excess of ferric salt.
54. Nitrides of Iron. Iron and nitrogen combine with

difficulty. On
exposure at red heat to the action of gaseous
ammonia, iron becomes white and brittle, and increases in weight
by i 2 to i
3 per cent., which corresponds to Fe 4 N 2 .
The best method of preparing iron nitride is by acting with

dry ammonia gas on anhydrous ferrous chloride heated to dark
redness in a porcelain tube. NH 4 C1 is liberated, a substance
which is decomposed by water into Fe 2 O 3 and
,
NH 3 sublimes,
and there remains in the tube a lustrous grey swollen mass

endowed with the same properties as the nitride prepared from
Fe and NH 3.
According to Rogstadius, when iron, reduced from the

oxalate, is carefully heated in ammonia gas, there results a dull
black mass which contains Fe 3 N 2 and which, when strongly
,
heated, gives off nitrogen and changes to Fe 6 N 2 .
When reduced to powder, iron nitride burns readily. On

calcination it gradually parts with its nitrogen, the final traces
being, however, difficult to eliminate. When heated in a current

of hydrogen it yields iron and ammonia ;
and at red heat, in a
current of steam, forms ferric oxide and ammonia. HC1 and

H SO
2 4 hydrogen being given off and a ferrous
dissolve the nitride,
salt formed together with an ammoniacal salt.
55. Nitrates of Iron. A. FERROUS NITRATE, (NO 3 ) 2 Fe".
This salt is prepared either by dissolving ferrous sulphide in cold
dilute nitric acid, or by double decomposition between barium
nitrate and ferrous sulphate, ferric nitrate being formed, together
with ammonium nitrate, when iron is dissolved in dilute nitric acid.
On evaporating neutral solutions of this salt at a low
temperature it forms crystals with 6H 2
O. It is a greenish salt
of low stability, dissolves in i part of water at o and in part
at 25 C., the latter solution having a density = 1*50. When
boiled, ferrous nitrate is converted into insoluble ferric nitrate,
the decomposition being facilitated by the presence of an acid.
VI
B. FERRIC NITRATES. I. Xormal Ferric Nitrate
(NO 3 ) 6 (Fe2 ) .
The method of preparation is by dissolving ferric hydrate in

HNO 3 or by attacking iron with nitric acid of sp. gr. ri5.
,
With weaker acid only ferrous nitrate or a mixture of ferrous-,

ferric-, and ammonium nitrates would be formed. The liquid
obtained by using acid of sp. gr. ri 15 is brown, and crystallises
with difficulty in consequence of the presence of a basic nitrate.
It is preferable, in order to obtain the crystallised nitrate, to take
an acid of sp. gr. i'332, and dissolve iron therein until the
density reaches 1*5 ; by this means colourless limpid crystals are

obtained on cooling. An excess of iron must be avoided, or the
product will consist of basic nitrates instead of the normal salt.
Normal ferric nitrate forms several hydrates, the most

common being that containing i8H 2 O, and separating out as
clinorhombic crystals when a concentrated solution is slowly
evaporated or cooled down. According to Ordway, the solution

should be an acid one, containing 3 molecules of water to 2 of
HNO 3
.
With a solution containing (NO 3) 6 Fe2 per 2(HNO 3 +H 2 O),

crystals with I2H 2 O are obtained, this hydrate being, accord-
ing to Scheurer-Kestner, always formed when the solution is
evaporated on the water bath, an operation resulting in super-

saturation. On cooling below zero C., a crystalline mass contain-
ing 2H 2 O is obtained, the mother liquor of which deposits
crystals with I2H 2 O.

Ordway observed a hydrate with 6H 2 O, but this lacks
further confirmation.
Commercial ferric nitrate, employed as a mordant in dyeing,
also deposits crystals with 1 2 HO

2 when concentrated to
50 B.
The nitrate containing i8H 2 O melts at 47-2, and boils, with
decomposition, at 125 C. ; sp. gr. in the crystalline state, r6835,

that of the melted salt being 1-6712. When mixed with sodium
sulphate and dissolved in water the temperature of the solvent is
reduced.
The following table gives the density of solutions of ferric
nitrate of different strength, measured at 17-5 C. (Franz):
Density.
I -0100 34 per cent.
I '0320 36
I -0472 38
I '0620 40
I -0770 42
I
-0934 44
1-1098 46
1-1268 48
1-1440 5
I'l6l2 52
1-1812 54
I '2012 56
I-22I2 58
60
I '2622 62
1-2838 64
II. Basic Nitrates. Various basic nitrates are obtainable by

dialysis, but their composition varies with the duration of the
operation.
When a saturated solution of iron in nitric acid is prepared,
basic salts are always produced, and to obtain the normal salt the
proportions should be regulated according to the equation

8HNO + 2Fe = (NO 3 3) 6 Fe 2 + 2NO + 4H 2 O.
The basic nitrates cannot be crystallised, and, moreover, their
presence prevents the normal salt from crystallising.

When normal ferric nitrate is treated with sodium carbonate,
or employed to dissolve ferric hydrate, a nitrate is obtained which
is soluble in water and alcohol, may be precipitated by nitric acid,
and corresponds to the formula

Fe 2 3,
2N 2 5
= 2[(N0 3) 6 (Fe )], Fe O 3
2 2 .
On dissolving ferric hydrate in the normal nitrate, in any

desired proportion, the salt
Fe 2 3, N 2 5
= (N0 3) 6 (Fe 2 ),
2 Fe 2 O 3 = (NO 4) 2 (Fe 2 r
is obtained, representing the orthonitrate, derived from ortho-
/7/
nitric acid (NO 4) H, corresponding to phosphoric acid (PC^y'Hg.
The action of boiling water on these nitrates, or on the
normal salt, results in the formation of
(1) 2Fe 2 3, N 2 5 + H = (N0

2 3) 6 (Fe 2), 5 Fe2 O 3 +3H 2 O,
(2) 3 Fe 2 3,
N 2 5 + 2H = (N0 2 3 )6 (Fe2 ), 8Fe2 O 3 + 6H O, 2
(3) 4 Fe2 3,
N 2 5 + 3 H = (N02 3) 6 (Fe2 ), i iFe 2 O 3 + 9H O. 2
These nitrates are ill defined and uncrystallisable, and their

method of preparation in itself indicates that a whole series of
analogous bodies of variable composition can be obtained.

When solutions of ferric nitrate are boiled, they part with
nitric acid and deposit a more highly basic nitrate.
If the elimination of nitric acid be prevented by heating the

liquid in a sealed tube, the colour changes to brick-red, and a
modified hydrate can be precipitated. A similar result is brought
about by the action of light.
56. Phosphides of Iron. A number of these have been

described, but, according to C. Freese, the only ones that can be
regarded as definite compounds are Fe 3 P 4 Fe 2 P 2 and Fe4 P 2 , ,

.
All these phosphides are soluble in nitrohydrochloric acid,

AND COMPOUNDS OF THESE METALS IO7
and nitric acid, with liberation of phosphoric acid. Dilute hydro-

chloric and sulphuric acids dissolve them but slowly, phos-
phoretted hydrogen being formed. They are only slightly
fusible, and when heated in the air are converted into the corre-
sponding phosphates, except in the case of Fe 3 P 4 which commences

,
by giving off phosphorus.
Phosphites
57. of Iron. ^.FERROUS PHOSPHITE
(FeHPO 3). This salt is prepared by precipitating ferrous
sulphate with phosphorus trichloride, neutralising the liquid

with ammonia, washing the precipitate with boiling water, and
drying in vacuo. It is readily oxidised, and decomposes, when

heated, with incandescence and evolution of hydrogen.
FERRIC PHOSPHITE, (Fe 2 )H 3 (PO 3) 3 is prepared by treat-
B. ,
ing ferri-ammonium sulphate with a mixture of ammonia and

phosphorus trichloride. The white precipitate first formed is
re-dissolved, but finally reappears ;
it should be washed with
cold water and dried in vacuo. It contains 9H 2 O, and, when
heated, decomposes, with emission of light.
58. Hypophosphites of Iron. A. FERROUS HYPOPHOS-

PHITE. Prepared by dissolving iron in pyrophosphorous acid
out of contact with air. On evaporation in vacuo the solution
deposits a crystalline mass containing FeH 4 (PO 2) 2 .
B. FERRIC HYPOPHOSPHITE, (Fe 2 )H 12 (PO 2) 6 prepared , by

dissolving ferric hydrate in cold hypophosphorous acid, is a
white salt only sparingly soluble.
59. Phosphates of Iron. A. FERROUS PHOSPHATES.

I.
Phosphate. Fe 3 (PO 4 ) 2 is derived from orthophosphoric acid,
H PO 3 4 and is obtained as a voluminous, white, gelatinous precipi-
,
tate on adding sodium phosphate, drop by drop, to a ferrous salt.

It oxidises rapidly, and turns blue in so doing. It may be
prepared, containing I molecule of water, by the action of water

at 50 C. on di-ferrous- phosphate, and in this condition forms
small dark green crystalline grains.

This phosphate is insoluble in pure water, but soluble in acidi-
fied water, and slightly so in water charged with carbon dioxide.
nature known under the names of vivianite, triplite, etc.
it is
The phosphate FeHPO 4 is obtained, as a semitranslucent
tin
white powder, by the imperfect precipitation of ferrous sulphate
by disodic phosphate, or boiling together phosphoric acid and

iron. In the latter case the precipitate consists of small colour-
less needles, which turn blue in air and contain FeHPO 4 +H O. 2
Erlenmayer obtained the phosphate
Fe+2H O 2
by dissolving iron in 48 per cent, phosphoric acid. It forms a
green solution, which on addition of water deposits a white
amorphous precipitate. When the solution is concentrated in

an atmosphere of hydrogen there separates out a crystalline
incrustation, which, on being washed with ether, resolves into i
a crystalline white powder of the formula
PO.H,/'
II. Ferrous Pyrophosphate (P 2 O 7 Fe" 2 ). ,
This salt is derived
from pyrophosphoric acid, P 2 O 7 ,

H 4 .
Sodium pyrophosphate gives with ferrous salts a white pre-

cipitate which changes in air, is insoluble in water, but soluble
in dilute acids, ammonia, or in an excess of the ferrous salt or
of an alkali pyrophosphate.
On a mixture of ferrous sulphate and sodium
agitating
'
phosphate with ammonia, a flocculent precipitate of ammoniacal

pyrophosphate is formed, changing into crystalline flakes which
are white when dried in vacua. If a ferrous salt, saturated with
nitrogen dioxide, be treated with sodium phosphate a brown

precipitate of ferrous nitropyrophosphate, P 2 O 7 Fe 2 -f NO, is
formed. This precipitate absorbs oxygen from the air and

turns white, being converted into a mixture of ferric phosphate
and ferric nitrate.
B. FERRIC PHOSPHATES. I. Phosphate, (PO 4) 2 (Fe 2 ) + 4H 2
(ferric orthophosphate),obtained by precipitating a solution of

is
ferric chloride by ordinary sodium phosphate. This precipitated
phosphate is soluble in HC1, 3 citric acid, HNO

or tartaric , acid,
but insoluble in sodium phosphate or phosphoric acid. It
readily dissolves in water charged with carbon dioxide.

II. Phosphate, (P 2 O 7 ) 3 (Fe 2) 2 (ferric pyrophosphate), is obtained
AND COMPOUNDS OF THESE METALS IOQ
in precipitating sodium pyrophosphate with ferric chloride. The

precipitate is soluble in sodium pyrophosphate, provided the
ratio Fe 2 Cl 6 3P 2 O 7 Na 2 has not been attained; but when the

:
proportion 2Fe 2 Cl 6 3P 2 O 7 Na 2 is reached, precipitation is com-

:
,
plete and the solution no longer contains iron. The precipitate

is soluble in a large excess of Fe 2 Cl 6 .
The above data indicate the existence of a sodium ferric salt
Na6
and ferric pyrophosphate (P 2 O 7 ) 3 (Fe 2 ) 2 . This double salt, how-

ever, has not been isolated.
Ferric pyrophosphate is soluble in acids, but the solution is
re-precipitated by boiling. The precipitate has the same com-

position as the original salt, but is no longer soluble in dilute
acids, though soluble in ammonia.

Ferric pyrophosphate is used in medicine, the phosphate
of the German Pharmacopeia containing I or 2 molecules of
sodium pyrophosphate in excess, and having the presumptive
formula
Rieckher prepared the corresponding ammoniacal salt, con-
taining ioH 2 O.
C. VARIOUS FERRIC PHOSPHATES. I. Phosphate (PO 4 H) 3
(Fe) 2 + 2-|H 2 O (ferric triphosphate). This salt was mentioned
by Rammelsberg, who obtained it in the form of cubic crystals
by leaving a saturated solution of the normal salt in an excess

of acid for a year. Millot prepares it by dissolving ferric oxide
in an excess of phosphoric acid, diluting with water and boiling.
The crystalline white precipitate re- dissolves slowly in the mother
liquor on cooling. The calcined salt is insoluble in acids.
4 2 2
II. Phosphate, ^
\Fe + 5 H O
2 2 (ferric tetraphosphate),
is formed by the action of air on the acid ferrous phosphate,

IIO THEORETICAL STUDY OF ALUMINIUM, IRON,
It was obtained by Erlenmayer, as bright red quadratic

crystals, by the spontaneous evaporation of triferric phosphate
in an excess of phosphoric acid. These crystals are unaltered
by air and insoluble in cold water, but are decomposed by boil-
ing water into phosphoric acid and triferric phosphate.

Millot prepares this salt by dissolving ferric hydroxide in
phosphoric acid.
(PO 4 H ~2) "2 \
Erlenmayer obtained the salt ,
pn as a rose-red
;5 /^>(Fe 2 ).,,
crystalline powder, by concentrating a solution of acid ferrous
phosphate in the air.
III. Phosphate (PO 4 2 ) 6 (Fe 2 )

H
(ferric hexaphosphate). To
prepare this phosphate, ferric hydroxide is added to a 48 per
cent, solution of phosphoric acid until a white deposit is pro-
duced ;
the solution then contains 1 4PO 4 H 3 per Fe 2 O 3 . On
evaporating it on the water bath there is formed a crystalline
incrustation, which, when washed with ether, yields a rose-red
powder that decomposes, on exposure to air, into

crystalline
phosphoric acid and a less acid phosphate, 2P 2 O 5 Fe.>O 3 , ,
8H 2 O.
Cold water converts ferric hexaphosphate into a nearly neutral
phosphate,
Fe)
(P0 4 H) 3 / (
which is also obtained when the above-mentioned solution, con-

taining I4PO 4 H 3 per Fe2 O 3 is poured into 21 times its own
,
volume of boiling water. With cold water the same solution

furnishes a yellowish-grey precipitate containing
(P0 4) 4
(PO 4 H)3 / (
With alcohol the salt
is obtained.
Boiling water decomposes all these salts in converting them

into forms more and more approximating to the normal phosphate
(P0 4) 2 (Fe2 ).
AND COMPOUNDS OF THESE METALS I I I
IV. Basic Ferric Phosphates. On precipitating acid solutions

of the foregoing acid phosphates by ammonia there results the
basic phosphate 2(PO 4 ) 2 (Fe 2 ),Fe 2 O 3 -f 8H 2 O, which is characterised

by its insolubility in ammonium citrate and solubility in ammonium
oxalate.
If ammonia be added to the acid solution of this basic salt
the phosphate (PO 4) 2 (Fe 2 ), Fe 2 O 3 is obtained ;

this is only
sparingly soluble in ammonium citrate or oxalate.
A natural basic phosphate, occurring as a brown mass with

the composition (PO 4) 2 (Fe2), Fe 2 O 3 + i 2 or 24.H 2 O, is met with
at Bernau (France) and in Mauritius.
60. Arsenides of Iron. Arsenic combines with iron in
several proportions, forming bodies harder, more brittle, and

more fusible than iron itself. When heated, the arsenides of iron
yield an arsenical sublimate ; and, when roasted in the air, furnish

arsenious anhydride and a magnetic residue. They are soluble
in nitric acid and in aqua regia.
6 1. Arsenites of Iron. A. FERROUS ARSENITE (FeH,
AsO 3 ).
This is a white precipitate, soluble in NH 3, oxidising
rapidly in air to an ochreous yellow substance, and is prepared
by treating ferrous sulphate with ammonium arsenite. When
calcined it parts with water and arsenious anhydride, a rust-
coloured residue being left.
FERRIC ARSENITE (Fe2 ) VI (AsO 3) 2

B. Potassium arsenite .
gives with Fe 2 Cl a rust-coloured precipitate consisting of an

arsenite more basic than the normal salt. The same basic salt
is formed on digesting ferric hydroxide with arsenious anhydride
and water; and the insolubility of this compound explains the
action of freshly prepared ferric hydroxide as an antidote for
arsenious acid poisoning.

62. Arsenates of Iron. A. FERROUS ARSENATE (FeHAsO 4 ).
This is obtained, as a white precipitate, on treating ferrous
sulphate by ammonium arsenate. It rapidly turns a dirty green
colour in changing into ferro-ferric arsenate. When heated it
loses arsenious acid, and leaves a residue of ferric oxide and ferric
arsenate. It is sparingly soluble in NH 3.

VI
B. FERRIC ARSENATES. The neutral arsenate (AsOJ 2 (Fe 2 )
is obtained on oxidising the ferrous salt by nitric acid and pre-
cipitating the solution by ammonia.

This arsenate when heated to redness becomes suddenly in-
candescent. Only a portion of the arsenic acid in this salt can

be removed by caustic potash and ;
in order to effect complete
decomposition, digestion with ammonium sulphide is necessary.

The acid arsenate (Fe2 )
VI
H 3 (AsO 4 ) 3 + 4|H 2 O is a white powder
insoluble in water. When heated it parts with water, becomes
red, and subsequently yellow, by changing into pyro-arsenate,
(Fe2 ) 2 (As 2 7) 3
.
Several ferric arsenates are met with in nature, among them

being
Eisensister :
VI
(Fe 2 ) (AsO 4) 2 + Fe H O + 9H O 2 6 6 2 ;
Scorodite :
VI
(Fe2 ) (AsO 2 )
2
+ 4H O 2 ;
Wurfelera: (Fe") 3 (AsO 4) 2 + 2[(Fe v '(AsO + 2) 4) 2 ]

v
4 (Fe 2 ) 'H fl
O6
+ i8H 2 O.
63. Sulpharsenites of Iron. A. FERROUS PYROSULPHAR-
SENITE (Fe" 2 As 2 S 5 ). This is a blackish-brown precipitate dis-
solving to a yellow solution in an excess of alkali sulpharsenite.
When heated it parts with arsenic, a residue of ferrous sulphide
being left.
B. FERROUS SULPHARSENITE. An olive-green precipitate
soluble in an excess of the precipitant, fusible, and decomposed at
red heat, leaving behind a residue of ferrous sulphide. Berzelius
gives it the formula Fe2 S 3 (As 2 S 3) 5 .
64. Sulpharsenates of Iron. A. FERROUS PYROSULPH-

ARSENATE (As 2 S 7 )Fe" 2 A
dark brown precipitate, soluble in an
.
excess of the precipitating reagent. It decomposes on desic-
cation.
B. NORMAL FERRIC SULPHARSENATE vl

(Fe 2 ) (AsS 4 ) 2 . A
greenish-grey, flocculent precipitate, readily soluble in an excess
of alkali sulpharsenate.
65. Carbides of Iron. In a state of fusion iron combines

direct with carbon, forming a series of carbides. When the
carbon is in excess it dissolves in the molten metal, but a portion
separates out, on cooling, in the form of crystallised graphite,
which remains embedded in the metallic mass.
The carbide Fe3 C (cementite, normal carbide, carbide of white

cast iron, cementation carbide) is the only definite iron carbide
known (H. le Chatelier, Revue generate des Sciences, Jan. 15,1 897).
Owing to its tendency to split up at high temperatures into iron
and graphite, cannot be prepared by fusing the metal in presence
it
of carbon. Marguerite obtained it by heating finely divided

ferric oxide to incipient redness in carbon monoxide. Abel,
Muller, and Arnold, by treating tempered steel and white cast
iron with suitable reagents, extracted metallic scales of a very
high degree of hardness, corresponding to the formula Fe 3 C.

The calcination of ferrocyanides furnishes a carbide contain-
ing C 2 Fe in the form of a readily ignitible black- powder.

Prussian blue yields on calcination another carbide correspond-
ing to C 3 Fe 2 .
The different grades of cast iron and steel are nothing more
than iron carbides of variable composition.
66. Carbonates of Iron. A. FERROUS CARBONATE (FeCO 3).
Metallic gradually dissolved by water charged with
iron is
carbon dioxide, ferrous carbonate being formed. By passing a

current of CO 2
for several hours through water containing in
suspension iron reduced by hydrogen, a solution of ferrous car-

bonate (0*91 grm. per litre) is obtained.
Hydrated FeCO 3 is obtained by double decomposition, as a
voluminous white precipitate which oxidises and turns brown in
the air. It is insoluble in water, but dissolves, as a bicarbonate,
in water charged with CO 2 . This solubility varies inversely with

the temperature, the saturated solution containing i'39 grms. of
ferrous carbonate per litre at I5C. whilst at 24
;
C. not more
than 0*098 grm. is present. On driving off all the CO 2
the
whole of the FeCO 3 is precipitated. thrown down by It is also
alkali carbonates, though the bicarbonates have no such action.
Chlorides and sulphates appear to impart stability to the solution.

Ferrous carbonate is met with, in nature, in a crystalline or
amorphous state (siderose, spathic iron), and forms one of the

best ores of iron. When calcined it gives off carbon monoxide
and carbon dioxide, a residue of intermediate magnetic oxide
being left.
8
B. FERRIC CARBONATE. The normal salt has not been

isolated, attempts to prepare it by double decomposition resulting
in the production of the hydrate containing more or less CO 2.
Alkali bicarbonates dissolve ferric hydroxide to a red solution,
precipitable by boiling, and from which ferric hydroxide is separ-

ated by alkalis.
67. Sulphocarbonates of Iron. A. FERROUS SULPHO-

CARBONATE (FeCS 3). When an alkali sulphocarbonate is added
to ferrous sulphate a red liquid, gradually becoming almost black,
is obtained. An excess of sulphocarbonate deepens the colour of
the solution, whilst an excess of the ferrous salt throws down the
compound in the state of a black powder.
B. FERRIC SULPHOCARBONATE is a dark brown precipitate
collecting in granules insoluble in water. Under the influence of

heat it parts with sulphur and carbon disulphide, ferrous sulphide
being left.
68. Iron Nitrosulphocarbonate (Fe,S(NO) 6 CS 2 , + 3H 2 O).
This body is related to the nitrosulphides of Roussin. It was

discovered by O. Lcew, and
prepared by gradually adding and
is
stirring a mixture of dissolved sodium sulphocarbonate and nitrite

to a solution of ferrous sulphate, the whole being then raised to
boiling and filtered. On cooling, black needles are obtained,

which are purified by re-crystallising in water and ether, and
correspond to the formula Fe 4 S(NO) 6 CS 2 3H 2 O. These crystals
, ,
are soluble in water, alcohol, ether, etc. The aqueous solution is
black, and yields up its salt to ether. When kept for some time
the crystals lose water and nitrogen dioxide.
Acids and alkalis have little effect on the solution in the cold ;
but in the warm, alkalis liberate ammonia and precipitate ferric

hydroxide, a new class of alkali salts being formed at the same
time.
Potassium cyanide converts iron nitrosulphocarbonate into
alkali nitrocyanide. O. Lcew regards this nitrosulphocarbon-
ate as the nitro-demvative of a hypothetical sulphocarbonate,
Fe,S 4 CS 2 .
69. Silicates of Iron. Normal ferrous silicate (SiO 4 Fe2) is
formed ^during the refining of cast iron. It is very fusible, and

AND COMPOUNDS OF THESE METALS I I
susceptible to attack by acids, and occurs either in amorphous

masses or as grey crystals of metallic aspect.
When a crystal of ferrous sulphate is introduced into a
solution of potassium silicate, partially carbonated, it becomes
covered with a grey vegetation (tree of Mars), which contains
basic ferrous silicate and potassium carbonate in the proportion
of 2K CO 32
to 3Fe" 2 SiO 4 6FeO. This product is insoluble in
,
water ;
on exposure to the air it oxidises and is transformed into
ferric silicate (Fe 2 ) 2 (SiO 4 ) 8 + 4Fe 2 O 3 .
Silicates of iron are abundant in nature.

70. Iron Boride is obtained on reducing the borate by
hydrogen. It is a hard white body dissolving in acids to form
boric acid and a ferrous salt, hydrogen being liberated. Boiling
water decomposes it into boric acid and iron.
71. Borates of Iron. A. FERROUS BORATE. This is
obtained by double decomposition, and appears to correspond to

the formula BO 2 Fe, but loses boric acid when washed.
B. FERRIC BORATE. This salt forms an insoluble yellow
powder, turning brown on calcination and vitrifying at a bright
red heat.
3. IRON ORES
72. Anhydrous Oxides. A. FERRO-FERRIC OXIDE. I.
Magnetic Oxide (magnetite) (Fe 3 O 4 ) consists of ferro-ferric oxide,
frequently associated with small quantities of titanium, manganese,

and magnesium.
FIGS. 36, 37, and 38. Ferro-ferric oxide.
Magnetite occurs as isolated crystals or in granular masses,

lamellar or compact, or as rounded grains. It is of a dark iron-
grey colour, lighter in the case of the crystals, which have a
brighter lustre. The powder is black.

Il6 THEORETICAL STUDY OF ALUMINIUM, IRON,
This oxide is found almost exclusively in the crystalline
metamorphic rocks frequently in considerable masses, as at

;
Taberg in Sweden, and Blagodat in the Ural, where it forms

veritable mountains.
It is extensively mined, and forms the best iron ore for high-
class steel. It occurs disseminated in the form of small grains
in many schistous rocks and in the majority of the eruptive rocks.

The finest specimens of crystals are obtained at Traverselle in
Piedmont, and at Normark in Wermeland.
Magnetite is soluble in HC1. It fuses with difficulty before
the blowpipe ;
in the oxidising flame
it loses its magnetic properties ;
with
fluxes it gives the reactions for iron.
Magnetite will scratch fluor spar, but
is itself scratched by quartz. The degree
of hardness is 5'5 to 6; sp. gr., 5 to 5*2.
It is highly magnetic, and crystallises
FIG. 39. Magnetite. n the cubic system, regular octahedra
j
being the most general form, though sometimes it occurs as

rhomboidal dodecahedra or a combination of these two forms
with the icositetrahedron, the trioctahedron. The cube facets
are rare.
B. FERRIC OXIDE. I. Haematite (syn. Specular iron, red :
oxide, oligistic iron) (Fe 2 O 3)

is most frequently met with as
crystals, or lamellar or scaly masses. The colour is steel-grey
with a metallic lustre, and the crystals have an iridescent surface.
In thin plates it is translucent, and the powder is red.
Haematite is one of the most abundant minerals. The
crystalline variety belongs principally to the crystalline rocks,
where it is found in veins or in masses, associated with quartz, in
Sweden, Norway, the Ural Mountains, on the island of Elba, etc.
In Brazil it constitutes a true rock (itabirite) formed of a mixture
of haematite and quartz. In the volcanic rocks it is met with as
lustrous plates.
The compact and fibrous varieties form deposits at the contact
of gneiss or granite with liassic or other limestones. They are
found in certain strata of primary or secondary rocks, such as the
red sandstones, Vosgian sandstones, etc. This oxide also enters

into the composition of ochre.
FIG. 40. Oligistic iron FIG. 41. Oligistic iron "FiG. 42. Oligistic iron
(haematite). (Primi- (haematite). (Primi- (haematite). (From
live basal form. )
tive and rhombo- the Altenberg mines. )
hedral.)
The sp. gr. is 5-2 to 5-3 ; hardness, 5-5 to 6*5. It is soluble
in boiling concentrated HC1, is infusible in the oxidising flame,
and but slightly fusible in the reducing flame, in which it is
converted into magnetite.
FIG. 43. Haematite (Framont). FIG. 44. Haematite (St. Gothard).
The crystalline form is that of the rhombohedron (86 10'),

but is rarely met with unmodified.
FIG. 46. Haematite

^Mont-Dore).
FIG. 49. Haematite

(primitive based by
facets of the equiaxial
FIG. 47. Haematite. FIG. 48. Haematite (Elba). rhombohedron).
Il8 THEORETICAL STUDY OF ALUMINIUM, IRON,
The name of martite has been given to haematite, crystallised

in octahedra and resulting from a pseudomorphosis of magnetite
into haematite. Some mineralogists, however, have regarded
haematite as actually dimorphous.
II. Ilmenite is composed of ferric oxide (Fe 2 O 3), in which a
portion of the Fe is replaced by Ti. It occurs in rhombohedral
crystals resembling those of haematite ; frequently also

in lamellae flattened parallel to the base ;
and sometimes
in very pointed rhombohedra, iron-black in colour and
of faintly metallic lustre. The fracture is plain.
Ilmenite is found in granite rocks, sands, etc. It is
soluble with difficulty in HC1, and the solution turns

blue when boiled with tin. With sodium, ammonium
phosphate, and tin, in a reducing flame, it gives the
FIG. 50. violet coloration of titanium.
Ilmenite.
Hardness, 5 to 6 ; sp. gr., 4-5 to 5.
73. Hydrated Oxides. A. LIMONITE, or brown haematite,

is a natural ferric hydroxide (2Fe2 O 3 3H 2 O), and an extremely ,
abundant ore of great importance. It occurs as fibrous limonite,

in kidney-shaped concretions, or in masses with a lustrous black
surface, or again in compact dark brown masses, of plain fracture,
as veins in the older rocks and in contact deposits (Pyrenees,
Isere, etc.).
The pisolitic ore is found in globules, with a compact
fracture, disseminated in the clays of the middle tertiary deposits,
or cemented by an argilo-calcareous paste. Such deposits fre-
quently cover the plateau of Jurassic limestone or chalk they ;
are common in the districts of Berry, the Bourbonnais, Lorraine,
Franche-Comte, etc.
The oolitic ore is found in smaller grains than the preceding
variety. These agglomerated together, form rocks

grains, often
that for the most part are situated at the base of the oolitic lime-
stones. This ore contains fossils, and is of lower value than the
pisolitic variety. It is worked in the departments of Gard,
Ardeche, Aveyron, Cote-d'Or, Jura, Haute-Marne, etc.
Earthy Limonite has a smooth fracture, and is often highly
argillaceous. It is found in various secondary and tertiary rocks.

AND COMPOUNDS OF THESE METALS IIQ
Bog Ore contains a large proportion of phosphorus, and

furnishes a phosphoric cast iron.
Limonite is soluble in acids, and frequently leaves a
siliceous residue. Heated in a tube it gives off water.
The dust is yellowish brown. Hardness, 5 to 5*5 ; sp. gr.,
3-6 to 4.
The following table gives the results of analyses performed on
several varieties of limonite :
B. GCETHITE (lepidocrocite, pyrrhosiderite). This is a ferric
hydroxide (Fe 2 O 4 H 2 ), occurring as longitudinally striated crystals,

as crystalline lamellae, in scales, or fibrous masses
of a brown, yellow, or red colour. It isfound along
with other iron ores, but more particularly near
Siegen and in Cornwall.
The crystalline form is the orthorhombic prism,
7; = 94 52',
1
/2
1
/2
= 121 4', ^Yz^Va in front 126
f
1 8'. Cleavage, g perfect.
C. TURGITE (hydrohaematite) is another ferric
hydroxide (2Fe 2 O 3 ,
H 2 O), forming
an abundant ore
of iron, resembling limonite, but harder, and yielding a paler
red powder. When heated in a tube it decrepitates and gives
off water.
74. Iron Spinels. A. FRANKLINITE is a spinel of iron,

zinc, and manganese
RR O 2 4 ;
R = Fe, Zn, Mn ;
R 2 = Fe Mn 2, 2,
occurring in octahedral crystals or in granular or compact

black masses, accompanying red zinc oxide in a crystalline lime-

stone at Hanbury (New Jersey).
This body is soluble in HC1; it is infusible before the blow-
pipe. With borax it gives an amethyst-violet bead in the oxidis-

ing flame, and a bottle-green bead in the reducing flame.
The degree of hardness varies between 5 '5 and 6'5, and the
sp. gr. between 5*6 and 5*9. The powder is brownish red. The
crystalline form is the regular octahedron, modified by facets of
the rhomboidal dodecahedron.
75. Sulphidic Ores. A. PYRRHOTINE (hepatic pyrites,

magnetic pyrites) approximates in composition to Fe 7 S 8 This .
sulphide is occasionally met with as very fine flattened hexagonal

crystals more frequently in lamellae or compact masses with a
;
faint metallic lustre, yellow or bronze, and conchoidal fracture.
It occurs at Konigsberg, Modum, Snarum (Norway), Andreas-

berg (Hartz), and Bodenmais (Bavaria). It frequently contains
nickel, and then forms an important ore of that metal (Varelle,
FIG. 52. Magnetic pyrites. FIG. 53. Fyrrhotine.
Piedmont, etc.). The specimens of crystals come from the

finest
gold mines of Moro-Velho (Brazil). Pseudomorphic forms are

met with in pyrites, limonite, and siderose.
This mineral is soluble in acids. Heated in open tubes it
gives off sulphur dioxide, and on charcoal it furnishes a black
magnetic mass which, in presence of a flux, gives the reactions of

cobalt and nickel.
The hardness is 3' 5 to 4^5 ;
the sp. gr., 4/4 to 4-7.
Magnetic pyrites crystallises in the form of a regular hexagonal
prism, in which one of the sides of the base is nearly equal to the
height. The crystals exhibit cleavages parallel to the 6 facets of
the prism and one in the direction of the base, the latter being
particularly definite.
B. TROILITE consists of ferrous sulphide in grains or nodules

of various sizes cemented in meteoric iron. It exhibits an
unequal fracture.
FIGS. 54 to 57. Crystals of pyrites.
C. PYRITES (yellow sulphide of iron). Pyrites consists of the

iron sulphide FeS 2 . It is nearly always crystalline, but is occasion-
ally met with in concretion as

compact, globular, stalactitic, granular,
pseudomorphic masses, modelled on crystals of other substances
or on fossils. The crystals are often very handsome, of a golden-
yellow colour with a fine polish and a bright metallic lustre.
Pyrites is abundantly distributed throughout nearly all geo-
logical ages. Occasionally it has undergone modification into

limonite. It is mined in considerable quantity at Chessy (near
FIG. 58. Cubo-dodecahedral pyrites, FIG, 59. Pyrites from a Cumberland mine.
Lyons), etc., as a sulphur mineral and for sulphuric acid
manufacture.
Pyrites is unacted upon by hydrochloric acid, but is dissolved

by nitric acid, with separation of sulphur. When heated in a
tube it yields sublimed sulphur and a magnetic residue, and on
carbon it burns with a blue flame. It strikes fire with steel.
The degree of hardness is 6 to 6'5 ; sp. gr., 4*8 to 5*2; fracture,
unequal or conchoid ; texture, brittle. The powdered substance is
of a greenish-grey colour.
The crystals of pyrites belong to the cubic system, but are
affected by hemihedry with parallel facets. This hemihedry is
generally manifested, even on the cubes, by striae, which on each

facet are parallel to two opposite sides of the face in such a
FIGS. 60 and 61. Crystals of pyrites.
manner as to be mutually perpendicular in three adjoining facets.
In addition, the octahedron a 1 is frequently encountered, often
modified by faces of the pentagonal dodecahedron b z and forming ,
b2
the icosahedron a 1 when the forms equilibrate. The pentagonal
dodecahedron ft is very frequent, as well as hemihexoctahedron

l 5 3 4
with parallel faces (b\ t>
/3, ^/,), etc. The faces b\ P, & J2,
t>
/.2 , /3,
6
t>
/5 (the two latter frequently the reverse of the dodecahedron b"-\
1 l
(b\ & J 5 , JVin), (b\ d / 5)
J 1 /*), (b\
P/ B P/i), etc., are also met with. ,
The cube is almost invariably the general form, despite the

number of facets with which the crystals are often surcharged.
Groupings of crystals parallel to the faces of the cube or of
the octahedron are also known occasionally two crystals inter- ;
sect each other in two rectangular positions.

D. MARCASSITE or white pyrites is composed, like the pre-
ceding variety, of FeS 2 It . is

yellowish or greenish -white in
colour with a metallic lustre,
FIGS. 62, 63, and 64. White pyrites.
and occurs as crystals in veins, or as balls or fibrous renal

masses of radial structure disseminated in clays, marls, chalk, etc.;
AND COMPOUNDS OF THESE METALS I2 3
or again, in particles (often imperceptible) in schists, lignites,

coal, etc. Its property of rapidly oxidising in air causes it to
be worked in large quantities for the manufacture of ferrous
sulphate or alum. The aluminous schists
or containing marcassite are
lignites
attacked by the sulphur dioxide resulting
from the decomposition of this sulphide
and its conversion into ferrous sulphate.
FlG. 65. Marcassite. Group-
This pyrites is also met with in imi- ing of crystals known as
" Crete de "
. ,
j . .
, i r coq (cockscomb).
tative dendritic or pseudomorphic forms.
It is insoluble in HC1, but attacked by HNO 3. Healed in a
closed tube it furnishes a sublimate of sulphur. The hardness is
6 to 6 -
5 ; sp. gr., 4/6 to 4'8 ; fracture, unequal; colour of the

powdered substance, greenish grey.
The crystalline form is the orthorhombic prism, the most
frequent shapes being prismatic or octahedral. The crystals
are often macleated parallel to m, so as to form pentagonal
lenticular masses.
E. CHALCOPYRITE (cupreous pyrites). This

is a sulphide of iron and copper (Cu 2 S, Fe 2 S 3 ),
which forms one of the most abundant ores of the
latter metal. It occurs in compact concretionary
masses, or as octahedral or tetrahedral crystals,

of a deep golden-yellow colour with an iridescent
reflection ;
in veins embedded in gneiss, argilla-
FIG. 66.
ceous schists, etc. The crystalline form is the
Chalcopyrite.
quadratic octahedron.
76. Sulphatic Ores. A. MELANTERITE (green vitriol) con-
sists of ferrous sulphate (FeSO 4 7H 2 O). ,
It occurs as clear
crystals, or as fibrous or concretionary masses resulting from

the decomposition of pyrites. It changes and turns brown on
exposure to air. The hardness is 2 ; sp. gr., 1*8 to 2 ;
and the
crystalline form is the clinorhombic prism.
B. FlBRO-FERRITE (stypticite). This is a hydrated ferric
sub-sulphate (3Fe 2 O 3 , 5SO 3 + 27H 2 O), occurring as masses or

fibrous bundles,' translucent, pale yellow or greenish, and with
a silky lustre.
It is insoluble in water. When heated in a tube it liberates
water and (at a high temperature) sulphur dioxide and sulphur

trioxide, leaving a residue of ferric oxide.
C. COPIAPITE is also a hydrated ferric sub -
sulphate,
2Fe 2 O 3 , 5SO +i8H 3 2 O, forming hexagonal, tabular, fibrous or
yellow granular masses, and is found in the Copiapo copper
mines (Chili).
D. COQUIMBITE is another hydrated ferric sulphate, of the
formula Fe 2 O 3 , 3SO 3 + 9H 2 O, and is a yellowish
- white salt
completely soluble in water. It crystallises in hexagonal tables,
cleaving parallel to the base, or occurs in granular masses. The

hexagonal prisms are frequently modified at the basal edges.
E. BOTRYOGENE (red vitriol). A hydrated ferro - ferric
sulphate containing magnesia lime, and forming small and

crystals or botryoid masses, red to brown in colour, and found
incrusting gypsum or pyrites in the mines of Fahlun.

This salt is partly soluble in water, leaving an ochreous
residue. The hardness is 2 to 2'5 ; sp. gr., 2^04 ; crystalline
form, the clinorhombic prism.

77. Phosphatic Ores. A. VIVIANITE (phosphatic iron).
Vivianite is hydrated ferrous phosphate ; formula, (PO 4) 2 Fe 3 ,
8H 2 O. It forms more or less elongated light

blue prismatic crystals, frequently modified, and
then presenting a blackish appearance. It is
transparent, tender, and flexible.
Vivianite is often found associated with
pyrrhotine and chalcopyte in the stanniferous

veins of St. Agnes (Cornwall), in clay beds,
and in the cavities of fossils (Crimea). It has
FIG. 67. Vivianite.
been discovered in burned-out colliery workings
(Cransac, Aveyron).
It is soluble in HC1 ;
heated in a tube it gives off water,
bleaches, and becomes exfoliated. Before the blowpipe it melts
readily, and imparts a greenish-blue colour to the flame. The

powder is bluish-white; hardness, 1*5 to 2; sp.gr., 2'5 to 2*7 ;
crystalline form, the clinorhombic prism.

B, TRIPHYLLINE is a phosphate of manganese, iron, and
lithium, RLiPO 4 ;
R = Fe, Mn, with Mg, Ca, Na, etc. It is
occasionally met with as large crystals, more often as cleavable
masses, greenish grey or blackish in colour it crystallises in ;
orthorhombic prisms.
Nordenskiold has given the name tetraphylline to a mineral
he discovered at Keild in Finland, and which possesses the same
form and external characteristics as triphylline.
C. TRIPLITE. This phosphate occurs in blackish brown
imperfect lamellar masses, and cleaves in three apparently
rectangular directions. It is a fluophosphate of iron and
manganese, PO 4 R(R"F)' R = Mn, ; Fe, with traces ef lime.
The lustre is greasy or resinous, the fracture subconchoidal.
It is fragile, and gradually soluble in acids. The hardness is
4 to 5-5 ; sp. gr., 3-4 to 3-8. It has been found in pegmatite
near Limoges, and at Peilau (Silesia).
D. DUFRENITE (Delvauxine). This is a hydrated ferric
phosphate, P0 4 [Fe 2 , 3(OH)]"' = |[P 2 O 5 2Fe 2 O 3 3H 2 O], and

, ,
forms concretionary or fibrous masses dark green in colour,

changing to yellow and brown when subjected to alteration. It
is soluble in acids the hardness is 3-5 to 4

;
the sp. gr., ;
3-2 to 3-4; the crystals are in the form of orthorhombic prisms.

E. CACOXENE. This is a hydrated phosphate of iron and
alumina, which occurs as ochre-yellow fibrous masses, with a

faint metallic lustre and of ill-defined composition. Hardness,
2-3 to 3-3.
78. Minerals containing Arsenic. A. MISPICKEL (arsenical
pyrites, arsenopyrites). The formula of this ore

is 2FeAsS = FeS 2 + FeAs 2 . It forms elongated
prismatic crystals or fibrous, compact, crystalline
masses of a handsome silver-white colour, some-
times yellow on the surface, and with a bright
metallic lustre.
Mispickel is found principally in crystalline

rocks associated with ores of tin and silver. Nitric F IG . 58.
Mispickel.
acid attacks it and separates sulphur and arsenic
acid. When heated in an open tube it yields a white sublimate
of arsenious acid, whilst in sealed tubes it furnishes at first a red
sublimate of arsenic sulphide and subsequently a black sublimate

of metallic arsenic.
The degree of hardness ranges between 5-5 and 6; the
sp. gr. from 6 to 6*4 ;

the crystalline form is the orthorhombic
prism, mm = 1 1 1
l l
53'; e e = 99 5 2'.
B. IRON ARSENATE (pharmocosiderite) is a hydrated ferric
arsenate containing a little phosphorus and copper : 2As 2 O 5 ,
3 Fe 2 3, I2H 2 0.
This mineral, which is dark green (or occasionally brown) in
colour, is always crystalline. It is also found in lustrous,
translucent, granular masses (Cornwall, St. Leon-

ard near Limoges, Horhausen in Nassau). In
hardness it compares with carbonate of lime, and
the sp. gr. is 2-9 to 3. It is soluble in HC1.
Heated in a tube it turns red and gives off
FIG. 69. water and before the blowpipe, on charcoal,

;
Pharmocosiderite.
arsenical fumes are evolved. The usual form
of the crystals is the cube with tetrahedric hemihedry.
79. Iron Carbonate. A. SIDEROSE (spathic iron) consists

of ferrous carbonate (FeCO 3), containing in admixture variable
quantities of CaCO 3 MgCO 3 MnCO 3
, , ,
etc.
It sometimes occurs in darkish crystals, but more commonly

as lamellar, granulated,' amorphous, or renal masses.
The lamellar variety has received the name of spathic iron,
and the amorphous kind is known as lithoid carbonate of iron.
FIGS. 70 and 71. Spathic iron.
Siderosewhite in colour, inclining to pale yellow, but

is
when altered assumes various shades yellow, brown, or ochre

red. Occasionally it is black (lithoid carbonate in colliery work-
ings), and may be transparent, translucent, or opaque, the lustre

being vitreous or tarnished, and the powder grey. It is met
with in beds or veins in the older rocks, and forms a valuable
FIGS. 72, 73, and 74. Spathic iron.
iron ore. The lithoid variety is met with as continuous beds,
or regularly deposited renal masses, in the coal measures ;

and the
oolitic variety occurs in the sandstones and clays of the Secondary
or Tertiary formation.
is soluble in acids, with effervescence, gradual in the
Siderose
cold, very brisk when heat is applied. Before the blowpipe it

blackens and runs together to form a magnetic mass. The
hardness is 3'5 to 4/5 and the sp. gr., which fluctuates between
;
37 and 3-9, decreases to as low as 3 in the earthy varieties.

The primitive and most frequent crystalline form is an obtuse
rhombohedron, ppio ^, 1
with three easy cleavages parallel to

the faces of the rhombohedron, which faces are often curved.
The obtuse rhombohedron b, formed by tangential modifications
"
on the edges, and termed equiaxial," is as plentiful as the
primitive form.
80. Silicates of Iron constitute an extremely numerous
series in nature, principally, however, in combination with other
silicates.
A. FAYALITE. This mineral, obtained on the island of
Fayal, an anhydrous iron silicate, SiO 4 Fe 2 =2FeO, SiO 2

is , ,
and occurs in masses composed of dark green crystalline grains,

exhibiting a reddish, or occasionally black, tinge. These crystals
belong to the orthorhombic type; their hardness is 6' 5, and the
sp. gr. 4.
Fayalite gelatinises in presence of acids, and melts before the

blowpipe to form a black magnetic bead. It is formed artificially
during the smelting of iron ores in blast furnaces, and also during
the refining of crude copper.
B. CHLOROPHCEITE
is a hydrated ferrous silicate containing
a magnesia, and forming small, fibrous or compact, trans-

little
lucent or opaque, pistachio-green or black masses, and is also

found as crystalline needles. It has been met with in a green
amygdaloid rock among the basalts of the Isle of Rum, and in

Fife. The hardness varies between 1*5 and 2, and the sp. gr.
from I '8 to 2.
C. KNEBELITE. A ferro -
manganous silicate (MnFeSiO 4),
forming crystalline or amorphous masses, grey, reddish, brown,
or green in colour, in Ilmenau granite and the iron deposits of
Danemora (Sweden). Hardness, 6' 5 ; sp. gr., 3-7 to 4't.

D. HlSlNGERlTE an iron hydrosilicate of variable composi-
is
tion, containing ferrous and ferric oxides, and forming compact

masses (hardness, 3 sp. gr., 3*04) at Riddarhyttan (Sweden),
;
Bodenmais (Bavaria), etc.
E. NONTRONITE. A hydrated ferric silicate forming a straw-

yellow, canary-yellow, greenish, or sometimes rose-red mineral,
unctuous, tender enough to be scratched by the finger-nail, and
readily soluble in HC1. It is found in renal masses at Saint-
Pardoux in the Dordogne district, Andreasberg in the Hartz

Mountains, etc.
8 1. Multiple Silicates of Iron. A. ANHYDROUS SILICATES.

I. Peridot. This is an orthosilicate of magnesium (Mg 2 SiO 4 ),
wherein a portion of the magnesium is
replaced by iron in the
state of ferrous oxide. The colour is a more or less brownish
bottle-green ;
the fracture, conchoid and lustrous. It is trans-
FIGS. 75 and 76. Peridot.
parent or translucent. The crystals have received the name of
chrysolite, whilst the granular variety is known as olivine,

Peridot is infusible before the blowpipe, unless the proportion
of iron is high ;
it is soluble in acids.
Hardness, 6 to 7 ; sp.gr., 3'! to 3-5; crystalline form, the

orthorhombic prism. The simplest crystals are those from
Vesuvius and Puy, which exhibit none of the faces of the
primitive form.
II. Augite. Under this title are grouped the aluminous or
other pyroxines of calcium and magnesium, in which the pro-
FIGS. 77, 78, and 79. Augite.
portion of ferrous oxide exceeds 5 per cent., without, however,

exceeding that of the magnesia.
FIGS. 80, 81, 82, and 83. Augite.
Augite, properly so called, is the pyroxine of lavas and

basalts (Vesuvius, Auvergne). It is derived from an oblique
rhomboid prism. The secondary forms of these crystals are
prisms with six of the faces flattened in consequence of the
enlargement of the modification k
l
The ends are generally .
formed of the sloping faces e'e', which are well developed, any
other facets forming part therewith being very small and without
influence on the general contour of the extremity. The crystals
are often macleated parallel to A1 .
Augite is deep black in colour, with a sp. gr. = 3-3 to 3-4;

hardness, 6.
9
1
3o THEORETICAL STUDY OF ALUMINIUM, IRON,
III. Hedenbergite. This is another variety of pyroxine,

characterised by the substitution of iron oxide for magnesia.
The formula is (Ca, Fe) SiO 3 but ,
traces of magnesia are rarely
absent. The hardness is 5-5, and the sp. gr. 3' 5.
It is found in laminated masses with chalk, cupreous pyrites,
quartz, and mica, near Tunaberg (Sweden).

IV. Hypersthene. This mineral, which has often been classed
with pyroxine, resembles the latter in composition and its angles
of cleavage. The fracture is lamellar ;
the colour black or bronze-
red. It is hard enough to scratch glass, and has a sp. gr. = 3*4.
V. Almandin Garnet. This substance belongs to the garnet
group, and is still known as the Syrian or Oriental garnet or
carbuncle. The formula is Fe 3 Al 2 Si 3 O 12 It is . the most abundant
FIGS. 84, 85, and 86. Almandin garnet.
of the group, is of a fine red colour, and is employed in jewellery.
Acids attack it with difficulty, and before the blowpipe it fuses to

a black translucent, magnetic glass. The sp. gr. varies between
3*7 and 4*3, and the degree of hardness from 7 to 7*5.
It crystallises in the cubic system, the most frequent forms
being the rhomboid dodecahedron and the trapezohedron ;
crystals bearing the facets of both forms are also met with,
whilst other forms, principally exhibiting the faces of the cube,
are more rare.
VI. Epidote. The epidotes constitute an important family,

whose members are differentiated by the proportion of the bases
entering into their composition. They consist of an orthosilicate
of alumina and lime, wherein part of the alumina is replaced
by ferric oxide and part of the lime by ferrous oxide and

magnesia.
AND COMPOUNDS OF THESE METALS
The ferruginous epidotes seem to approximate to the mean

formula
iSCaO (4Fe 2 3, 8A1 2 O 3 ) 2;SiO 2 .
They crystallise in the clinorhombic system.

VII. Ilvaite (lievrite, yenite, calcareo-siliceous iron). Ilvaite
occurs as crystals, bacillary masses, or amorphous masses of a deep

black colour. The fracture is resinous and somewhat bright.
FIGS. 87, 88, and 89. Ilvaite.
The sp. gr. is 3-8 to 4, and the degree of hardness between

that of glass (which it
scratches) and felspar (by which it is
scratched). It is faintly magnetic, fuses readily to an opaque
glass before the blowpipe, and is soluble in HC1. In composi-
tion it is a silicate of iron and lime, with a little manganese and
water.
The following oxygen ratio was deduced by Rammelsberg
from personal analytical results :
(RO + R 2 O 3 ) SiO :
2
: H O=92
: 8 :
075.
The mineral is found in crystalline schists, with amphibole,
quartz, etc., at Rio le Marina (Elba) and Kangerdluarsuk (Green-

land).
The crystals of ilvaite are derived from the orthorhombic
prism, and generally terminate in a wedge, the principal facet of
which is a z (Figs. 87, 89). In nearly all the crystals the facets
b make their appearance in proximity to 2 and in some cases ,
predominate, the crystals then terminating in quadrilateral pyra-

mids (Fig. 88).
VIII. Achmite is a silicate of iron and sodium, containing a
little Mn, titanic acid, and lime, and forming elongated, opaque,
blackish-brown crystals, met with in Rundemyr granite (Norway),
and exhibiting a vitreous lustre. It is slightly acted upon by
acids, and fuses readily before the blowpipe to a black magnetic
globule. The hardness is 6, and the sp. gr. 3^2 to 3'6.

The crystals of achmite are derived from an oblique rhom-
boid prism, the angles of which resemble those of pyroxine.
FIGS. 90, 91, and 92. Achmite.
The prisms are octahedral, considerably flattened owing to the

1
enlargement of the face A and are mostly terminated by pointed
,
extremities with four faces resulting from the modification e B with ,
which is occasionally associated el (Figs. 90 to 92). Basal
crystals are also encountered, and frequently the crystals are

macleated parallel to h l .
IX. Arfvedsonite. A ferro-sodium silicate remarkable for its
high percentage content of iron. The crystals are imperfect, and

probably isomorphous with those of amphibole.
X. Wichtine. A silicate of alumina and ferrous oxide, form-
ing black masses with an imperfectly conchoidal fracture, and
found in the district of Wichtis (Finland).
B. HYDRATED I.SILICATES.
StUpnomelane. This is a
hydrated silicate of iron with

per cent, of alumina, a little mag-
5
nesia, lime and potash, found at Obergrund near Zuckmantel, in

Silesia. It is attacked with difficulty by acids gives off water ;
when heated in a tube has a sp. gr. = 3 to 3^4, and a degree of

;
hardness =3 to 4.
II. Cronstedtite, A hydrated magnesia, and
silicate of iron,
manganese, occurring as reniform masses of divergent bacillar

needles, of a handsome black colour, vitreous lustre, and opaque.
Found at Przibram (Bohemia), and formerly looked upon as a
variety of tourmaline.
This body is readily acted upon by HNO 3, nitrous fumes
being evolved. The solution finally gelatinises. The degree of

hardness is 2-5 ;
the sp. gr., 2-35 ;
and the powdered substance is
dark green in colour.
The crystals are regular hexagonal prisms, or radial crystals

forming orbicular kidneys, the constituent needles being triangular
pyramids belonging to the tips of a sharp-pointed rhombohedron.
III. Glauconite (chlorite) consists of a ferrous hydrosilicate
containing potash, lime, etc., but is of exceedingly variable
composition.
PART II
MANUFACTURE OF ALUMINIUM SULPHATE AND

SULPHATES OF IRON
CHAPTER III
MANUFACTURE OF ALUMINIUM SULPHATE AND THE ALUMS
I. MANUFACTURE OF ALUMINIUM SULPHATE
82. General Remarks.At a not very remote date aluminium

sulphate was regarded as merely a laboratory product, and
still
it was only about the year 1845 when Pommier of Paris

commenced to prepare it on a proper manufacturing scale that
this substance began to be used industrially. Difficulties were
encountered at the outset, consumers hesitating to give up the

alum to which they were accustomed, and which they could rely
on obtaining pure, in favour of the amorphous, pasty, deli-
quescent, acid, and often impure product forming the aluminium
sulphate manufactured at that date. This distrust was, moreover,
heightened in consequence of certain mishaps (due to excessive

acidity) that attended the employment of the new product as a
mordant and in the sizing of paper but as soon as a method of
;
producing it in a neutral condition and free from iron was

devised, aluminium sulphate was promptly adopted and sub-
stituted for alum in numerous branches of industry.
The reason is not far to seek. The various applications of

alum are based on its content of alumina, which is barely 10 to
io 6 per
-
cent., whereas aluminium sulphate contains from 14

134
ALUMINIUM SULPHATE AND SULPHATES OF IRON 135
to 1 6 per cent. Given equality of price, it is therefore more

economical to employ the latter, which, besides being more
soluble, is more convenient in use.
The raw employed in the manufacture of

material at first
aluminium sulphate was kaolin, together with other aluminous

clays, but these have now been almost entirely abandoned. The
utilisation of clays for this purpose is due to Curandeau, who
founded works at Javel near Paris, about 100 years ago, and to
Chaptal, who introduced it almost contemporaneously at Mont-
pellier, though the object of these savants was not to prepare
aluminium sulphate for direct use, but to convert it into alum
by brevetage (Girardin, Chimie elementaire, p. 411).
Large quantities of impure aluminium sulphate are obtainable
by treating pyritic shales and lignites, but except perhaps in
Belgium this method of manufacture has now almost entirely
disappeared. Other aluminous substances, notably aluminium
phosphate, have also served in the preparation of this product,
but at present scarcely any other raw materials are used but
aluniteand bauxite, from which some 12,000 to 14,000 tons of
aluminium sulphate are now annually produced in France.
The French industry is not a very profitable one, owing to
foreign competition, chiefly by the Germans, who, possessing
better appointed factories and cheaper sulphuric acid and labour,
are able to supply a purer article at lower rates.
Although the production of aluminium sulphate from kaolin

and other clays is now a matter of little more than historical
interest, it cannot be passed over altogether, and a brief de-
scription of these older processes will be given in the following
pages, followed by a more detailed exposition of the treatment

actually applied to alunite and bauxite for the same purpose.
83. Production of Aluminium Sulphate from Kaolin, or
Clay, The principal deposits of kaolin
and Sulphuric Acid.
are met with
Cornwall, and (in France) at St. Yrieix near
in
Limoges, in the departments of Allier, Puy-de-D6me, Brittany,

etc. The composition of the different kaolins having been
already given (Chap. I.

3), need not be gone into again now.
"
According to Pommier (Encyclopedic ckimique, vol. v.),
in
136 MANUFACTURE OF ALUMINIUM SULPHATE
preparing aluminium sulphate, a commencement is made by

reducing kaolin to the finest possible state of division by milling
and sifting, after which it is calcined for 2 to 3 hours in vaulted
reverberatory furnaces, each holding from 4 to 6 cwts. (200 to

300 kilos.) of material. The object of this calcination is to
peroxidise the iron present in the kaolin, and thus reduce its
susceptibility to the action of acid whilst, on the other hand,
;
the alumina rendered more open to attack if the calcination

is is
not carried on at a too elevated temperature. Dull red heat is
the most suitable. The calcined kaolin is taken out of the

furnace by the aid of an iron vessel and turned, just as it is, into
a cylindrical leaden pan holding 1200 to 1500 litres (265 to
330 galls.) and heated by a perforated steam coil. The charge

consists of 200 kilos. (440 Ibs.) of kaolin and 300 kilos. (660 Ibs.)
of 5 3 Be. sulphuric acid, the latter being run in on the hot kaolin.
"
The reaction commences immediately, and, to prevent the
mass becoming too thick, water is added, the steam tap being
at the same time turned on more fully. Care is taken to keep
the mixture well stirred with a wooden paddle throughout the
duration of the reaction, in order to ensure that no portion of the
kaolin escapes attack. When the reaction is at an end the mass
is left for 2 or 3 days to enable the liberated and precipitated
silica to subside. The clear liquid, which constitutes a 20 to 25
Be. solution of aluminium sulphate, is then syphoned off into
a hemispherical leaden vessel heated by a steam coil, also of lead.

In this vessel it is concentrated to a convenient degree, depending
on the quality desired, and is then poured out into a crystallising
pan or table of lead with turned-up edges.

"
In cooling down the mass thickens rapidly, and is then
divided into cakes of different sizes, by means of a wide-toothed,
wooden rake, and left until quite cold, whereupon the cakes are
separated and packed. This completes the process.
"
To ensure that all the alumina contained in the kaolin is
properly acted upon it is necessary to employ a larger quantity

of acid than is theoretically requisite, the result of which is the
presence in the finished product of a little free acid, which,

however, is no drawback for certain purposes. Nevertheless,
AND SULPHATES OF IRON 137
when a neutral sulphate is desired, the excess of acid can be

neutralised during the stage of concentration by adding pure
aluminium hydroxide prepared from cryolite. It is, however,
important that an excess of alumina should be avoided, other-

wise a basic sulphate will be formed, which, being naturally of a
yellow colour, will tinge the entire mass and reduce its com-
mercial value."
The various kinds of clay would be treated in the same
manner. The process now possesses scarcely more than a
historical interest, and need not be further dilated upon. It seems,
however, that the Societe-Industrielle de Landenau (Finistere)
still manufactures aluminium sulphate from kaolin. The author

is unaware of the details of the process employed by this firm,
but it is probably similar to that pursued with alunite or bauxite,

namely, the progressive exhaustion of the mineral by successive
attacks in the manner described later on.
84. Alum Cake.

This product is merely a crude aluminium
sulphate charged with silica, which is utilised in the manufacture

of common qualities of paper. It is chiefly manufactured in
England by treating kaolin or other clays. A variety of alum

cake has also been prepared from bauxite.
The kaolin or clay, previously ground, is introduced in a
hot condition from the calcining oven into a cast-iron pan. Hot
5 3 Be. sulphuric acid is poured over the mass in the proportion
of 150 parts (by weight) per cent., the reaction, which proceeds
vigorously, being soon completed. The mixture is kept con-

tinuously stirred with iron stirrers, and the paste is cast in
moulds or is divided into cakes before it has set hard. Thus

prepared, the product contains the whole of the silica present
in the raw material, which silica becomes incorporated with the
pulp in paper-making and increases the weight.

85. Manufacture of Aluminium Sulphate from Shale, Clay,
and Sulphurous Acid. Sulphurous acid reacts with some energy
on argillaceous substances, and produces aluminium sulphate
therefrom. This reaction is evidently based on the conversion of
the sulphurous acid into sulphuric acid when brought into contact
with atmospheric oxygen. Ferric oxide, when present, also con-
siderably facilitates this transformation in virtue of its oxidising

action.
The production of aluminium sulphate by means of sul-
phurous acid has long been carried on in certain localities, metal-

lurgists who treat blende or galena having at hand a ready
use for the sulphurous acid liberated during the roasting of

these ores.
As an example may be cited the Ampsine works in Belgium,
where De Laminne causes sulphurous acid to circulate through
a series of channels practised in the interior of heaps of spent
clay shales from the manufacture of alum. These spent shales

contain-
Silica 63 per cent. Magnesia
6 per cent.
Alumina . . . . 18 ,, Potash, etc /
Iron oxide . . .
13 ,,
They are obtained by treating ampelite, an aluminiferous rock

first discovered at Amay, and subsequently detected over an area
of 2 to 3 miles in length between Flemalle and Autheit, vid
Flone and Ampsine. Here the rock forms the oldest bed of the
coal measures, and is 20 to 45 feet in thickness, dipping towards
the south at an angle of 70.
The average composition is
Silica 60 'O per cent. !
Pyrites 7
-
o per cent.
Alumina ... . .
17-0 , , Lime and Magnesia .
5 x> , ,
Potash 2-5 ,, Carbonate of iron .

4'o ,,
j
Carbon 4-5 .,
This mineral was treated in numerous factories, I 8 of which

were 808, and dealt, on a average, with 12,000
in full activity in I
cubic metres (15,700 cubic yards) per annum. The rock was
roasted in the open air, then carefully lixiviated, and the residue
discarded. In the process followed by De Laminne, these resi-
dues, when brought into contact with sulphurous acid, absorb it
entirely. When the mass is sufficiently converted into aluminium

sulphate it is lixiviated, the liquor being then concentrated and
cast in cakes in the usual manner. The product is impure, con-
taining an excess of sulphuric acid and ferric sulphate (about
3 to 6 per cent.), and in this condition is restricted to a very
limited sphere of utility.
De Laminne has, however, succeeded in purifying it

by heat-
ing spent shale on the bed of a reverberatory furnace, and incor-
porating itwith the solution of crude sulphate so as to obtain a
thick pulp. The reaction set up is expressed by the equation
(S0 4) 3 2 A1 2 (HO) 6 + (S0 4 ) 3 Fe2 = 2 [(SO 4 ) 3 A1 2 ] + Fe 2 (HO) 6
A1 + .
After a certain period of repose the mass is extracted with

water and the solution concentrated.
86. Production of Aluminium Sulphate from Argillaceous
and Pyritic Lignites. This process, which
had its day, is now almost entirely obsolete,
there being only one factory in France
and that of small importance where it is
still in use.
The object of this industry was not so

much to provide a commercial aluminium
as to furnish alum makers with a product suitable as a raw
material for their purposes. This very impure article was known
as magmas.
The argillaceous lignites, a more detailed account of which
will be given later, were mixed and piled up
in prismatic heaps
on a level open space, whereupon the contained pyrites began to

oxidise. The heaps were then ignited and left to burn, the
oxidation of the pyrites proceeding vigorously under the influence
of atmospheric oxygen, and furnishing sulphurous acid which
attacked the clay. The iron sulphate formed was itself decom-
posed by the high temperature prevailing, and yielded sulphurous
acid and sulphur trioxide, which combined with the clay and left
a residue of ferric oxide. Finally, a red mass known as red ash
was obtained, comparatively rich in aluminium sulphate, and con-
taining but a small quantity of iron (ferric) sulphate.
This mass was lixiviated in wooden or dressed stone vats
provided with false bottoms, covered with brushwood to serve as
a filtering medium.
The filtered liquor was concentrated to 42 to 44 Be. in large
brickwork chambers, and then poured into crystallising pans,
where it solidified to a pasty mass rich in aluminium sulphate.
The concentrating chambers were about 50 to 65 feet long,
and 40 to 60 inches wide, and the depth of the liquor varied

between 20 to 30 inches. The hearth was separated from the
chamber by a sloping bridge about 60 inches long, intended to
prevent the conveyance of ash into the chamber and to keep the
liquor from direct contact with the flame (see Figs. 93 to 95).
The aluminium sulphate obtained by this process exhibited
the following average composition :
Anhydrous aluminium sulphate 36'oo |

Calcium sulphate .... O'2O
Ferric sulphate 5'oo Water and undetermined
Ferrous 0-40 matters .
58-40
Frequently it contained a notable quantity of alum, due to
FlGS. 94 and 95. Reverberatory evaporator for liquor to be converted

into magmas.
the presence of a certain quantity of potash in the lignite, and

the absorption, during evaporation, of the ammonia present in the
furnace gases.
87. Manufacture of Aluminium Sulphate from Pure

Alumina, derived from Cryolite or Bauxite. Cryolite is a
double fluoride of aluminium and sodium. It may be employed
for the production of soda, with which object it is treated with
quicklime or calcium carbonate, either by the wet or dry process,

the result of which is the formation of sodium aluminate and
calcium fluoride. The mass is then extracted with water, which
dissolves out the aluminate and leaves the fluoride behind. On
treating the solution with a current of carbon dioxide, pure
alumina is precipitated, whilst sodium carbonate is left in solution.
This alumina, which forms a waste product, can be advantage-
ously utilised for the production of aluminium sulphate, an
industry that is principally centred in Northern Germany. The

alumina obtained from the treatment of cryolite is almost chemi-
cally pure, being entirely free from silica, iron, and all impurities,
except a certain and by no means unimportant quantity of

sodium carbonate.
To
prepare aluminium sulphate from this material a leaden
pan charged with 53 Be. sulphuric acid, which is then heated
is
by steam to a temperature of 80 to 90 C. The alumina is

added gradually until the acid is saturated, by which means a
concentrated solution of pure aluminium sulphate containing
a little sodium sulphate is obtained this liquor is drawn off ;
and cast into moulds after concentration. The resulting alu-

minium sulphate is very fine, and gives no blue coloration with
potassium ferrocyanide.
An analogous product has been prepared from bauxite, the
pure alumina being obtained from the intermediate stage of
sodium aluminate. A large quantity of aluminium sulphate is
manufactured France by this method at the Salyndres works.

in
The bauxite, reduced to a fine powder, is mixed with sodium

carbonate and placed in a reverberatory furnace, where it is
strongly heated and well stirred until the whole of the sodium
carbonate has been attacked, the operation taking about 5 hours.
The aluminate is then lixiviated by successive extractions, first
with weak liquor from a previous batch, and finally with pure
water. The liquors are kept separate, the stronger solution being
stored, whilst the weaker final runnings are used over again.
The operation is performed in a cylindrical vessel of sheet-
iron with a perforated false bottom of the same metal covered by

a cloth (see Fig. 96), the top of the filtering vessel being closed
by a tight-fitting metal cover. To work the apparatus, a charge

of about \ ton of aluminate is placed on the filter, the cover is
fastened down, and steam under pressure is blown into a closed
tank (F, Fig. 96), containing the weak liquor from a previous
operation and communicating with the upper division of the

filtering vessel by a pipe dipping nearly to the bottom of the

tank, thus forcing the weak liquor up into the former vessel.
Steam is injected to heat the contents of the filter quickly, and
the strong solution collecting below the false bottom is drawn off'
through a tap. When the density of the extract falls below

"
4 Be*, the liquor is set aside as weak," and pure water is intro-
FIG. 96. Lixiviation of crude aluminate.
A, Filtering vessel ; B, filtering surface ; G, steam inlet pipe F, weak liquor tank ;
;
E, pipe delivering weak liquor to filtering vessel ; C, steam pipe for heating
filter D, outlet pipe
; H, feed-water pipe.
;
duced through a separate feed pipe. The average strength of

the strong liquors is about I 2 Be".
These liquors are run into a boiler (Fig. 97) forming part of
the precipitation plant, where they are treated with a strong
current of carbon dioxide produced either by the combustion of
coke, decomposition of chalk by heat, or by the action of HC1

on the last-named substance. Each boiler holds about 1200
litres(265 galls.) of solution, and is fitted with an agitator for
keeping the contents continually in motion. Whilst the opera-
tion is in progress steam is admitted, to raise the temperature of

the liquid to 70 C. The introduction of the CO 2
is arranged so
that the current enters the vessel containing the most exhausted
liquor first, methodical precipitation being thereby ensured.

The resulting precipitated alumina and the dissolved sodium
carbonate are collected in a reservoir underneath each vessel.
The solution is then decanted, and concentrated for the recovery
of the employed, minus
salt
waste, whilst the alumina is

drained in a hydro-extractor ;
and, after being clarified by the

aid of pure water, is treated with
sulphuric acid in the manner

already described, pure alumi-
nium sulphate being obtained.
The method is, however, an ex-
pensive one.
Cheaper processes have been
devised for obtaining alumina
from aluminates, and among

them the interesting method
originated by Baeyer should not
be overlooked. This method
is based on the discovery that
when a solution of sodium FIG. 97. Carbonating the aluminate
solution.
aluminate is agitated with a
A, Pan B, agitator ; G, steam pipe ; C,
;
small quantity of freshly preci-
feed pipe for aluminate solution ; E,
pitated aluminium hydroxide blow-off; D, CO 2 pipe ; F, effluent ; H,

reservoir.
such as formed by the action
is
of carbon dioxide on aluminate solution in the cold the pre-
cipitate of alumina goes on increasing, and at the end of a

certain time only a small proportion of alumina (i molecule
per 6 mols. of soda) is left in solution.
This reaction may be observed when a solution of aluminate is
agitated out of contact with carbon dioxide ;

and it must be borne
in mind during the lixiviation of calcined bauxite with soda, since
the residue may easily retain alumina precipitated in this manner.

The following are the result of sundry experiments made by

the author :
A clear solution containing 63-49 grms. of alumina and 66-96

grms. of soda (Na 2 O) per litre was treated with a little aluminium
hydroxide and shaken up cold in a corked flask ; precipitation
ensued, the liquid gradually becoming poorer in alumina in the
following proportion :
After 48 hours the solution contained 35-78 grms. of A1 2 O 3 per litre,
,, 62 29-44
,, no ,, ,, 2i'8o ,,
134 15-50
but no decrease followed when the agitation was further pro-
longed.
With a solution (4000 litres) containing 61*95 grms. of
A1 2 O 3 and 70*68 grms. of Na 2 O per litre the same treatment
gave the following results :
At the end of 12 hours, 49-42 grms. of A1 2 O3 per litre,
24 3978
36 33 '97
48 ,, 29-00
,, 72 ,, 23-68 ,,
84 17-80
This curious reaction, which occurs solely in the case of

alumina precipitated from the aluminate, is difficult of expla-
nation.
The industrial application of the process is a matter of great
interest on the one hand, it dispenses with the employment of
:
carbon dioxide, and, on the other, the alumina is free from silica
and phosphoric acid, neither of which is thrown down ;
further-
more, the reaction occurs in the cold and requires no apparatus

beyond an agitator and, finally, the liquids used furnish much
;
better results in the treatment of bauxite than are obtainable

from the sodium carbonate usually employed.
Moreover, it is convenient to dispense with this carbonate andj
to repair the waste of alkali by an addition of caustic soda. By
this means it becomes possible to work with quantities absolutely
in accordance with theoretical calculations, and the yield of!
alumina is considerably increased (Diet, de Wurtz, 2 Suppl.

p. 185).
The Baeyer process is in use at the Larne Harbour Alu-

minium Factory, where it is employed in the preparation of pure
alumina for conversion into aluminium.
The raw material is Antrim bauxite, containing
Alumina 56 per cent. Titanic acid ... 3 per cent.
Ferric oxide ... 3 ,, Water . . 26
Silica . 12
The ground mineral is calcined in a roasting furnace of the

Oxland and Hocking type, and consisting of an iron pipe 33 feet
long by 3^ feet in diameter, coated with firebrick and mounted

on trunnions so as to be capable of receiving a rotary motion.
The pipe is mounted on the slope, and heated by a fire placed at
the lower end, the hot gases traversing the pipe and escaping
into a smokestack at the farther end. The mineral is fed con-
tinuously in the top, and, by the assistance of the rotary

at
movement of the furnace, is discharged in a roasted condition

at the other end, on to a platform provided with an aperture just
large enough to allow the passage of the lumps. Thence it falls
into a second pipe 30 feet long by 2 feet 6 inches wide, placed

beneath and sloping in the opposite direction, where it is cooled
down in a current of air blown in by a fan. The roasted mineral
isnext ground fine enough to pass through a sieve with 30
meshes to the linear inch.
Thus prepared, the bauxite is exposed to the action of caustic
soda solution tanks provided with holes for introducing and
in
removing the charge, and also with safety valves and inlet and
outlet pipes for steam and water respectively.
The soda solution has the sp. gr. 1-45, and is put into the
tanks before the bauxite, which then added slowly, the mass
is
being kept stirred. Steam is next turned on, and a pressure of

70 to 80 Ibs. per square inch is maintained for 2 to 3 hours,
after which the tanks are emptied into reservoirs at a higher
level, where the solution is diluted to 1*23. A passage through
the filter-press separates a red residue, for which no application
has as yet been found. The washings of this residue are united
with the main solution, which is then clarified by passing it
through wood shavings.

The precipitation of the alumina is effected, as already de-

scribed in the Baeyer process, by agitating the solution in presence
of a certain quantity of freshly prepared alumina. For this
purpose the requisite quantity of aluminium hydroxide is intro-

duced into a circular decomposing tank, the aluminate solution
being then run in and the whole kept in constant agitation. At
the end of 36 hours, 70 per cent, of the alumina will have come
down, whereupon the agitation is suspended, the weak liquor
FIG. 98. Grinding mill.
drawn off and stored, and the alumina is passed through the
filter press, washed and dried.
The residual liquor, which has a density of i'2, is concentrated

in triple-action concentrators to 1*45, and is then used over again
for attacking the mineral (Moniteur Scientifique, 1897, p. 596).
88. Treatment of Bauxite. A. GENERAL REMARKS.
Bauxite and alunite form the most important minerals at pre-
sent employed for the production of aluminium sulphate. The
methods briefly described above are now no longer employed,
except perhaps the one wherein the alumina is precipitated from

aluminates and furnishes a product entirely free from iron, and
the one in which shale is attacked
by sulphurous acid.
Although simple, the treatment of bauxite is a somewhat
delicate operation, and never furnishes products of the same
degree of purity as those yielded by alunite.

In connection with this subject the author is indebted to
M. Lacarriere, chemical
manufacturer, Noyon, for a mass of
information on the treatment of bauxite, and for opportunities of
examining the method pursued in his works.

The mineral used in France comes from the south, and costs
i 8 to 20 francs (145. 6d. to i6s.) per ton on trucks at the mines.
The composition of the aluminium minerals having been already
described, all that need now be said is that the sellers guarantee
a minimum content of 60 per cent, of A1 2 O 3 and a maximum ,
percentage per cent of Fe 2 O 3 the average composition

of 3 ,
supplied, to keep within these limits, being

Alumina .
62*5 to 65 'oo per cent. Matters insoluble inH 2 SO 4 , 10*50 per cent.
Ferric oxide . . . 2 '90 ,, Loss at red heat . . .
19-00 ,,
Calcium carbonate .
5'io ,,
The bauxite is delivered in lumps about the size of the fist,
and has to be broken down and then ground.

B. PREPARATION OF THE MINERAL. The material is
pulverised by a series of very hard millstones (Fig. 98). The

upper stone A is rigidly mounted in a wooden frame fixed in
strong masonry, and is pierced in the
B
centre by a cylindro-conical aperture, the
smaller diameter of which measures 8
inches, to allow of the passage of the

driving shaft C, and of the material to
be treated.
The movable millstone B is carried
by the shaft C, on which it is rigidly FIG. 99. Face of the

mounted at a, and which runs on a millstones.
socket bearing D. The distance between the two stones is
adjusted by the special arrangement figured in the sketch.

The stones are dressed with grooves, as shown in Fig. 99.
The material to be ground is thrown on to the stationary

millstone and falls through the feed aperture E, whence it makes
its way between the stones and discharged at the periphery
is
in the state of more or less finely divided grit, which in turn has
to be subjected to the operation of grinding, properly so-called.
FIG. 100. Mill for grinding and sifting bauxite.
The apparatus is comparatively economical, a mill of the

following dimensions
Diameter of upper stone 48 inches.
,, lower ,, 40 ,,
shaft 2|
,, square shank A . . .
3i i
Thickness of stones . 8
being able to crush 15 to 20 tons of mineral per 12 hours
shift, at an expenditure of 3 to 4 h.p. In the case of bauxite,

the chief inconvenience arises from the rapid wear of the stones
on account of the hardness of this material.
As a rule, however, the bauxite

is not subjected to any
preliminary crushing, but ground at one operation in special
is
mills. At the Noyon works the ingenious though uneconomical

apparatus shown in Fig. 100 is used.
This consists of a small circular bed-plate A, of cast-iron or
hard stone, on which rotates a cast-iron or hard stone runner B,
which may also consist of a brickwork centre with an outer ring
FIG. 101. Collector.
or tyre of metal. The runner is set in motion by a central shaft

C revolving in a socket bearing D.
Behind the runner is a collector E (shown separately in
Fig. 101), which is turned by a train of cogwheels and collects
the crushed mineral, which it then delivers through a hopper G

on to a truncated conical screen F, shaken automatically by a
cam on the shaft C. The unsifted portions are returned to the
bed-plate by a scraper attached to the shaft C whilst the fine;
powder discharged into a hollow below the mill.

is The entire
apparatus is enclosed in a sheet-iron case, to prevent incon-
venience to the workmen from the dust. This mill will grind
about 4 cwt. per hour, fine enough to pass through a No. 60
I5O MANUFACTURE OF ALUMINIUM SULPHATE
sieve, at a cost of about 55. to 6s. 6d. per ton, which is rather
expensive.
It is necessary to reduce the material to a very fine powder,
otherwise the subsequent chemical reaction goes on very slowly and
imperfectly. The ground powder is ready for immediate treatment,

roasting being unnecessary, because bauxite is in itself a readily
attackable aluminium hydroxide, and the little iron present is
already in the state of ferric oxide and sparingly soluble in acid.

C. CHEMICAL TREATMENT. The process, though simple,
requires attention and constant supervision to ensure economy
of manufacture, the loss of alumina in the residues, the
degree of neutrality of the finished sulphate, and the con-

sumption of fuel all depending on the care with which the
chemical treatment is carried on.
The operation is effected in wooden vats lined with sheet-
lead about \ inch thick, and heated internally by injecting steam
through perforated- leaden pipes (V, Fig. 102) running along the
bottom of the vat, which is covered with planking to protect the
lead lining from the perforating effect of the high-pressure jets
of steam.
Three outlets, closed by plugs, are situated at different levels in
the side of the vat, for drawing off the liquor, etc., the first being
about 27 inches from the bottom, the second about 12 inches

lower, and the third on a level with the bottom itself (Figs. 102, 103).
The vats have the following dimensions :
width, about
lO'S feet; length, about 137 feet; depth, 5-^ feet; cubical
capacity, 780 to Sio cubic feet. The weight of the leaden
lining is about 2i tons, and the total cost ^72 to 80 per

vat. Of course these dimensions need not be rigidly adhered
to, and are merely quoted to give an approximate idea of the

installation. Two vats of the above size will be sufficient for
a works producing 1200 tons of aluminium sulphate per annum.
With such an installation a staff of four workmen is required,
three of whom are employed for stirring the boiling mass
with wooden paddles. The chemical reaction progresses very
favourably; nevertheless, as it
partly depends on the way in
which the stirrers perform their task, and as the stirring, however
AND SULPHATES OF IRON
carefully they may work, is always defective, owing to the

difficulty of keeping the mineral matter in suspension and pre-
venting its accumulation in corners, it follows that the production
of a neutral solution is difficult and the extraction is imperfect,
thus causing a loss of acid and alumina. Attempts have therefore
been made to design more suitable apparatus, one of which, in
use at the Noyon chemical works, is shown in Fig. 104.
E V ,
FIGS. 102 and 103. Rectangular vat, in plan and longitudinal section.
The principal feature of this plant is a cylindro-conical tank

of thin sheet-lead lagged with wood, the cylindrical part measur-
ing ii| feet across and 8| feet high, whilst the truncated cone,
which is 46 inches in smaller diameter and of equal depth, forms
the bottom of the apparatus (see Fig. 104).
The base is lined with pumice a matter of some importance,
because the jet of steam is generally situated there, and the un-
protected lead would very soon get worn through. There are
four outlets for drawing off the contents of the vat; the top one
being about 40 inches below the upper rim, the second 84 inches,
the third 8 feet from the top, and the fourth at the very bottom.
Steam admitted through a vertical lead pipe A, which is
is
suspended by a pulley a, whilst a second pipe B, supported by
another pulley b, is mounted beside the first one and extends
FIG. 104. Cylindro-conical vat, with automatic air-blast agitator,
nearly to the bottom of the vat. This second pipe is connected

with a Koerting injector, and serves to blow air through the
contents of the vat and maintain constant agitation so as to
keep the mineral matter in suspension during the whole of the

chemical process.
The pulleys a and b are mounted on a fork, which in turn
is supported by a chain passing over two pulleys c and d, and

terminating in a counterpoise C. The system is thus kept in
equilibrium, and the vertical adjustment of the pipes in the vat

becomes an easy task. A vat of the above description costs
about ^240.
The mineral is fed in by means of the elevator shown by
dotted lines at the one side of the figure.
This system of installation has numerous advantages. The
constant agitation by the air blast, and the cylindro-conical shape
of the vessel, combine to prevent the accumulation of deposited
mineral, and a more intimate contact between the ingredients is

produced. The reaction goes on more rapidly, a condition of
neutrality is more quickly reached ; and, with a smaller quantity
of sulphuric acid, the conversion of the materials is more complete
and the residue more effectually extracted. Furthermore, a by

no means inappreciable saving of labour is effected, since, in place
of the four men needed for working the rectangular vats, one
man. will suffice.
Whichever system be employed, the progress of the reaction

is the same.
Thus, for example, if we now take into consideration the
rectangular vats, leaving the cylindrical system until the alunite

process is discussed, a calculated quantity of an acid solution of
aluminium sulphate from a previous treatment is put into one
of the vats. The solution has a density of 35 to 40 Be., and
contains 250 to 300 grms. of SO 3 per litre. The charge measures
about 350 cubic feet, which corresponds to 2^3 tons of sul-
phuric acid, calculated as SO 3 .
Heat is applied by injecting steam, and as soon as the liquor

is hot the corresponding weight (e.g. 3 to 3| tons) of the
powdered mineral is added, the whole being mixed by the aid
of wooden rakes, the heating and agitation continuing for 7 to
8 hours on end. The mass, which will then be (or should be)
nearly or quite neutral, is next diluted and left at rest to clarify,

the unattacked mineral depositing on the bottom of the vat. On
the following day the liquor is decanted and transferred to leaden
cisterns, wherein it deposits the final traces of matter in suspension

before passing to the concentrators. This liquor has a density of
about 32 Be., and constitutes a neutral, or nearly neutral, slightly
ferruginous solution of aluminium sulphate. The residue is
lightly washed with fresh water, which is then run into the
cisterns, the residue "being afterwards treated with a highly acid
liquor at 45 Be". With this it is heated, stirred up, left to sub-
side,and separated by decantation. The final attack is made

with 60 Be. sulphuric acid assisted by heat, and, towards the end,
by an addition of acid liquor from a preceding batch.

After subsidence and decantation, the residue, now practically
exhausted but still impregnated with liquor rich in sulphuric acid,
is first washed in the extraction vat with weak (5 to ioBe.)

liquor. This being decanted, the muddy residue is run off into
cisterns and exhausted with water.
All the grades of liquor except those from the first treat-
ment, which are concentrated direct are used over again, either
for attacking the mineral or in washing.
The chief difficulty in this process is the decantation. In the

case of bauxite the liquors do not clarify readily, and in general,
to obtain satisfactory deposition, it is necessary not to employ too
large a proportion of mineral. On the other hand, an excessive
deviation in the contrary direction, so as to produce very weak
liquors, leads to an excessive consumption of fuel for the evaporat-
ing pans. Thus it is evident that there is a medium course, which

will have to be decided by practical experienceeach particular in
case. The proportions already given are averages from satisfac-

tory workings, but will necessarily vary according to the class of
mineral treated. As far as possible the liquor should clarify
sufficientlybetween night and morning, a condition not always
realised when bauxite is used. Filter-presses have been resorted
to for the purpose of accelerating the work, facilitating washing
and diminishing the amount lost in the residues, but without
success, the pores of the filtering medium being speedily clogged
by the small quantity of clay and finely divided silica in the
sediment. The amount of residue obtained varies according to
the manner in which the work is performed, and generally fluctu-
ates between 20 and 25 per cent, of the raw material taken. It
consists mainly of silica, a little clay, about 8 to 10 per cent,

of alumina, and a little ferric oxide. The quantity of alumina
lost in the residue in normal working is therefore about 2 per

cent, of the mineral employed a fairly low proportion.
According to the quality of aluminium sulphate produced, and

the more or less satisfactory performance of washing, the treat-
FIG. 105. Concentrating the liquor.
ment of a ton of bauxite entails a consumption of 45 to 50 cwt.

of 60 Be. sulphuric acid, the yieldbeing about 4 tons of
aluminium sulphate.
D. CONCENTRATING THE LIQUOR. The final stages of the
work present no special difficulties. The liquid, which has a
density of 33 to 34 Be., from the treatment of the fresh mineral,
FIG. 1 06. Cutting rake.
is drawn off and evaporated in leaden vats heated by steam

(Fig. 105).
Those employed at Noyon measure 12*8 feet x 4*25 feet x
f
40 inches, and are heated by a leaden coil i^ inches in diameter J /3o

(T inch metal), forming 10 rings of 32*8 feet each, thus giving a
heating surface of about 1 1 8 square feet. These figures are, of 1 1 4-
course, not invariable but, to ensure satisfactory working, the

;
/ *2r- O
heating surface should be at least & square feet per^ cubic foot of f
vat capacity.
When sufficiently concentrated, the liquor is drawn off
through a syphon on to leaden tables in front of the concentrat-
ing pans, the edges of the tables being turned up slightly all
round to prevent the liquor from running over. Here it is left
to cool and as soon as a certain consistency has been attained
;
the mass is divided, by means of a cutting rake with 3 or 4 teeth

(Fig. 1
06), into cakes about 8 or 9 inches square, which are then
stored. The extent to which the concentration of the liquor
is carried depends on the quality of product in view. For
FIG. 107. Pulveriser. Cross section.
common grades of low percentage the final strength of liquor is]
46 Be., whilst for the ordinary quality of cakes, lumps, etc.,

known as second whites, it is concentrated to 48 50 Be., and:
poured out to a depth of 4 to 5 inches on the crystallising trays.
This product contains 12 to 13 per cent, of alumina. When
concentrated to 52 Be. the liquor furnishes a sulphate containing
14 per cent, of alumina. For the purest kinds to be subsequently;
powdered, the concentration is carried to 56-58 Be., and the

depth of liquor on the crystallising trays is not more than about.
2 inches : in this case the product contains about 1 6 per cent, of
alumina.
E. TREATMENT OF THE FINISHED ALUMINIUM SULPHATE.

The ordinary kinds are usually reduced to coarse powder in a
107 and 108) consisting of a vertical disc A
pulveriser (Figs.
mounted on and provided with 6 oblique slits a, in
a shaft C,
which are bolted the rasp blades c (Fig. 109). This disc is set
in a wooden case containing at one side an aperture B coinciding
with the one end of a trough D, into which the blocks of sulphate
to be pulverised are placed by hand and pushed in succession
FIG. 109. Blade

FIG. 108. Pulveriser for aluminium sulphate. Front view. of pulveriser.
against the teeth of the disc, which runs at high speed. This
apparatus works well, but takes a considerable amount of motive
power.
The grades
destined to be converted into fine powder are put
through a special mill. The trip-hammer mill, invented by

L. Loiseau (maker, F. Weidknecht of Paris), has been seen at
work by the author, and gives very good results and the new ;
pattern (Weidknecht and Schoeller system) now described is

also highly satisfactory. These mills contain an arrangement
of articulated hammers or beaters, oscillating upon axes and
striking in their flight the material fed through the hopper

(Fig. no).
The object kept in view by the inventor is the imitation of
hand labour ; for, just as the stonebreaker employed on the
roads is armed with a flexible-handled hammer, so this machine
is provided with flexible hammers intended to produce the
identical effect attainable by hand. These movable hammers,
working at a certain speed, strike the material introduced
through the hopper and break it into pieces of various sizes.

These pieces are projected, by the shock, against t)ie massive
head-piece of the machine, and, as they meet in their upward
flight other fragments that are by this time descending, further
breakage ensues without additional consumption of energy, this

being the result of the projection. The materials then fall on to
the hammers again and are caused to travel over steel grids
which act as screens, the current of air set up by the motion of
the hammers assisting the sifting action of the screens, which
allow all the finer particles to pass away. The hammers then
act as scrapers, removing all the insufficiently triturated material,
arid the process continues until the task is completed.
This operation also enables an intimate mixture to be obtained

of products of different density.
Being loosely mounted, the hammers simply oscillate on their

axes, and give way if the resistance to be overcome is excessive :
thus danger of breakage is prevented, the more so since there

all
is no contact between the hammers and any other part of the

soachine. This method of action furnishes, among other advan-
tages, that of ability to reduce certain products to an infini-
tesimally fine powder when required or inversely ,

a valuable
consideration sometimes.
The hammers being loose, but little motive power is required
in comparison with the capacity of the mill, the hammers acting
like fly-wheels. Any desired degree of fineness of division can
be procured, since the material cannot escape from the mill except
through the screens, which can be provided of various gauges.

Bauxite has also been converted into a kind of alum cake by
the following method :
Forty parts of powdered bauxite are mixed with 50 parts of

50 Be. sulphuric acid and 10 of water. The mixture is heated
gently, either in a reverberatory furnace or in lead-lined sheet-iron
vats, and the aluminium sulphate sludge thus obtained is run into
moulds where it sets very hard on cooling. This product has been
utilised in the manufacture of paper of low quality.
89. Purifying Aluminium Sulphate. The chief impurity
to be eliminated is iron, the presence of which is highly objection-
able in many instances. Its removal is an operation of great
delicacy by reason of the similarity between the properties of the
two metals, and has formed the subject of a number of inventions.
A. PRELIMINARY REMOVAL OF THE IRON IN THE
MINERAL BY THE AID OF DILUTE ACIDS. Attempts have
aeen made to remove theoxide present in bauxite, by
ferric
treating the powdered mineral with dilute acids, and principally

oxalic acid, which readily dissolves this oxide. The result is,
icwever, imperfect, even when the oxide has been previously

reduced by heating in the presence of reducing gases.
B. TREATMENT OF THE SULPHATE LIQUOR WITH ZINC.
This process does not eliminate the iron, but simply transforms
nto ferrous sulphate the ferric sulphate present in the solution,
tkjs, moreover, attended with the disadvantage of introducing
zinc sulphate into the product.

C. SEPARATING THE ALUMINIUM IN THE FORM OF IN-
SOLUBLE BASIC SULPHATE. This method, proposed by Auge

& Co., is based on the fact that if a suitable base, such as potash,
soda, magnesia, alumina ;

or a salt, such as the carbonates of the
above alkalis or magnesia, sodium aluminate, etc, whether hot or
cold be carefully added to a solution of aluminium sulphate con-
;
taining iron sulphate, reduced by any means to the lowest stage
of oxidation, the alumina will be sooner or later precipitated in the

form of basic sulphates containing a large proportion of the sul-
phuric acid, whilst all the extraneous salts will remain in solution.
It is then sufficient to wash the precipitate and add sulphuric acid,
to obtain an aluminium sulphate of a high degree of purity.
According to the author's experience of this method, it seems

to be a highly delicate one and not very practicable.
D. ELIMINATION OF IRON BY POTASSIUM FERROCYANIDE.
The ferrous liquors are diluted to about 20 Be., and placed in
wooden vats holding about 220 gallons, in which the iron is then
thrown down as Prussian blue by means of potassium ferro-
cyanide (yellow prussiate) added as a hot solution until the
precipitate ceases to increase a condition recognised by testing

small samples of the filtered liquor from time to time. If the
end point has been exceeded, the surplus ferrocyanide is thrown

down by a further quantity of the sulphate liquor.
After leaving the liquor at rest for about a fortnight, the clear
portion is drawn off and evaporated. The Prussian blue pre-
cipitate is washed with water, filtered, pressed between felt, and

sold. The quality is, however, inferior, and the blue is only fit
for colouring common grades of paper. By treating the pre-
cipitate with sodium carbonate, it

may be also converted into
sodium ferrocyanide for use over again.
This process, although enabling the whole of the iron to be
removed, and furnishing a very fine product in a simple and at
first sight very economical manner, is really very expensive and
not to be recommended, at least in some countries, since all
depends on the rate of wages, the price of fuel and acid, and
other considerations.
In fact, to enable the blue to settle down, it is
necessary to
AND SULPHATES OF IRON l6l
greatly dilute the liquor, and consequently a large additional

consumption of fuel is requisite for the evaporation process.
Furthermore, the extremely slow rate at which the blue is
deposited greatly retards the manufacturing process, unless the

precipitation plant has been specially installed on a large scale
for this process, it being necessary to leave the (20 Be.) liquor for
at least a fortnight after the addition of ferrocyanide, in order to
give the precipitate time to subside.

The method has been carried on in England, coals and sul-
phuric acid being cheap ;

but would be unsuitable in France under
the conditions prevailing there.
E. NEWLAND'S PROCESS. Newland obtained a very pure
product, containing only 0^082 per cent, of iron, by treating in a
filter-press the evaporation products of solutions of crude alu-
minium sulphate. The iron remains in the mother liquors, and

the products of the second operation are treated over again.
F. THE CHADWYK AND KYNASTON PROCESS. In this
process, which is worked England, the liquor obtained by

in
attacking bauxite is treated with arsenious acid to throw down

the iron. The operation is completed by an addition of calcium
ferrocyanide and zinc sulphate.
G. FAHLBERG'S PROCESS is based on the total precipitation
of iron as a plumbate, when a ferrous solution of aluminium sul-
phate is treated with lead dioxide.
According to Pommier, the method of working is as follows:

"
The lead dioxide for this purpose is readily obtained
by the
reaction of 75 parts of 36 Be. nitric acid on 100 parts of red lead
(miniuni) in the cold. The resulting dioxide is of a brown colour,
not black, the latter kind being a denser modification of the
oxide and unsuitable for the purpose in view. Should the
temperature of the operation be too high, this black oxide

will be produced. The excess of nitric acid, together with the
lead nitrate formed during the reaction, is removed by washing
with water, and subsequent decantation. The work is carried on
in clay vats.
" and
Another method easily applicable on the large scale,
preferably used by the inventors, consists in treating lead chlorite

1 62 MANUFACTURE OF ALUMINIUM SULPHATE
with a solution of bleaching powder. The lead chlorite is

pre-
pared, in the first place, by mixing 2 parts of litharge and I
part
of common salt in a mill, and grinding them in a little water or
brine until the pasty mass has turned perfectly white. This mass,
which consists of an alkaline basic lead chlorite, is transferred to
an iron vat along with a concentrated solution of bleaching
powder, and boiling is continued until the whole is of a brown
colour, whereupon a slight excess of the bleaching powder is
added. Finally, the mass is purified by a series of washings and

decantations. It should be noted that the lead dioxide must be
used moist state, and not dry, and for this reason it is
in a
employed in the pasty condition in which it is found after the

washing process.
"
The lead dioxide having been prepared by one of the
methods just described, the next stage is performed in the same
way as the ferrocyanide treatment. A predetermined quantity of
the pasty dioxide is added to the cold solution of aluminium
sulphate to be purified, whereupon the iron comes down as an
insoluble, reddish - brown iron plumbate. Half an hour is
sufficient for the complete separation of the iron. The proportion

of dioxide required is naturally dependent on the quantity of
iron present in the liquor, and determined precisely by a series
is
of tentative experiments. The ratio between the two is 20 parts

of lead dioxide for each part of ferric oxide.
"
It is necessary for the ferruginous solution to be in a basic
or neutral condition, otherwise a portion of the lead dioxide
would be attacked by the free sulphuric acid. The supernatant
liquid may be separated from the precipitate by decantation after
several days' rest, or at once by the aid of the filter-press.
"
The purified solution is concentrated and cast in the usual
manner. The iron plumbate is collected and treated for the re-
covery of lead dioxide, with which object it is mixed with sulphuric

acid or nitric acid in a leaden vessel, to dissolve out the iron and
leave lead dioxide behind. After syphoning away the solution of
iron sulphate or nitrate, the traces of acid are removed by washing \
with water. Any unconverted lead dioxide which might have

been present with the iron plumbate is recovered intact in this I
operation. The recovered lead dioxide may be used over and

over again indefinitely, it being sufficient to make good the
amount lost by washing.
"
The cost of this process, which is employed in the works
of Harrison Brothers & Co., Philadelphia, is 5s. per ton of alu-
minium sulphate containing o -
5 per cent, of iron."

Manganese dioxide behaves in a similar manner to lead
dioxide and stannic acid has also been recommended by Spence
;
Glaser for the same purpose. A long time back, Persoz recom-
mended the precipitation of ferric oxide by gelatinous aluminium
hydroxide.
2. ALUM MANUFACTURE
" "
90. Introduction. The name alum is generally applied in
commerce to a double sulphate of aluminium with a base, such as
potash, soda, ammonia, etc.
In ancient times the efflorescence of certain rocks supplied

the Greeks, Romans, and Egyptians with a product known by
the name of alumen, largely employed in medicine, dyeing,
tanning, etc. According to Dioscorides and Pliny, several species

of this product were known, some of them perfectly white, others
more or less coloured, and all possessing a styptic flavour. They
were all more or
complex mixtures of aluminium sulphate
less
and iron sulphate, and the term alumen (from which the word
alum is derived) had in those days a much wider significance
than now.
Under the name of " glacial alumen," Geber described a sub-
stance which was obtained from Rocca in Mesopotamia (the
modern Edesse, near Smyrna), and which was really an alum in
the restricted sense of the term. Various other authors sub-
sequently described bodies analogous to the alums, notably

"
Paracelsus, who made use of the distinctive name Rocca
"
alumen," which has been corrupted into the French term alun
"
de roche (rock alum).
The oldest method of preparing alum consisted in treating
alunite or alum stone. This industry, which was of Oriental
origin, was introduced into Europe about the thirteenth century,

and the first important alum factory was established on the

island of Ischia, towards the fifteenth century, by a Genoese
merchant named Perdrix, who had travelled extensively in the
East. The example was soon copied by Jean de Castro, another
Genoese, who, struck by the resemblances existing between the
rocks at Rocca and those at La Tolfa near Civita Vecchia, pro-
spected for alunite, which he was not slow to discover. He then
set up at La Tolfa an alum works, which afterwards attained
great celebrity.
Finally, Antonio de Piena shortly afterwards founded a similar
factory at Volterra, in the Grand Duchy of Tuscany.
In the seventeenth century a commencement was made with
the manufacture of alum from alum earth in Hesse, Thuringia, and
Saxony ;
but it was not introduced into England until the
eighteenth century, during which period T. Chaloner set up the

first alum works in Yorkshire.
Subsequently the method of preparing alum from aluminous

and pyritic shales and lignites was elaborated in Germany and
Picardy ;
whilst the process based on the direct union of alkali
sulphates with aluminium sulphate obtained by treating clay,
bauxite, cryolite, etc., is of comparatively recent origin.

The manufacture of alum has considerably declined in im-
portance since the introduction of aluminium sulphate into com-

merce. Nevertheless, some 10,000 to 12,000 tons are still
produced annually in France, the greater portion being obtained
from alunite and pyritic lignites. This last - named method
furnishes ammonium alum, and employs as a crystallising reagent
sulphate of ammonia, which has been procurable at a very cheap
rate for some years past.
Sodium alum, which until very recently was looked upon as
merely a laboratory product, is at present manufactured in small
quantities at several aluminium sulphate obtained

works,' from
from bauxite. The two processes most in use are those of
Aug^ and Kessler, descriptions of which are given below from the
patent specifications of the inventors.

We will now proceed to describe the various methods that
have been in use or are still employed for the preparation of
alum, laying most stress on the treatment of alunite and pyritic

lignites.
91. Manufacture of Alum from Clay, Kaolin, Bauxite,

etc., Sodium Alum. A. ORDINARY ALUM. The first stage
of the process is invariably the preparation of a liquor rich in
aluminium sulphate. This is effected by methods already de-
and therefore need not be repeated.
scribed,
The liquor is heated up again and mixed with the requisite
quantity of potassium sulphate, potassium chloride, or ammonium
sulphate; and as soon as the added salt is dissolved the
hot liquor is run into the crystallising pans, where the alum
crystallises out. To convert this alum into a merchantable form
it must be re-crystallised.
The mother liquors obtained in this process are very trouble-
some, and their concentration is a very important operation, since
it ensures the recovery of the excess of sulphuric acid from the

initial stage, as well as a somewhat considerable quantity of alum.
With this object the mother liquors and washings are run into
lead-lined wooden vats, and concentrated by steam heat to
40 Be., the resulting hot being mixed with a suitable

lye
quantity of sulphuric acid and used over again for attacking
the alum mineral employed. By proceeding in this manner
none of the mother liquor is wasted, which is an important
consideration. On the other hand, when a ferruginous mineral
is employed, the iron continues to accumulate in the mother
liquor to such an extent as to eventually render the latter unfit
for use.
J. Wiernick (Zeitschrift filr angeivandte Chemie, May 15,
1894; Moniteur Scientifique, 1895, p. 221), however, has shown

that the mother liquor can be freed from iron in a very simple
manner by effecting the concentration under special conditions.
In fact he states that if the concentrationbe continued to
50 Be. instead of 40 Be., a deposit of an iron salt, the com-
position of which varies according to the conditions of the
operation, is formed in the concentrators. This precipitate

separates very quickly, leaving a clear liquor almost entirely free
from iron and fit for use over again.
The following analyses show the progressive diminution in the
iron content as the concentration of the liquor increases :
Fe per
.... Be'. litre.
Mother liquor at 30 contains 1 6 '80 grnis.

,, evaporated to . .
42 ,, I3'2O ,,
45 "'56
. 47 8-80
,, ., 49 8-04 ,,
The composition of the precipitate requires to be carefully

watched, as it varies according to the state of oxidation of the
iron in the liquor. With liquors that have been fully oxidised,
the precipitate is yellowish white, crystalline, and insoluble in
water ;
and
readily forms incrustations on the steam coil in the
it
concentrating vessel, thus preventing the transmission of heat.

Furthermore, it causes a loss of alumina and potash, or ammonia,
the yellow insoluble mass formed containing the sulphates of
these bodies in addition to iron sulphate.
When washed, dried, and analysed, this precipitate has been
found to contain
(i.) (ii.)
Fe2 O3 23-88 23-02

S03 53-90 58-77
A1 2 O3 7'25 7-50
NH 3 2-36 2-40
KO 2 7-06 6-92
and therefore consists of a basic salt corresponding nearly to the

formula
2Fe 2 3, 5S0 3 ,
A1 2 (S0 4 ) 8> K SO (NH SO
2 4) 4) 2 4,
the exact equivalent of which is represented by the composition
Fe2
S0 3
3 . . . .
23-37 NH
K2 O
3 ....
.... 2-48
A1 2 3 ....
. . . .
58-48
7-52
6-86
being desirable to prevent as far as possible the formation

It
of this compound, it is necessary to reduce the ferric salts to the

ferrous state, and for this purpose Wiernick finds shavings of
green poplar wood form a very
suitable reducing agent.
If, after
shavings have been placed in the
these vat, the
concentration of the liquor be continued to about 50 Be., the
greater part of the iron is deposited as an amorphous black mass

67
consisting exclusively of iron salts, as shown by the following

analytical data :
(i.) (ii.)
FeO 16-98 17-20
Fe2O3 25-76 28-48
S03 57-68 57-22
which figures agree very closely with the formula

3 Fe3 4, 2Fe2 (S0 4 ) 3 .
The foregoing method of purification is said to have yielded
very satisfactory results.
B. SODIUM ALUM. I. Introductory Remarks. In the same

manner as aluminium sulphate forms alums with the sulphates of
potassium and ammonium, it also furnishes with sodium sulphate

a product known sodium alum, Na 2 SO 4 A1 2 (SO 4) 3 24H 2 O, a
as , ,
body differing, however, from the others by its ready solubility in

water (
i i o parts per cent.).
From the industrial point of view, the chief importance of this
property is the difficulty that thereby arises in the separation of

sodium alum from other salts in solution, notably iron sulphate ;
and it is this consideration that has prevented the extension of

the sodium alum industry, notwithstanding the relatively very
low price of sodium sulphate in comparison with the correspond-
ing potassium and ammonium salts.
For the manufacture of sodium alum a comparatively pure

raw material, such as bauxite, is absolutely essential and hence ;
the whole process be regarded as the reverse of sensible,

may
from an industrial point of view, since the direct conversion of
bauxite into aluminium sulphate gives a product richer in alumina
than is the final product aimed at (sodium alum), and one
sufficiently pure for most purposes.

Nevertheless, in certain cases, and by working under well
defined conditions, the crystallisation of sodium alum may be
managed so that the mother liquor removes a portion of the
impurities, a product of sufficient purity for certain delicate

applications being thus obtained. In this case the manufacture
of sodium alum becomes a matter of interest, in view of the
cheapness of the crystallising reagent.

Even when working with pure materials the manufacture of

sodium alum is a very delicate operation, the affinity of sodium
sulphate for aluminium sulphate being comparatively feeble and

their union toform alum accomplished with difficulty in fact,
only complete under certain well defined conditions. Thus by

cooling down to a low temperature (in winter) a mixture of
equivalent proportions of aluminium sulphate and sodium sulphate,
in solution, the author has obtained a mixture of sodium alum
with a larger or smaller quantity of sodium sulphate, instead of
the crystallised alum alone.
Moreover, even highly concentrated solutions of sodium alum

have a great tendency to become supersaturated, and crystallise
with great difficulty. A highly concentrated solution when quite
cold will become turbid immediately, and deposit crystals on
decantation or agitation. These phenomena of supersaturation
become more and more accentuated as the degree of impurity of
the solution increases.
The process of solution of sodium alum in water exhibits
certain interesting peculiarities.
Thus, if the alum crystals be heated very briskly in water
they subside into a pasty white mass, which, notwithstanding the

ready solubility of this compound in water, becomes disseminated
throughout the liquid, and forms a very thick milky emulsion.
Even when the proportion of water is large, the solution often
remains opalescent and exhibits nacreous striations.
Here we are evidently in presence of a phenomenon of

dehydration within the bosom of the liquid, a peculiarity observed
in the case of other salts, especially ferrous sulphate, but to a
particularly remarkable degree in the instance now under con-

sideration.
Remarkable peculiarities are also exhibited in the crystallisa-

tion of this alum. In one experiment sodium alum was dissolved
in distilled water, and the solution concentrated to 39 Be.
When cooled the liquid solidified to a white mass, the surface of
which was found next day to be covered with beautiful flattened
triangular crystals representing a modification of the octahedron,
the sides of some of them measuring up to I cm. With a view
to re-dissolving the mass it was then sprinkled with a little water

and stirred with the thermometer, whereupon, to the author's
surprise, crystallisation proceeded rapidly, accompanied by a rise
in temperature, until finally the capsule contained a large number

of well formed transparent crystals of sodium alum, together with
a mother liquor in which nearly all the iron of the solution was
retained.
Curiously enough, these observations, made incidentally by

the author in the course of experiments on the manufacture of
sodium alum, had already was subsequently ascertained
as
been utilised industrially by Auge and Kessler, brief abstracts of

whose patent specifications are given below.
At the present time sodium alum occupies a certain position
in the industrial world, though the output, which a few years
"
back appeared likely to threaten that of the other alums, has

now become stationary. It is chiefly employed in paper-making,
and is besides, in virtue of its great solubility, more convenient in
application than either potassium alum or ammonium alum.
The Auge Process.
II. In this process a solution of sodium
sulphate is mixed with one of aluminium sulphate, and the whole

concentrated to 39 40 Be. The resulting paste is then spread
out on inclined leaden plates, so as to allow the mother liquor
(forming about \ of the total weight) to drain off. The tempera-

ture is maintained at about 10 or 15 C. during the period of
crystallisation. The mother liquor removes almost the whole of

the impurities.
The temperature has an important influence on the percentage
of alumina in the alum ; and, in fact, if the crystallisation be effected
at about zero, only 7 per cent, of alumina is present in the product.
The author has examined the alum furnished by this process.
It is in the form of small, highly efflorescent, exceedingly white
crystals, which assume but a very slight bluish coloration when

tested with ferrocyanide. It is probable, however, that this low
content of iron is due more to the extreme purity of the materials
employed than to the method of preparation.
III. The Kessler Process. Several methods of obtaining
sodium alum have been patented by this inventor.
1
One of them consists in concentrating a solution of the two

sulphates so as to obtain a pasty mass, as in the Auge process.
This paste is then mixed with a sufficient quantity of the water
drained from a previous batch, and a number of crystals are
added to serve as nuclei for the crystallisation which then
ensues. The iron remains in the mother liquor.
Another method is to prepare a concentrated solution of
aluminium sulphate (5 3 Be., measured at boiling temperature),
which is then cooled until just on the point of setting, whereupon
it is mixed with sufficient mother liquor from a previous batch to
form a liquid measuring very little more than 40 Be. (at 40 to
50 adding sodium sulphate equivalent to 40 per cent,

C.) after
by weight of the aluminium sulphate taken.

Finally, a third process consists in adding to mother liquor or
water alternate solutions (more or less concentrated) of the two
sulphates, in the proportion of 40 parts of sodium sulphate per

100 of aluminium sulphate (53 Be. strength at boiling tempera-
ture), so that the liquid finally measures no more than 40 Be. at
45 C., the solution being left to crystallise after each addition.
In his patent specification Kessler describes the various opera-

tions in the following manner :
The solution of sodium alum is

evaporated to 45 Be. strength
and cooled down to 16 or 22 C. It first sets to a pasty mass
which crystallises spontaneously in transparent crystals, the opera-
tion being, however, accelerated if a few crystals are
dropped in.
In the summer time
50 Be. solution of sodium alum
a 40 to
may be poured, even boiling hot, over ready formed crystals of

the same alum impregnated with the mother liquor, and neither
turbidity nor magma will be formed, provided the mixture is

stirred and incorporated quickly. Assistance is afforded in this
respect by the reduction in temperature resulting from the lique-

faction of the crystals. The operation is arrested before the
appearance of a turbidity, which would occur at about 40 or
if the mixture has not been effected with sufficient rapidity.

When the temperature reaches 22 to 23 C. the solution is
poured into vats, where it sets completely.

The procedure may be modified by introducing sodium sul-
phate crystals, reduced to very fine powder, into the aluminium

sulphate solution.
To prepare the alum solution, sodium bisulphate may be used,
the salt being dissolved in 45 or 60 Be. sulphuric acid, and the
resulting solution employed for attacking the aluminous mineral.
Again, the sodium bisulphate may be dissolved in aluminium
sulphate solution, the result being to liberate sulphuric acid, which
may be utilised as a solvent for the calcination products of
the mother liquors from several crystallisations. The sodium
sulphate introduced is recovered by sufficiently diluting the
alum solution and cooling it down to 10 C., whereupon the
excess of sodium sulphate crystallises out, leaving the alum
behind in solution.
A small sample of Kessler's sodium alum, preserved in the
author's laboratory, is in the form of larger and harder crystals
than those from the Auge process ; they are also more trans-
parent and less efflorescent. On the other hand, the colour is
somewhat inferior, having a very pale violet-yellow tinge. In

contact with ferrocyanide they exhibit a strong blue coloration,
and therefore contain a notable proportion of iron.
92.Manufacture of Alum by the Spence Process. This is

a very old method, dating back to 1845, and one that has been
largely employed.
The raw material used is a black clay (shale), forming an
extensive vein, situated directly under the true coal bed in the
Lancashire basin. This clay is combustible on account of its
large content of organic matter.

The raw material is first burned in heaps, from 40 to 80
inches high, which are replenished in proportion as they subside.
The operation of roasting takes about 10 days, and when pro-
perly carried out temperature not exceeding dull red heat
at a
yields a reddish, friable, and porous residue. This residue is

then placed in large open tanks heated from below, and treated
with 34 Be. sulphuric acid, the temperature being maintained at
about I 10 C. Each charge consists of about 20 tons of mineral.
Whilst the formation of aluminium sulphate is in progress, and
the temperature is at the level indicated, a current of ammoniacal
vapour, from a distilling apparatus or from the ammonia water

of gas works, is blown into the tanks, the quantity admitted being
carefully regulated so that a large excess of sulphuric acid is
always present. The liquor in the tanks is thus gradually con-

verted into a concentrated solution of ammonium alum, and, when
sufficiently clarified by repose, is drawn off into crystallising pans,
where the alum is precipitated by rapid cooling and continued

agitation. The alum powder thus obtained is drained and washed
with a saturated aqueous solution of alum.

The product is entirely free from iron, but has to be brought
into a merchantable condition by re-dissolving it with steam and
running the solution into lead-lined wooden moulds, where the

alum which are chipped out with axes.
crystallises in blocks
On the average, about i 5 cwt. of the black clay are needed
to produce I ton of ammonium alum. Spence also subjected
aluminium phosphate to a similar treatment for the preparation of
the same product.

93. Production of Alum from Natural Felspar. At the
present day no interest attaches to the methods proposed foH
utilising these materials : a few words may, nevertheless, be de-
voted to the manner in which attempts have been made to
recover the alumina and potash in felspar for the manufacture of
alum.
Mohr recommended the mixing of I 30 parts of felspar with
70 or 88 parts of potassium carbonate, sufficient water being
added to form a plastic paste. The mass was divided into
briquettes, and, after being calcined moderately, moistened with
water, and treated with 1 96 parts of concentrated sulphuric acid,
furnished a solution of alum and a residue of silica.
Turner proposed to fuse felspar with potassium sulphate, and
incorporate the molten mass with potassium carbonate. The
vitreous mass, when treated with water, parts with its soluble
potassium silicate and leaves a residue which, on being treated
with boiling sulphuric acid, furnishes alum and silica.
Another proposition was to react with sulphuric acid on a
3 of fluorspar, the mass being

mixture of 2 parts of felspar and
kept at red heat until the disengagement of hydrofluoric acid
vapour ceased. The residual mass yielded alum when Extracted

with water.
94. Treatment of Alunite. Joint Production of Alum

and Aluminium Sulphate. Alunite, as a mineral product, has
already been dealt with on an earlier page, so we may now pro-

ceed at once to the methods of treatment to which this body is
exposed.
A. THE LA TOLFA PROCESS. The mineral, broken in lumps
the size of paving setts, is subjected to a very simple method of
treatment, consisting in roasting the lumps in heaps or in kilns.
The operation requires to be very carefully performed,it being
necessary to avoid an excessively high temperature, which would
decompose the aluminium sulphate and liberate sulphur trioxide

and dioxide. When such liberation begins manifested by the
appearance of dense white acid fumes the operation is stopped,

and the roasted mass transferred to brickwork bins, where it is
left to effloresce for 3 or 4 months, with occasional waterings.
At the end of that time the whole will have become in a measure
slaked, and is then lixiviated to extract the alum. The liquor is
concentrated and run into the crystallising pans, where the alum
crystallises out ;
but as the liquor contains in suspension a kind
of rose-red mud, rich in ferric oxide, the alum crystals are tinged
with the same colour.
This alum crystallises in cubes and not in the ordinary octa-
hedral form. It constitutes the Roman alum so highly prized by
consumers on account of its freedom from soluble compounds of
iron.
B. THE POMMIER PROCESS. Messieurs Pommier treated

Madriat alunite for the purpose of obtaining alum and aluminium
sulphate at the same time.
The following is the method employed (Pommier's article
on Aluminium Sulphate and Alum, in Fremy's Encyclopedic) :
"
The alunite is first reduced to a very fine powder in a
mill fitted with heavy cast-iron runners and with a collector
which scrapes the ground mineral on to a shaking sieve. After

this it is calcined in a reverberatory furnace with a flattened
arch, at a temperature not exceeding dull red heat, as otherwise

a portion of the sulphuric acid in the alunite is decomposed.

At the end of about 2 hours the charge is drawn from the
furnace and placed in an iron box, from which it is transferred
to a cast-iron pan about 60 inches in diameter, set in the ground
so that only about I 2 inches project above the surface. Here it
istreated with 35 Be. sulphuric acid, previously heated in a small
leaden boiler, the quantity being regulated so that 525 parts by
weight of acid are used to 400 parts (original weight) of alunite.

A violent reaction ensues and is quickly terminated, the mass
being meanwhile kept stirred with large iron paddles to ensure
uniformity of action throughout.
"
The mass then quickly sets hard and is divided, by
long
iron tools with cutting edges, into manageable pieces which are
loaded on open trucks of sheet-iron. The loaded trucks are run
on rails into a furnace heated to a low temperature by means of
coal or (better) coke, and consisting of a low brickwork chamber

built on the ground and closed by a cast-iron door, the hearth
being at the opposite end. The object of this operation is to
complete the attack by several hours' exposure to moderate heat,
the brief duration of the violent reaction being insufficient to
attain this result. On leaving this furnace the lumps of crude
product are spread out on flat ground covered by shed roofs,

where they are left for several weeks, it having been found that
the reaction still continues and becomes completed thereby, so

that even the hardest lumps are finally disintegrated and con-
verted into dust. Then follows the process of lixiviation in a
cylindrical leadenpan heated by direct steam. When all the

soluble matters have been extracted by the water the mass is
left at rest for about 48 hours; the insoluble portion, largely
consisting of silica, is deposited, and the clear liquid, which is
nothing more than a solution of alum and aluminium sulphate,

is decanted. The density of this solution is between 20 and
25 Be., and is increased to 30 Be. by evaporation in a con-
centrating pan, whereupon the liquor is poured out into a
rectangular leaden vat holding about 4500 gallons, on the walls

and bottom of which the alum crystallises out on cooling. After
the lapse of a week or 10 days the mother liquor (a solution of
aluminium sulphate) is syphoned off, concentrated (generally to

about 50), and run into a crystalliser in the usual manner.
"
As for the alum, that portion which settles on the walls of
the vat consists of small true octahedral crystals, which are readily
separable and form the commercial

'
granulated alum,' which is

ready for sale as soon as it has been drained. On the other
hand, the portion deposited at the bottom (the bulk) is in the
state of a fine crystalline powder, retaining some of the mother
liquor and forming an unsaleable, dirty, wet paste, which has to

be re-crystallised to bring it into a merchantable condition."
C. METHOD NOW IN USE. I.

Preparation of the Mineral.
The process now to be described is the one in most general use
at the present time, those mentioned above being of little more
than historical interest.
The mineral employed in France is derived from the deposits
at La Tolfa in Italy, those in Auvergne being neglected for some
reason unknown to the author.
The average composition of the crude, sifted La Tolfa
alunite, utilised in the manufacture of alum and aluminium
sulphate, is
Alumina 23 '50-29 'oo per cent.

Iron oxide
Sulphuric acid
Potassium sulphate
.... . .
2 'oo
i6'3O-2O'oo
io'oo-14'oo
, ,
,,
,,
Insoluble in HC1 . . .
17*40 ,,
Loss at low red heat . . .

35 '80 ,,
The lump alunite is finely powdered by the aid of mills

similar to those already described in dealing with the treat-
ment of bauxite, and is then roasted in a reverberatory furnace

with a flattened arch (Figs. I 1 1, 112), the mineral being spread
on the bed to a depth of 4 to 6 inches. The temperature
employed is equal to about the fusing point of copper, and the
operation results in a loss of weight, varying in accordance with
the composition of the mineral and the manner of roasting, but
averaging about 33 per cent.
The roasted material has the following mean composition :
Loss at dull red heat .

4-30 per cent. Iron oxide . . .
3'o8 per cent.
Insoluble in H SO
2 4 . 26*20 Sulphur trioxide .
.24-40 ,,
Alumina . . .
34*92 ,, Potash . .
7-50
1
II. Attacking the Mineral. The apparatus used is the same

as in the case of bauxite, and the operation is conducted in a
similar manner, with certain modifications necessitated by the
nature of the material and greatly influencing the purity of the
product.
In crude alunite the iron is present for the most part in
the form of ferrous compounds, and the operation of roasting,

far from raising this iron to a higher stage of oxidation, tends
to minimise the proportion of ferric compounds, chiefly by reason

of the reducing action of the sulphur dioxide formed.
In the chemical treatment the peroxidation of the iron by
means of oxidising agents one of the principal aims in view,
is
the ferric sulphate thus formed being eliminated from the liquor,
FIG. in. Longitudinal section. FIG. 112. Transverse section.
Reverberatory furnace for roasting alunite.
either as an insoluble iron alum or as basic sulphate, by a simple

manipulation during the subsequent treatment. Contrary to
what happens in the case of bauxite, the solutions obtained from
alunite are thereby considerably purified, the results, though
generally imperfect, being none the less of great importance.
In considering the method of conducting this chemical treat-
ment, let us take, for example, the case of the trunco-conical

vessel described in connection with bauxite
The cubical capacity of the truncated cone is 5 '200 cub. m.

,, ,,
Total ....
cylinder ,, 24*500 ,,
29 700 cub. m.
For a vessel of this capacity, about 30 cub. m. (6600 galls.),
the charge of alunite will amount to 8 tons and the acid to
4 tons, calculated as SO 3 . This sulphuric acid is introduced in the

state of acid liquors from previous operations and containing

300 to 350 grms. of SO 3 per litre, the volume of 35 to 40 Be.
liquor being therefore about 2500 gallons. Directly the acid

liquor is run in, the steam and air taps are turned full on, the
charge of roasted alunite is admitted, 2'2 Ibs. of sodium nitrate
per ton of material (17^ to 22 Ibs. altogether) being added at the

same time.
When the reaction is terminated (i.e. the liquor obtained
is
neutral), which generally takes about 2 or 3 hours, a solution
of chloride of lime is introduced into the mass in order to
complete the peroxidation of the iron, the proportion of chloride

of lime required being usually about 3-3 Ibs. per ton of alunite
(i.e. about 26i Ibs.). Water is then immediately added to dilute
the solution to about 30 to 35 Be., the steam is shut off, and
only the kept going, in order to keep the
Korting injector
temperature of the mass as near 80 C. as possible. It is at
this stage that the purification of the liquor goes on, and the
longer the temperature of 80 C. is maintained the better is this
cleansing effected.
This heating process is continued for 20 to 30 hours to
" " "
produce superior aluminium sulphate, while for the " purified
quality it is
necessary to keep the temperature at 80 C. for 120
hours. If this condition of temperature is not accurately main-
tained, the purification will oftentimes be imperfect and the liquor

become acid again. In such event the method is being im-
properly conducted. A general rule for the production of neutral
liquor is to employ a very strong and highly acid liquor for the
reaction, the temperature being then higher at the outset and the
attack proceeding more rapidly and completely. It is also
necessary that a rapid fall in temperature should occur as soon

as the concentration of the liquor increases, the temperature
being reduced to 80 C. as quickly as possible, and never allowed
to rise again. In this event the final liquor should remain neutral.
The liquor will exhibit a density of about 32 Be., and a
degree of acidity varying with the accuracy of performance
attained. It is then left to clarify, which it will do in less time
than is
required for bauxite, and is decanted as soon as possible,
for removal to the crystallising plant. A high temperature should

prevail during decantation, in order that the whole of the alum
present may be retained in solution. The residue is lightly
washed, and, the washings being decanted after dilution to 20 to

25 Be., the remaining mass is treated with acid, an operation
requiring great care in order to produce the best results.
For this purpose about 10 tons of pure 52 Be. sulphuric
acid are run in, and followed, whilst the application of heat is
still proceeding, by a further (gradual) addition of 6 tons of
5 2 Be. acid in the form of acid sulphatic solutions of 40 Be.
density, and containing 300 to 360 grms. of SO 3 per litre, the

total acid being equivalent to I
part of SO 3 (cr6 in the pure state
and o 4 -
as acid
liquor) per About i o to 12
i
part of mineral.
hours are required for this operation, during which time the
application of heat and the injection of air are continued without

interruption, and a variable quantity of acid sulphatic liquor
measuring 40 to 41 Be. density, and containing an average
of 350 grms. of SO 3 per litre is obtained. In the case under
consideration the volume of liquor is 44005000 gallons.
As soon as this liquor has been run off, the residue is washed
with weak (5 to10 Be.) liquor, and removed to leaden tanks
where it is washed with water, the whole of the washing liquors
being employed again in the cycle of operations.
The total length of time occupied by the treatment is about
80 hours in the case of the " superior " quality of product, but
" "
much longer for the purified aluminium sulphate, in conse-
quence prolonged exposure at 80 C. then necessary.

of the
Other considerations, such as the nature of the mineral, the
duration of the attack, the conditions of decantation, etc., also
influence the time taken up by the process.

The progress of the purification is controlled by tests for the
iron, and the precipitation of the can also be checked by

latter
colorimetric tests with ferrocyanide or thiocyanate. For control-

ling the progress of the attack, recourse is had to the Baume
areometer, acidimetric titration of the liquor, and analysis of the
residues.
In working with the rectangular vats described in dealing
with bauxite, the progress of the attack, etc., is the same as
already defined. In any case, endeavours are made to restrict

the consumption of sulphuric acid to 100 parts of 60 Be. acid
per i oo parts of mineral, for the production of inferior grades,
and to 90 parts for neutral alum, though these figures are always
slightly exceeded in practice. About 120 to 130 per cent, of
sulphuric acid represents the average consumption in attacking

the alunite, i.e. a loss of 20 to 25 per cent, of acid, either left in
the residues or carried away as free acid in the inferior grades of

alum. The outlay involved is a variable quantity, and is least
when trunco-conical vats are employed and the residue is properly

exhausted.
The residue, calcined after w ashing, should contain 90 per
r
cent, of matters insoluble in hydrochloric acid, and 1*4 to 1*5

per cent, of alumina and iron oxide. When trunco-conical vats
are used, the residue, merely dried at 100 C. without calcination,
contains 87 to 90 per cent, of insoluble matter, and 3*75 per cent.,
at most, of iron oxide and alumina ;
whereas with rectangular
vats the insoluble matter in the residue amounts to only 75 per
cent., whilst the iron oxide and alumina attain to 7 and even 14
per cent., thus representing a considerable nett loss.
The efficient performance of the work greatly depends on the

men in charge of the operations, since on their carefulness hangs
the neutrality of the products and the proper exhaustion of the

residues. As a general principle the quantity of alumina escaping
attack should be reduced to a minimum, as well as the quantity
of free acid in the liquors destined for the production of neutral
sulphate, the final excess being saturated with pure alumina at

the stage of concentration.
In order to obtain good results in these respects a system of
premiums and fines, given or levied as the work is well or ill done,
is of use in stimulating the men and inducing them to look
properly after their duties.
III. Crystallising and Purifying the Alum. -As we have
seen, the liquors resulting from the acid treatment of the mineral
are delivered to the crystallisers. These vessels differ in various
works. Sometimes they are large brick tanks lined with lead
l8o MANUFACTURE OF ALUMINIUM SULPHATE
and embedded in the ground ;

but this system is very expensive,
and is inconvenient on account of the difficulty in discovering
leakages. The crystallisers used in Lacarriere's works at Noyon

are of a much more efficient type, being made of wood lined with
thin sheet-lead, and slightly raised above the level of the ground,
thus enabling leaks to be at once detected, and increasing the
rate of cooling.
The alum crystallises on the walls of the pans, and, when the
temperature is sufficiently reduced, the mother liquor is drawn off
and sent to be concentrated, whilst the alum itself is broken out
and re-crystallised to bring it into merchantable condition. With
this object the crude alum is placed in a copper or leaden cylinder
into which steam is introduced as required, and produces a con-

centrated solution of alum, of the density 40 to 42 Be. at boil-
ing temperature. After leaving the solution for an hour, to allow

the insoluble matter to settle down, it is syphoned off into leaden
moulds of a cubical capacity of 70 to 90 cubic feet.
The moulds are made of two or three breadths of plank
covered on the inner side with thin sheet-lead, the lateral joints
being packed with sheet-caoutchouc and tightened with nuts and

screws, whilst the joint against the boarded floor is luted all
round with clay. The alum crystallises to a depth of i o to 12
inches all round the interior of the mould. After about a fort-
night the moulds are taken to pieces, the blocks of alum are
broken to allow the mother liquor to drain away, and the lower
part of each block is cut away with axes, being impure and con-
taminated with the clay luting, and requiring purification by a

second re-crystallisation. The remainder is formed into solid
transparent blocks and sold in that condition, or else broken into
lumps about the size of the fist and packed in bags or casks.
These operations will be described later on in dealing with the
treatment of lignites. Sometimes the alum is desired in a
pulverulent form, and in such case the 40 to 42 Be. solution

is poured into ordinary crystallising pans, so as to be cooled at a.
more rapid rate than in leaden moulds, the liquid being kept
stirred all the time. The resulting finely divided flour of alum is
freed from the accompanying mother liquor in a centrifugal

AND SULPHATES OF IRON l8l
separator, like those used in sugar works, but lined with lead, the
alum being discharged in an almost dry, pure condition.
The re-crystallised alum invariably gives a slight blue colour
reaction with ferrocyanide, and, if desired perfectly pure, must be
again crystallised in the same manner as before.
Occasionally a demand arises for alum in the form of coarse

powder. This may be produced by grinding the crystals in mills,
which will form the subject of description later on.

IV. Concentrating Liquors for Aluminium Sulphate, and
Handling the Product. The mother liquors from the alum
crystallisers are concentrated in the manner already described in
dealing with bauxite. always advisable to have the liquor

It is
for concentration of as high a density as possible, since by this
means the loss of alum, by retention in solution, is reduced to a

minimum, and less fuel is required for the concentration process.
The most suitable density for the liquor is 35 Be. in summer and
34' Be. in winter, and this strength should be attained in the
crystallisers.
The different grades of aluminium sulphate and degrees of
concentration required for their production have already been
discussed, and need not be gone into again, except to mention
that for purified sulphate, very rich in alumina and low in iron,
the liquor is concentrated to 6o-62 Be. and poured on to
copper plates. The product from alunite is handled in the same
way as that from bauxite, and it is therefore unnecessary to
describe the various operations again.
It will be apparent that, apart from the mixed production of
alum and aluminium sulphate, the principal differences in the
treatment of alunite and bauxite are, that the one mineral needs
roasting whilst the other does not ; secondly, the liquors from
alunite require treating with oxidising agents, a superfluous
measure in the case of bauxite. The main divergence between
them, however, so far as the final results are concerned, is that in
the one case the purification spontaneously under
is effected
enabling products of a
slightly different conditions of attack, thus
high degree of purity to be obtained, whereas from the other

none but inferior grades can be procured. It may be that this
1 82 MANUFACTURE OF ALUMINIUM SULPHATE, ETC.
is effected by the heat in presence of an excess of

purification
unattacked material, the alumina of which, under the influence
of time, replaces iron in the solution. It would therefore be
interesting to whether an analogous result could be
ascertain
obtained by adding to bauxite an excess of some readily attack-
able aluminous compound.
A ton of alunite furnishes about 14 to 16 cwt. of alum,
sometimes more, and about 2 tons of aluminium sulphate contain-
ing i 5 per cent, of A1 2 O 3 .
The subjoined figures give the composition of several grades

of aluminium sulphate:
Ordinary Neutral Retrograde
concentrated concentrated or
to 46 B6. to 56 B6. superior.
Total SO3 33-27 36-50 37-00
A1 2 O3 1178 14*36 15-10
Fe2O 3 1-42 1-14 0-30
Loss on calcination . . .
60-50 48-10 48*10
Free SO 3 8'6o o-oo o-oo
95. Production of Alum from Pyritic Shales or Lignites.

This operation entailing the conjoint production of alum and
ferrous sulphate, this interesting industry will be dealt with after
the various methods of preparing the last-named salt.
CHAPTER IV
THE MANUFACTURE OF SULPHATES OF IRON
I. FERROUS SULPHATE
96. Introduction. Ferrous sulphate, also named green

vitriol or green copperas, has been known for a very long time,
and is indeed one of the most important salts of iron. Formerly
its uses were restricted, and it did not make any headway until
the discovery of its possibilities in connection with the production

of Nordhausen on a manufacturing scale.
sulphuric acid At
a later date considerable quantities were consumed in the manu-
facture of coal gas, in dyeing, and in disinfecting ;
and though
at present its use in the dyeing industry has fallen away into
insignificance, agriculture, on the other hand, affords a large and

increasing outlet for ferrous sulphate,in consequence of new
discoveries of its utility, e.g., in connection with the treatment of

chlorosis in the vine, the destruction of wild mustard (sinapis
arvense], etc.
Strictly speaking, the manufacture of ferrous sulphate does not

constitute an industry at all. In some cases its production is of
a secondary and occasional nature, being pursued or abandoned
in accordance with the state of the market and the com-
mercial value of the product ;
whilst in certain industries it is
obtained as a bye-product in the manufacture of other substances,

seldom of an allied character. Under the latter circumstances,
ferrous sulphate often forms an inconvenient residue which
the maker is glad to get rid of at any price. Thus in the
-
metallurgy of copper, the pickling of sheet iron, cleaning
white iron, galvano

-
plastic operations, and the treatment
of pyritic shales and lignites, large quantities of this salt are
produced.
Other manufacturers, in order to utilise certain acid or metallic
residues of low value and difficult sale, occasionally go in for

making ferrous sulphate, notwithstanding its low price. Petroleum
refiners, for
example, way utilise in this the acid tar (sludge acid)
obtained in refining and containing up to 50 per cent., by weight,
of SO 3 Similarly, the waste accumulating in the wire-drawing
.
industry is occasionally utilised, on the spot, for making ferrous
sulphate. On
account of the different methods employed in the
preparation, commercial ferrous sulphate may contain highly
divergent impurities, such as copper, zinc, lead, alumina, lime,

magnesia, etc. As this variety cannot fail to possess a certain
amount of interest, the principal methods of producing this salt
will now be described.
97. Preparation from Pyrites. In addition to the minerals

utilised for the manufacture of alum, certain natural sulphides of
iron, such as the different varieties of pyrites, are treated for the
production of ferrous sulphate. This treatment is identical with

that employed for the alum minerals, and which will be described
later on.
Pyrites is piled in large heaps on a flat surface, previously

puddled with clay, where it is subjected to efflorescence and
roasting, i.e. conversion from the state of sulphide into that of a
sulphate, under the influence of moisture and atmospheric oxygen.

The arrangement of this roasting place is such as to facilitate the
collection and storage, in a suitable reservoir, of the liquor result-
ing from the lixiviation of the heaps by running water or water

pumped over them. The liquor collecting in the reservoir is
repeatedly pumped over the heaps, in order to ensure its pro-

gressive enrichment. When a given strength is attained the
liquor is left to settle and clarify, is then concentrated by

evaporation, and drawn off to be crystallised. The salt thus
obtained is invariably aluminous.
Occasionally, in certain localities, pyrites is found which has
oxidised spontaneously, and which may therefore be used direct
for the manufacture of ferrous sulphate without having to pass

through the stages of roasting and efflorescence.
Another mode of dealing with pyrites with a view to the
production of ferrous sulphate is intimately connected with the
manufacture of sulphur. In this case the pyrites is distilled in
clay retorts similar to those used in gas works, but smaller,
holding a charge of not more than 65 Ibs. Under the influence

of heat the pyrites decomposes and liberates sulphur, which is
condensed in chambers. At the end of 6 hours distillation may
be considered complete, and about 19 per cent, of sulphur will
have been obtained, the quantity remaining in the residue being
about double that distilling over. This residue forms a highly
suitable material for the production of ferrous sulphate. It is
thrown into heaps in admixture with the residue from a previous

and oxidation is started by setting fire to a layer of
lixiviation,
wood under the heap, the process then continuing automatically.
After about a year the mass is ready for extraction. This
operation is carried out in large flat basins, where the roasted

mineral is sprinkled with water, the resulting solution, which has
a density of about 20 Be., being drawn off, left to clarify, and
evaporated. When concentrated to about 41 Be. the liquor is
run into crystallising pans.

The residue from this process contains a large proportion of
ferric oxide, basic ferric sulphate, and impurities. Part of it is
used in the manufacture of colcothar, and the remainder is mixed

with the still residue and roasted over again.
98. The Spence Method. This method was designed to

utilisethe residue from roasted pyrites used in the manufacture of
sulphuric acid. It is necessary that the pyrites should be less
highly roasted, and should retain a larger proportion of sulphur

than usual in the sulphuric acid process, the residues from which
are mainly composed of ferric oxide.
To prepare sulphate from a residue of this kind,

ferrous
Spence digested with dilute

it sulphuric acid (about 22 per cent.
Be.), and obtained in about 1 2 hours' time a liquor of about
33 Be., which he concentrated and crystallised. The reaction of
sulphuric acid on the residue was accompanied by a slight dis-

engagement of sulphuretted hydrogen. The undissolved mass

was treated over again with sulphuric acid, and the process
repeated until a residue, very rich in sulphur, was obtained
suitable for use in the manufacture of the sulphur dioxide required
for the work of the leaden chamber.
Other methods have been proposed for utilising pyritic
residues. Negrier, in particular (French Pat. 217,602, Nov. 27,
1891), proposed to heat the residue to 100 C., and pass over
ita current of sulphur dioxide and steam, the reaction being
accompanied by an elevation of temperature up to 250 C.

99. Preparation of Ferrous Sulphate from Native Ores.
This process, which was first employed by Janicot in the prepara-
tion of a ferrous sulphate, utilised in dyeing at Lyons and St.
Etienne, consists in dissolving in 40 Be. sulphuric acid certain

native iron ores, such as spathic iron which for the most part
is composed of ferrous carbonate associated with carbonates of
lime and manganese, together with silica, clay, etc. When the
reaction is finished the mass is left to settle, the liquid is poured
off, and leaves behind a residue of carbonaceous matter, clay,
calcium sulphate, etc.
This process may also be applied to minerals comparatively
rich in chalk, provided they are previously treated with dilute
(4 Be.) hydrochloric acid, which merely dissolves the carbonates

of lime and magnesia without attacking the carbonate of iron.
The residue is then treated with sulphuric acid as already described.
100. Preparation of Ferrous Sulphate from Metallic Iron
and Sulphuric Acid. The ferrous sulphate obtained by this
process exceedingly pure, and meets with a ready sale.
is It
being uneconomical to employ materials of good quality for this

purpose, the residues from various industries are utilised, such as
waste from the tin-box makers, tinned iron cuttings, waste from wire-
drawing, contractors' works, and old iron generally, these forming

a cheap and comparatively economical raw material. The acid
residue from oil refineries, the tar obtained in refining petroleum,
containing about 50 per cent, of sulphuric acid expressed as SO 3 ,
and the waste liquor from sulphuric acid works, are all frequently
used for this purpose.
87
The treatment is carried out in a copper vat, the bottom of

which is supported by cast-iron plates, the vat being heated by
direct fire with flues for the hot gases carried round the sides.
The usual shape is rectangular with rounded corners. The gases
and vapours liberated during the operation are carried off through
a chimney stack. The vat being charged with sulphuric acid,
and diluted if necessary, is heated to boiling, and the scrap-iron
is thrown in, the mass being stirred as frequently as possible.
When the reaction is finished the charge is drawn, left to settle,
and the clear liquor removed for crystallising.
According to W. P. Thompson, the residual tar from petro-

leum refining can be profitably utilised for the production of
ferrous sulphate on the one hand, and, on the other, of a kind of
bitumen suitable for various purposes. The process in question
has been described by Rave. The acid tar, which may amount
to about 25 per cent, by weight of the refined petroleum, is
mixed with sufficient iron turnings to completely neutralise the

acid. The reaction is complete after a certain time, and the
mass is treated with boiling water to separate the tar from the
ferrous sulphate. The tar resembles bitumen in appearance and
properties, and can be thickened by heating in a still.
10 1. The Buisine Method. This method is based on the

same principle as that of Spence, from which it differs, however,
in the mode of application.
In principle the Buisine method consists in treating im-
perfectly roasted pyrites with hot concentrated sulphuric acid.

The object of this imperfect roasting is to bring the disulphide of
iron into a condition less rich in sulphur and more readily
attackable by sulphuric acid.
The disulphide itself is not attacked by this acid except at
a temperature of about 250, and furnishes ferrous sulphate and
sulphur dioxide whereas the lower sulphides are attacked
;
at a
temperature of about 100 to 110, or below that at which sul-
phuric acid reacts upon sulphur to form sulphur dioxide.

The imperfectly roasted pyrites is a mixture of Fe 2 O 3 the ,
sulphides FeS, Fe 2 S 3 Fe 3 S 4 with a

, , unoxidised pyrites, FeS 2
little .
When this mixture is treated with hot concentrated sulphuric

acid, the ferric oxide yields ferric sulphate, and the sulphides
fiynish ferrous sulphate, sulphuretted hydrogen, and sulphur,

according to the following equations :
Fe 2 3+ 3 H S0 = Fe (SO 4 + 3 H O,
2 4 2 )3 2
Fe 2 S 3 + 2 H SO 4 = 2 FeSO 4 + 2 H S + S,
2 2
FeS + H SO = FeSO 4 + H S.
2 4 2
The sulphuretted hydrogen, however, reacts on the ferric sul-

phate, forming sulphur and ferrous sulphate,
Fe2 (SO 4 ) 3 + H 2 S = 2FeSO 4 + S + H SO
2 4 ;
and if there is any excess of sulphuretted hydrogen, this is de-
composed by the hot concentrated acid,

3 H 2
S + H S0 = 48 + 4H
2 4 2 O,
so that finally the products consist entirely of sulphur and ferrous
sulphate.
The whole of the sulphur originally contained in the im-
perfectly roasted pyrites is left in a -free state. If the pyrites

contained at least 10 per cent, of sulphur the quantity of sul-
phuretted hydrogen formed is sufficient to reduce the whole
of the ferric sulphate formed at the same time but when the ;
roasted pyrites contained less than o per cent, of sulphur the I
mixture consists of ferrous sulphate and ferric sulphate, the pro-

portion of the former being in direct ratio to the amount of
sulphur in the pyrites. Consequently it follows that, to obtain
sulphur and ferrous sulphate exclusively, it is preferable to work

with imperfectly roasted pyrites containing at least 10 per cent,
of sulphur.
As regards the pyrites, i.e. the iron disulphide left unoxidised
in the imperfectly roastedmass, does not react upon sulphuric it
acid under the conditions prevailing, and is consequently found

in its entirety in the residue and returned to the furnace. In fact,
the disulphide is not attacked by sulphuric acid below about
250, whilst, as we shall see later, the actual temperature attained
is not over I 80.
The method of working is very simple, and does not require
any special plant beyond that in general use in chemical works.
In the first stage the pyrites is imperfectly roasted in ordinary
furnaces (e.g. those of Maletra), the sulphur dioxide formed being
conveyed to the leaden chamber ;

the crude pyrites, which con-
tains 50 to 52 of sulphur, is thus modified, so that the sulphur
content is between about i o and 3 5 per cent. Next, the roasted
pyrites is agitated with 60 Be. sulphuric acid in about the
following proportions: 100 to 125 parts by weight of sulphuric

acid to each 100 parts of roasted pyrites. The apparatus con-
sists of a cast-iron retort, covered in such a manner as to afford
connection with a washer a coke tower), and
heated by a
(e.g. is
fire underneath. As the temperature approaches 1 00 the reaction

becomes fairly energetic, and the temperature rises to between
i
50 and 1 80, at which point it is maintained for about a quarter
of an hour. During this reaction steam is given off, and carries
away with it a little sulphur, as well as traces of sulphur dioxide

and sulphuretted hydrogen, which are retained by the washer.
The crude product then treated with hot water, the resulting
is
solution depositing crystals of ferrous sulphate when cooled.

The insoluble residue contains, in a free state, almost the
total amount of sulphur present in the roasted pyrites, which
sulphur can be separated either by fusion, distillation, or ex-

traction with carbon disulphide.
In this manner the whole of the iron in the pyrites can be
converted into ferrous sulphate, and about 50
theoretically
per cent, of the original sulphur can be extracted, the remainder
being consumed in the production of the sulphuric acid taking
part in the reaction. The sulphur thus obtained in considerable
proportion, as a residue of the ferrous sulphate process, correspond-

ingly reduces the cost of the product, which is thus brought down
to a minimum.
It will be understood that the imperfect roasting of the
pyrites may, in certain be advantageously replaced by

cases,
distillation in a closed vessel as already indicated, which furnishes
the same result and facilitates the recovery, by condensation, of
that portion of the sulphur which has to be removed from the
pyrites to enable the reaction to take place.
If the pyrites employed be of a cupreous character the method
just described furnishes, as crude product, a mixture of sulphur,
ferrous sulphate, and copper sulphate, the proportion of sulphur
1
being greater or smaller according to the amount present in the

roasted pyrites. This mixture may be used direct for agri-
cultural purposes, particularly for treating certain diseases of the
vine ; and, in fact, is largely so used, either alone or as a con-

stituent of special mixtures. It is also clear that, if necessary,
the sulphur, copper, and ferrous' sulphate could be readily
isolated from the crude product. This is an interesting
application of iron pyrites, the considerable importance of which
in chemical industries is already known.
2. CONJOINT MANUFACTURE OF FERROUS SULPHATE

AND ALUM
A. Treatment of Shales
1 02. Introduction. The pyritic shales employed for the

manufacture of alum consist mainly of clay and quartz, with a
variable proportion of felspar, in a more or less advanced stage of
decomposition ;
in addition to this substance, pyrites, potash, lime,
magnesia, and carbonaceous matters are also present. The

colour is generally dark, blackish or brownish, occasionally bluish.
These shales are chiefly found in Sweden, Norway, and Belgium,
at La Tarentaise, Whitby, Glasgow, and also at Lautenthal in the
Harz Mountains, and in several parts of Thuringia, Westphalia,
etc. The deposits are mainly situated between the oldest sand-
stone and the orthoceratic chalk of the silurian age, or in the
carboniferous system (Knapp). These shales are of somewhat
variable composition, as will be evident from the subjoined
analytical tables furnished by Knapp.
As a rule, apart from iron sulphide, the matter soluble in
acids represents a very small fraction of the total substance.
When freshly extracted, the proportion soluble in water is
extremely low, and contains no salt of aluminium or iron.

When exposed to the air, these shales, especially when rich in
iron sulphide, effloresce and crumble down. This phenomenon,
which, moreover, forms the basis of the treatment to which they are
subjected, is due to the presence of pyrites, which absorbs oxygen
from the air, is converted into iron sulphate, and yields sulphuric
acid, which, reacting on the clay present, furnishes aluminium

sulphate.
103. Efflorescence (Weathering) and Roasting. The

object of this operation is to convert the bulk of the sulphur
present into salts of iron and aluminium.

In the first place, a flat surface is covered with stamped clay,
over which is laid a bed of fuel, consisting of faggots or brush-
wood mixed with small coal, care being taken to leave channels
in the mass. This done, the mineral is piled up and the fuel is
lighted. When the mass is well alight, fresh quantities of shale

are added until the heap size.
is The openings left
of sufficient
for the admission of then closed, and the heap is covered
air are
with a layer of spent mineral from the extractors. The object

of the operation is to retard the decomposition of the mass,
regulate the oxidation, and prevent the loss of sulphur dioxide

and sulphur which have a tendency to escape.
trioxide, By
repeatedly pumping water over the surface, the temperature is
maintained at a degree suitable for rendering the decomposition
as complete as possible. When the oxidation is complete,
and the heap has been left for a considerable time, the mineral
is ready for extraction. It contains a large quantity of soluble
matter, chiefly consisting of sulphates of iron and aluminium

sulphate.
The following analysis (Knapp) shows the composition of
oxidised Hurlet and Campsie shales :
1
04. Lixiviation. This operation is performed in large
boxes with perforated bottoms, the filtering surface being com-
posed of sleepers covered with battens, and the whole topped
with a bed of brushwood. On this bottom the roasted mineral is
piled to a depth of about i
3 inches, and the extracting liquor
is left in contact with it over night. The mother liquor from the
alum crystallising pans is employed for the first extraction, pure

water being used afterwards.
The crude extracts are stored in cisterns, and after the
bulk of the impurities have settled down are removed for
concentration.
105. Treating the Extract Liquor. The method adopted

varies according to the kind of shale employed. In the case of
Whitby which contain a considerable amount of magnesia,

shales,
the liquor contains magnesium sulphate, and the treatment
pursued is to evaporate the solution to sp.gr. ri25 1*137 m

leaden vessels, the mass being then left to clarify ; and, after
a further concentration to sp.gr. 1*25, a sample is tested for the
percentage of alum. When, as a result of evaporation, the liquor

has attained a density of 1*4 to 1*5, according to its content of
ferrous sulphate, it is treated with the necessary amount of
potassium chloride (or sulphate) or ammonium sulphate, in con-

centrated solution, and is run into the crystallising pans, where
the alum crystallises out, the crystals being purified by washing

and repeated re-crystallisation. The mother liquor is concentrated
by evaporation in order to obtain, in succession, crystals of
magnesium sulphate and ferrous sulphate.

In the case of Hurlet shales the extract liquor is free from
magnesium sulphate. The evaporation can be carried on in
reverberator}^ furnaces heated from above, there being no pro-

duction of any superficial incrustation to retard the conduction of
heat. During this stage abundant deposits are formed of basic
or dehydrated salts of iron, and of calcium sulphate. After
concentration the liquor is employed in the production of alum.
B, Treatment of Pyritic Lignites
1 06. Introductory. The pyritic lignites known as alum

earth (terre d'alun, cendres de Picardie, cendres pyriteuses] have
been, and still are, largely employed for the manufacture of alum
and ferrous sulphate. In France they have been utilised ever
since the eighteenth century, and, thanks to the abundance of the
mineral and the regular bedding of the deposits, they are still
worked mainly in the departments of Aisne and Oise. At one
time they constituted an important article of commerce as a
stimulating fertiliser for agricultural purposes, there being in 1825

no less than fifty works engaged in the department of Aisne alone
in extracting and oxidising these lignites with a view to their
employment in this direction. The price of the finished product
was at that time 5 o centimes per hectolitre ( = I f d. per bushel)
ex works.
Concurrently and in the same district there were seven

factories dealing with pyritic lignites, five of them producing
alum and ferrous sulphate, the remaining two merely evaporating
the extract liquor in order to prepare the magmas employed as
raw material in the other works. With the exception of two
which still survive, all these factories, and others succeeding them,
have now disappeared.
The oldest of these factories is that at Urcel,* which is still
in existence. It was erected in 1786 by an Englishman named

Chamberlain, in virtue of a decree of the Royal State Council
dated 2Oth May of the above-named year, by which permission
was granted to the said Chamberlain, for the space of twenty
years, to manufacture copperas, or vitriol martial, by a secret

process of his own.
In 1791 the concessionnaire ceded his rights and factory to
the brothers Moreau d'Olibon. For nearly 20 years the factory
produced an impure green copperas, which was unable to compete
" "
with the " de Beauvais and " English copperas, without the
nature of the impurity being known. When, however, it was
recognised as alumina, or rather aluminium sulphate, and Vau-
quelin's labours were made known, the production of alum was
carried on as well an example followed in the other factories
established at that period. Finally, in 1807, the expiring con-
cession was renewed, in perpetuity, by the Government.
Other factories were very soon started in the same depart-
ment, the second authorised by a Governmental decree of
May 5, 1802 being erected round the old Abbey of Cuissy near
Beaurieux. The discovery of the vast deposit of pyritic lignite
*
Urcel is a small place in the department of Aisne, about 10 kilometres from Laon
on the high road to Paris.
underlying the valley of the Aisne was made as a result of the

work carried on by a Mons. de Belly de Bussy, in prospecting
for coal.
In consequence of difficulties experienced in the extraction of

the mineral, the Cuissy works were transferred in 1822 to the
village of Bourg, about 5 This latter factory,

kilometres away.
which in its time attained a certain importance, has now passed
away.
Following the Bourg works came those at Chailvet,* still in
existence. They were installed and authorised by a decree
dated May 11, 1807 for the manufacture of copperas, alum,
artificial soda (soude factice), and Prussian blue. The reason
these works were established for the production of artificial soda
was that, on account of the Continental blockade and perpetual
state of war at that period between France and her neighbours,
commercial relations were interrupted and no Spanish soda could

be imported. However, this branch was discontinued after the
peace of 1814, and Prussian blue was never at any time manu-
factured in a continuous manner consequently, only alum and ;
ferrous sulphate were produced.

The works at Ouessy, about 5 kilometres from La Fere and
i kilometre from Quentin Canal, were built in 1810, and
St.
authorised by a royal ordinance dated March 16, 1819.

Here also the manufacture of artificial soda was carried on at
first. At about the same period, namely in 1812, another
factory, since disappeared, was started at Andelain.
The treatment of lignites, as carried on in the department of
Aisne, was also pursued in other districts possessing analogous
deposits ; but, with the exception of the two factories mentioned

above, all the works have now ceased operations.
The technical history of this industry in France is of only
minor interest, there being scarcely any improvements to chronicle.
One point, however, is interesting to record, namely, that in place
of the peat or lignite at first employed as fuel in nearly all the
works, coal is now used. In other respects little or no changes

*
Chailvet is a small place about I kilometre north of Urcel and some IO kilometres
away from Laon.
have been made, and the sum-total of the advance made is, so to
speak, nil.
This is due to the long-continued era of prosperity enjoyed
by the manufacturers, owing to the absence of any competition

which, by lowering prices, would have obliged the producers of
alum and ferrous sulphate to work more economically. Another
reason was the lack of technical education amongst them, in
consequence of which periods of crisis found them unarmed and, ;
in addition, the absence of unity between the manufacturers of

aluminous products led them into internecine struggles instead
of endeavouring to combine against foreign competition.
Matters began to draw to a head after 1 866, owing to the
development of the new aluminium sulphate industry founded in
France by Messrs. Pommier of Gennevilliers. Very shortly after,
this competition was intensified by the expansion of the alum

industry in other countries, and the importation, at low prices, of
English alum (mainly Spence's), Belgium alum and aluminium
sulphate from the Ampsine factory, Italian alum from La Tolfa,
etc., the last named afterwards becoming established at Rouen,
where a factory for treating La Tolfa alunite was built under the
very windows of the Maletra works.

The Aisne alum manufacturers, who were at the head of the
market, believed their trade was ruined, whereas it was only com-
promised ; and, wishing to make the most of their factories while
there was still time, they raised their prices. The logical con-
sequence of this step was to hasten the displacement of alum by

aluminium sulphate, which at first had made small headway
owing to defects in manufacture and conservatism on the part of
various consumers.
Finally, the resultwas a general break-up in the price of

alum, and a diminution in the demand. The struggle, however,
adjusted itself, and a syndicate combined a number of French
producers. For the Aisne alum makers this was merely a palli-
not a cure, but fortunately they had ferrous sulphate to fall
ative,
back upon, and, though the demand was at first small, the trade
grew, prices kept up, and for some years makers were able to
work at a profit.
97
This state of things was, however, transitory, and not even

the continually increasing call for ferrous sulphate, its ready sale,
and, of late, the imposition of a protective duty on alum, could

arrest the decadence of the industry employing lignites. Purer
and drier grades of ferrous sulphate than those produced by the
alum makers were put on the market by English competitors, and
in consequence of the utilisation of previously wasted ferruginous
bye-products from other industries metallurgical and oil refining
the resulting fall in prices hastened the fall of most of the
lignite treaters in France. At the present time only two import-

ant factories of this class have been able to survive, as a result
of a combination of economic considerations, such as position,
proximity to means of communication, and powerful equipment.

These two works, one at Chailvet, the other at Urcel two
adjoining communities in the department of Aisne still turn
out about 2500 to 3000 tons of alum about of the total
consumption every year, and 5000 to 6000 tons of ferrous
sulphate.
107. The Raw Material. A. DEPOSITS. Pyritic lignites are
extremely abundant in are of very fre-

certain localities. They
quent occurrence in the extensive plains of Northern Germany,
deposits being found near the Oder, at Freinwald, Gleissen,
Schermeisel, and Muskau ;
others at Mansfeld, Bornstedt, Hol-
denstedt, and finally at Schwemsal on the Mulde.

In France several deposits occur in the department of the
Rhone, and others in Picardy, Oise, the Ardennes, Champagne,

etc., the largest, most regular, and most easily worked, however,
being those in Aisne.

The deposits were formed
in stagnant lagoons during the
Tertiary period. An
examination of the geology of Aisne shows
that the cretaceous formations, which occupy a large area in
Thierache, the Picard and Champenois districts, disappear to-

wards the south-west under the tertiary plateaux of the Laon
district, extending from Laon to the southern border of the
department. They are arranged in parallel planes sloping from

N.E. to S.W., so that the formations appearing on the surface
of the northern plateaux are found to occupy progressively lower
positions on the slopes of the intersecting valleys farther south,

and finally, in the southernmost valleys, form the beds of the
valleys themselves. The arrangement of the entire series of

tertiary beds is in the following order Plastic clays underneath,
:
resting on white chalk then, in succession, nummulitic sands,

;
coarse lower and upper limestones, Beauchamp sands and sand-

stones, St. Ouen gypsum, green marls and pottery
travertine, clay,
Brie travertine, Beauce travertine, Fontainebleau sands, and mill-
stone clays.
The plastic clay found on the surface in the Vermandois
district, the mass of which is of cretaceous origin, forms the base

of the Laonnois plateaux! It also at one time covered the
Souche district, where it has left as evidence a number of isolated
hills covered with thick beds of diluvial sand. Even at one end
of the Laonnois district superposed on a thick bed of
it is
Bracheux sand, the remains of the newest cretaceous beds, which

have entirely disappeared from the Souche basin, and are masked
by plastic clay in the Vermandois district, but reappear in the
high Thon valley.
At the base of the plastic clay are lacustrine marls and lime-
stones, worked, for the production of hydraulic lime, in the south

of the department. The clay itself encloses the pyritic lignite de-
posits, worked manufacture of alum and extending for
for the
a length of 45 miles between Catelet and Reims, the breadth

between Houblieres and Goulancourt being 17 to 18 miles.
This clay occupies the bed of the Aisne, Vesle, and Lette
valleys ;
it is impermeable, and forms the main water-level of the
department.
The section of the strata at Chailvet, Urcel, etc. (Fig. I I
3),
shows, in the firstimmediately below the surface mould, a

place,
bed of siliceous sand, enclosing in places reniform masses of soft
sandstone, which here and there is replaced by a workable (and
actually worked) layer of hard sandstone. This sandstone is rich
in flora, leaf prints of laurel, oak, chestnut, sallow, etc. being very
plentiful. The animal kingdom is represented by shells, mainly
cerites, embedded in siliceous cement.
Underneath this layer is an interesting shell-gravel of con-
siderable thickness, constituted by the agglomeration of an

infinity of various shells cerithium> melania, and, above all,
ostrea bellomcina, many of which are in a perfect state of pre-

servation. This gravel is used for ballast ;but, despite its high
percentage of calcium carbonate and its approximation to the

composition of hydraulic limestones, the attempts made to work it
up for lime have proved failures.

Next follows a very compact layer of sand, agglomerated by
an argillaceous cement and we then ;
come to a workable deposit, 6 to

10 feet thick, composed of alter-
nate strata of pyritic lignite and

aluminous clay resting on a bed of
clay 10 to 13 feet thick. The top
part of this clay bank is black, laden
with organic matter, and rich in
pyrites ;
the lower portion white.
The content of alumina varies be-
{: ^ _ ..
;
..__ _ _ _-'<P
tween 20 and 28 per cent., and it is
worked for brick-making.

Between the clay bed and the
seam of lignite is a stratum enclosing
a large number of renal concretions
3>
of pyrites, all scattered on the same FIG. 113. Section of the strata
horizontal level.
The deposits, however, are not all of uniform regularity, the
bed being at Chermizy, for example, much thicker, more clayey,
and containing veins of dolomite.
B. COMPOSITION AND PROPERTIES OF THE ORE. The
composition of these ores varies considerably with the locality
and the place where the samples are taken. At Chailvet the top
layers are very poor in pyrites (8 to 9 per cent.), that in the

middle of the bed is a little richer (12 to 15 per cent.), and the
lower portion is very rich indeed (20 to 30 per cent.). The
following table shows the limits of variation.
The percentage of organic matter is from 20 to 30 per cent.
From the manufacturing point of view, an average of i

5 per cent.
ri., U. U LA.
of iron disulphide can be counted upon. In addition to this
principal element, the pyritic lignites contain a notable quantity

of clay, a high proportion of ferric oxide combined with the
organic matter, a little magnesia and chalk, traces of phosphoric
acid and potash, and 0*2 to 0-3 per cent, of nitrogen.
At Bornstedt three classes of ore are found, the analyses of

which are given below (Knapp) :
The colour of the pyritic lignites varies from greenish black

to lustrous They are more or less compact. In the
black.
fresh conditionthey yield up no sulphates to water, with the
exception of a minute quantity of calcium sulphate. They
exhibit the same property as the pyritic shales of weathering
on exposure to air, heat being liberated and soluble salts formed.
They are always more or less mixed with sand and clay, and
sometimes contain flakes of mica. Neither sulphur nor pyrites
can be detected by the unaided eye or under the magnifying
glass. Nevertheless, by means of careful levigation, a small
quantity 'of pyritic granules can be obtained from the clay

AND SULPHATES OF IRON 2OI
separating the strata of lignite. A small quantity of free
sulphur and resinous bodies can be extracted by means of

carbon disulphide.
Boiling hydrochloric acid attacks pyritic lignite, furnishing a
greenish-yellow liquid, and liberating a very small quantity of
H 2 S.
The liquid chiefly contains ferrous chloride, with traces of
ferric chloride. When strongly heated the pyritic lignite parts
with sulphur, which sublimes. This property is due to the
presence of pyrites.
C. METHOD OF WORKING THE DEPOSITS. The first thing
is to remove the top soil in trucks. The workmen, under the
supervision of a foreman, who has also to keep the tramways in
order, get out the soil with picks and dump it in the hollows left
by previous extractions. The lands thus reconstituted are sterile

and cannot be replanted for 4 to 5 years. Each truck is served
by three men, who receive on an average 3 francs per diem and ;
the amount of earth removed is about 8 or 9 cubic metres

(
i 2 to 13 cubic yards) per man (computed on the space actually
cleared), the work thus costing about 35 centimes per cubic
metre (2|d. per cubic yard).
This preparatory work is carried on during the winter, and
the actual winning of the mineral is commenced in the month of
April. The lignite is taken out in steps, and, by reason of the

compact nature of the mineral, costs 40 centimes per cubic metre
(3d. per cubic yard). The seam being immediately overlying a bed
of clay, the work is often retarded by water, which has to be drained
off through channels cut for that purpose through the workings.
The mineral is conveyed to the works in trains of 5 or 6
trucks, and is there tipped in long, parallel, prismatic heaps,
measuring about 3 cubic metres per running metre, as shown in
section in Fig. i 1
4. Since each of the existing works in
France deals with 10,000 to 14,000 cubic metres of mineral per

annum, it is evident that the superficial area required is con-
siderable.
Occasionally, when the labour of open cast working is too

difficult and expensive, the mineral got by driving headings.
is
This system, however, has little to recommend it, since a con-

2O2 MANUFACTURE OF ALUMINIUM SULPHATE
siderable quantity of mineral has to be left in the form of pillars

to support the roof; and inconvenience is often caused by water.
D. PREPARATION OF THE MINERAL. The preparation of
pyritic lignites, in view of their ulterior treatment for alum and

ferrous sulphate, is very similar to that pursued with shale. The
nature of the various constituents renders them particularly
FIG. 114. Preparing the mineral.
susceptible to oxidation ;
and in fact, under the influence of
aeration and moisture, pyrites is not slow to fix oxygen. The
temperature in the interior of the heaps rises rapidly, and if the
operation is allowed to continue for a month or six weeks the

mineral takes fire spontaneously. This, however, is not waited
for, the oxidation being assisted and regulated by turning the
heaps over with shovels to facilitate the access of air, whilst, at

the same time, small fires (Fig. 115) are kindled at intervals and
covered up as required. To enable the combustion to extend,
three flues are constructed of faggots.
The work of this first stage retenage, as it is called costs
about 10 or 12 centimes per cubic metre (fd.-id. per cubic yard).
Under the influence of this treatment, and provided the
climatic conditions are favourable, oxidation proceeds actively,
and combustion slowly progresses from the centre of the heaps
outwards, a whitish or yellowish
efflorescence forming on the sur-
face,and an abundance of steam,

carbon dioxide, and sulphur di-
oxide being disengaged. When
the fire reaches the surface, and
FIG. 1 1 5.
-Firing the heap. combustion becomes too ener-
getic, the
temperature of the ignited mineral is moderated by
covering the heaps with wet spent mineral from the extractors,
and pumping water into the mass. At the end of 3 or 4 weeks

the mineral is ready for the second stage, the object of which
is to extinguish the fire (whilst still aerating the mass) and
prevent the total destruction of the ferrous sulphate under the

influence of a progressively heightened temperature. After
leaving the mass to ripen for some time, it is put in larger

heaps before the bad weather comes on. These heaps measure
20 metres across the base and 1 2 metres high, and their
size is sufficient to protect them against the rains. The
mineral is then ready for lixiviation, but may with advantage
be left to age a little longer, this considerably improving the
quality as a result of complementary oxidation and various

secondary reactions. The loss in weight during combustion is
about th to ird.
The reactions occurring throughout this prolonged period and
the successive manipulations are of the following nature : The
efflorescence due to the fixation of atmospheric air by the
is
pyrites, and the production of ferrous sulphate and sulphuric

acid, the latter then acting on the alumina of the clay to form
aluminium sulphate, according to the following simple reactions :
(1) FeS 3
(2) 3 H 2 S
though in reality matters do not proceed in such a simple manner.
At first a portion of the sulphur distils and forms magnificent
lemon-yellow crystals on the surface of the heap. On the other

hand, the conversion of the pyrites into ferrous sulphate, with
the production of sulphuric acid and subsequent formation of
aluminium sulphate, is far from being so simple as the above

equations would imply. The amount of sulphuric acid produced
represents only a very small fraction of the sulphur in the pyrites,

the greater part being converted into SO 2
FeS 2 + 60 + ;H 2
= FeSO,, ;H 2 O + SO 2 .
A fractional portion of the SO 2

is lost by dissipation into the
air, along with the water vapour and carbon dioxide resulting
from the combustion of the organic matter. The rest is retained
in the
heap, and, in the presence of water vapour and the porous
cinder, absorbs oxygen, thus forming sulphuric acid, which acts on
I
the alumina of the clay. This reaction is greatly assisted by the

presence of water vapour, and it is for this reason that the
occurrence of spontaneous ignition is not awaited, since not
only would that proceed from the surface towards the centre,
which would be unfavourable to the utilisation of the sulphur,
but also would go on in a desiccated medium and produce
nothing but a large quantity of ferric oxide or insoluble sub-

salts, and a relatively small amount of aluminium sulphate.
Consequently the roasting fires are lighted whilst the material

is still damp.
Ferrous sulphate is unstable ;
it absorbs oxygen, and is con-
verted into soluble ferric sulphate and insoluble sub-salts. At
the time of roasting, the heat is sufficiently intense to decompose
a portion of these iron salts ;
and ferric oxide is formed simul-
taneously with the liberation (distillation) of sulphuric acid, which
attacks the clay immediately. This decomposition of the iron
salts would be carried almost to completion were it not inter-
rupted by the second handling ; and, in fact, the old alum makers
followed this course, the red cinder obtained by them being very
rich in aluminium sulphate but poor in ferric sulphate, and par-
ticularly so in ferrous sulphate.
Both ferric oxide and ferric sulphate play a part in the
production of aluminium sulphate, their oxidising properties

enabling them to convey oxygen to sulphurous acid and convert
it into sulphuric acid. Moreover, the mineral, when lixiviated
immediately after roasting, yields a lower proportion of aluminium
sulphate than when it has been left to mature a long time in
large heaps. Here not only the extra oxidation, but also the
reaction of the oxidation products on the excess of clay in the
material, have to be taken into account, since both ferrous and

ferric sulphate in time react on alumina and form the sulphate of
that base. As this action, though gradual, certainly exists, it
becomes a matter of interest to watch over the cinder previous
to lixiviation.
The reactions going on in the heap are therefore of an
extremely complex nature. They are in all respects identical
with those occurring in the treatment of shales, and are very

AND SULPHATES OF IRON 20 5
difficult to regulate, atmospheric conditions which vary from

year to year being a factor of the highest importance.
The composition of the material ripe for lixiviation may
therefore be expected to vary within very wide limits ;
and that
this is actually the case the following analyses will show :
The insoluble matter consists chiefly of organic substances,

silica,unattacked clay, iron peroxide, a little of the soluble
sulphates, unoxidised sulphur, etc.

The cost of the mineral when ready for lixiviation varies
according to the year, but may be estimated on the following

basis, in shillings per cubic yard (about I
5 cwt.) :
Extraction, Piling in Rent of Interest, Depre- Total Cost per

Haulage, etc. Cost of Tools. Turning. heaps. Ground. ciation, etc. cubic yard.
i~2i2 0-091 0*182 0-182 o -

i2i 0-333 2-I2I
1 Manufacture of Ferrous Sulphate.

08. This entails the
handling of a very considerable volume of liquor, and con-
sequently, to keep the expenses within reasonable bounds, the

works are generally laid out on a slope to enable the liquid to
flow by gravitation from one department to another, the lixiviation
plant being situated on the highest level. A plan of the general

arrangement of works for treating pyritic lignites is shown in
Fig. i 1 6.
A. LIXIVIATION. This operation is intended to separate the

soluble matters in the oxidised mineral from the insoluble portion.
The plant comprises -
(i) A tanks G, G, G (Fig. 1 1 8), lined

series of dressed stone
with a false bottom of boards supported on beams H, H, and
carrying a thick filtering layer of brushwood I, I. Each tank is

connected with its neighbour by a conduit K, arranged in such a
manner that the liquor drawn off from No. I

(for example), at the \
bottom, is discharged into the top of No. 2. Moreover, each
FIG. 116. General plan of works for treating pyritic lignite.
a, Lixiviation tanks ; l>, receptacles ; c, preparatory tanks ; d, lead-lined tanks ; e, copper

tanks ; F, crystallisers ; g, leaden re-casting boxes ; h, leaden turbines ; i, stores ;
/, generators ; K, engine ; L, sawmill ; M,

N, offices ; P, dwelling-
laboratory ;
house ; Q, fire engine R, soldering shed S, dwellings and offices (accommodation

; ;
for 4 foremen) T, carman's

;
rooms U, forge V, cart house. Part of the stores,
; ;
cooperage, stables, forage shed, granary, mechanics' and plumber's rooms, iron
stores, water reservoirs, etc., are situated outside the limits of the plan.
tank can be put in communication with any other member of the
series by means of a system of conduits L, L, which also serves to

AND SULPHATES OF IRON 2O7
convey the weak liquor employed for lixiviation. Fresh water is
supplied, through a conduit M, to each tank.
In front of each of the tanks is a small reservoir N, N, into

which the liquor drains' through the opening P after traversing
the layer of mineral O. This reservoir communicates with the

exterior by two conduits, one of which, Q, discharges the strong
liquor into a channel R, which delivers into the temporary storage
reservoir S, whilst the other T serves to drain off the weak liquor,
which runs away through the channel U into the cistern V.
The system of canalisation is formed of leaden pipes, or else
of hollowed tree trunks embedded in masonry, the circulation of
the liquor being regulated by wooden plugs. The tanks and
reservoirs are of dressed stone, and, to prevent leakage, are sur-
rounded by jackets of clay followed by a layer of rammed chalk.

(2) A pump, or Korting injector, raises the weak liquor from
the cistern V, and returns it to the lixiviation tanks.
(3) A set of tracks and points for the tramway trucks.

The lixiviation is carried on in the open air and in a
systematic manner. At Chailvet the installation is composed of

eight "elements," of about 1080 square feet in superficial area
and 3 feet in depth, forming two separate batteries.
" "
Each element takes a charge of about 3 tons, spread out to
a depth of some 16 inches, ft is delivered in trucks, and each
workman, in return for a daily wage equivalent to 3 shillings, has

to bring i 2 cwt. of mineral to the lixiviation tanks, spread it, and
afterwards remove the corresponding quantity of residue to the
waste heap.
In a normal season the strong liquor measures 28 of the
Baume hydrometer, the weak liquor having a density of 10 Be.
A 99 gallons of 28 Be. liquor.
cubic yard of cinder will yield about
The quantity obtained, however, varies between somewhat wide
limits, according to circumstances, such as the richness of the
mineral, the percentage of moisture, etc. ;
and the same also
applies to the density. Nevertheless, it is but seldom that the
figures fall below those cited.
The 28 Be. liquors collected in the reservoir S deposit there

the clay and impurities with which they are laden. They then
dark reddish - brown appearance, and contain all the

have a
of the but vary considerably in
soluble constituents cinder,
relative composition, according to the nature of the cinder

under
treatment, as the following figures will show :
Composition in Grams per Litre
a source of trouble.
The lixiviation residue is great
it as fuel for evaporating the
Attempts have been made to utilise
it on a hearth with forced draught.
How-
liquors, by burning
this had to be abandoned by reason of the low percentage
ever,
of carbon, in consequence of which the evaporation went on only
Figs. 117 to 121 . Plan and Sections of Lixiviation Plant.
.K
TuMj
FIG. 117. Plan.

AND SULPHATES OF IRON 2C9
G
Goupe CD.
FIGS. 118 and 119. Transverse sections.
FIG. 1 20. Coupe section.
ffiDnODDDODC
FIG. 121. General plan, showing arrangement of lixiviation tanks,

channels, reservoirs, and tramways.
very slowly, even when a large quantity of the fuel was consumed ;
and also on account of the extra labour involved in stoking, the

vast quantity of cinders produced, and their fusible character,
which led to the constant obstruction of the draught.
The analysis of this residue, by A. Vivien of St. Quentin,
furnished the following figures :
Water 2^28] Carbon

9-55
Organic matter Volatile carbonaceous matter
Mineral matter
.
9-33
5574
Sulphur (as pyrites) 2-52

Free sulphur 0-17
SO 3 in combination 271
2IO MANUFACTURE OF ALUMINIUM SULPHATE
In order to calculate the calorific power of this residue as
fuel, the composition may be conveniently expressed as follows :
18-98
5574
We then have :
(1) Heat disengaged by the combustion of the carbon

i
1-63 x 8080 = 93970-40 cal.
(2) Heat disengaged by the combustion of the hydrogen,

assuming the 6-32 per cent, of oxygen plus nitrogen contains
4-32 of oxygen
29,000 (i'03 = 14,210 cal.

4-r^
(3) Heat disengaged by the combustion of the free sulphur
and the sulphur in the pyrites

2162 x 2-69= 581578 cal.
Or a total of
93970-404- 14210-00+ 581 5-78 = i

13996-18 cal.
Allowance must, however, be made for loss : thus

The evaporation of the moisture present absorbs an amount
of heat estimated by the formula
Q = P(6o6'5 +0-305 x t-G).

Then, assuming the evaporation to be effected at 1 00 C.,
whilst the initial temperature of the fuel is I

5 C.,
Q= 25(606-5 +0-305 x 100 - 15)= 15,560 cal.
Or, taking the final temperature of the vapour as 300 C,

the last-named value becomes
15,560+ 25 x 200 x 0-475 = i7>935 cal.,
0-475 being the water vapour.

specific heat of
Again, a certain amount of heat is consumed in decomposing

the pyrites ;
and be approximately estimated, the heat
this may
of formation being 750 cal. per each i kilo, of sulphur combining
AND SULPHATES OF IRON 2 1 I
with iron. The heat absorbed in "the decomposition of the pyrites

will therefore be
750 x 2-52 = 1890 cal.
Altogether there are 2-69 kilos, of sulphur, furnishing 5-3 8

kilos, of SO 2
. To this must be added the sulphur in combination
as sulphates, namely roS kilos., yielding 2*16 kilos, of SO 2, the
total SO 2 produced being therefore 7' 5 4 kilos. This gas being
liberated at 300 C. (an assumption made in order to simplify the
calculation), and its specific heat being 0*409, the amount of heat
lost from this cause will therefore be
7-54 x 0-409(300 15) = 878-9 cal.
On the other hand, heat is absorbed in the decomposition of
the SO 3, namely
2300 being the difference between the heat of formation of the
sulphur combining with oxygen to form SO 3 ,

and that of the
same quantity of sulphur in forming SO 2 .
The i
1-63 kilos, of carbon produce 42-64 kilos, of CO 2,
the
specific heat of which is 0*2025. The heat consumed in this
respect will be
42-64 x 0-2025 x 285 = 2463-82 cal.
Again, the 2 kilos, of nitrogen (in the fuel) account for a loss of
2 x 0-244 x 285 = i
39 cal.
The next item to be estimated is the amount of nitrogen in
the air required to support the combustion of the fuel. Taking

first the theoretical quantity, we find that
Oxygen required for the combustion of 11-63 kilos, of carbon =31*01 kilos.
,, 0-49 ,, hydrogen = 3-92

,, ,, ,, 2*69 ,, sulphur = 2^69 ,,
Total . . .
37 -62 kilos.
This corresponds to 163-56 kilos, of air, of which i

25-94 kilos, is
nitrogen. The quantity of heat abstracted on this score is
125-94 x 0-244 x 285 = 8789-40 cal.
The heat removed by the water resulting from the combustion

of the hydrogen is
9-27 x 0-475 X 285 = 1254 cal.

On adding together these amounts of waste heat we obtain

the total
17,935 + 1890+879 + 77-1-2464+ 139 + 8789+1254

= 33,427 cal.
Under
The
of residue would produce
losses of heat amount to
......
the conditions assumed above, the combustion of 100 kilos.
....... x
.
113996
33427
cal.
,,
air) of ...........
Leaving a useful balance (combustion in presence of I vol. of
80569 cal.
If, however, the combustion be effected in presence of a larger

volume of air, the losses increase. Thus the specific heat of air
being 0-2377 for each extra volume (163-56 kilos.) of air, the
loss will be augmented by
163-56 x 285 x 0*238 = i

1,094 cal.
When, as is usually the case, combustion takes place in
presence of a threefold volume of air, the amount of residual

available heat will therefore be only
80,56911,094x2 = 58,381 cal.;

a very low figure, although no allowance has been made for the
other losses specified above.

If we desire to estimate the amount of such fuel required for
the concentration of the lixiviation liquor, the calculation is now

easily made.
Assume that I cubic metre of liquor measuring 28 Be. has
to be concentrated to 42 Be. strength,
The specific gravity corresponding to 28 Be. is d = 1-2407,
42 Be. is d' = 1-4100.
Then, taking V to represent a certain volume of solution, of
specific gravity d; and ^ the weight of water to be evaporated
in order to bring the specific gravity up to d', we may set down
the equation as
V(d'-d)=x(d'- i),
from which
Hence, taking V= 1000 litres,
x= 1000 1-4100- 1-2407

1-24
= 413 kilos, of water.
1-410-1
If we now apply the formula
+0-305 t-ff)
and substitute as follows,
P = 41 3 kilos.
f= 100 C.
0=i5C.
we have
= 413(606-5 + 30-5
- 15) = 256,886 cal.
as the quantity of heat theoretically requisite for the evaporation
of our 4 1
3 kilos, of water. To this must be added the amount
necessary to raise to 100 C. the residual volume of liquid, the
specific heat of the liquor being assumed equal to I
587 x 85 =49,895 cal.

The total amount of heat required is therefore
256,886 + 49,895 = 306,781 cal.;
a figure corresponding to a consumption of about 520 kilos, of

fuel, without making any allowance for the losses. Hence this
method of utilising the residue in question hardly appears
practicable.
B. REDUCTION (VERDISSAGE) OF THE LIQUOR. The
presence of ferric sulphate in the liquors is objectionable, since,
in the subsequent operations, it would form iron alum, and thus
contaminate the potassium-, or ammonium alum, produced. It is
removed by reduction, i.e. conversion into ferrous sulphate, under

the influence of iron and sulphuric acid.
With this object, the liquor in the storage reservoir is trans-
ferred by means of a conduit C (Figs. 122 and 123) and gulleys

c to two dressed-stone tanks A and B, connected by an aperture
a, which is kept closed during the treatment.
At one side is a leaden boiler E, heated by two furnaces F, F,
and communicating with the tanks A, B by conduits G, H. A
leaden vat D
containing sulphuric acid discharges into the two
tanks through a branched pipe d, which is closed by a leaden
plug e. On raising the latter the desired quantity of acid 15

to 20 kilos. (33 to 66 Ibs.) of 60 Be. acid per cubic metre

(220 galls.) of liquor is run into the tanks, and a certain
quantity of scrap-iron is thrown in. Heat is then applied to the
boiler, and, owing to the arrangement of the conduits H and G, an
inverse current is set up between this vessel and the tanks, the
cold liquor from the latter passing from A or B towards E, via G,
whilst the hot liquor from E passes towards A or B through H.
The liquor in the tanks is thus heated, and rapidly attacks the
.
s ?'K
Section M N.
FIGS. 122 and 123. Plan and section of the reduction plant.
A, B, Reduction tanks E, leaden boiler, with furnaces F, F

; D, sulphuric acid tank ; ;
G, G, H, H, conduits connecting the boiler and tanks C, feed pipe for the liquor to ;
be reduced c, c, gulleys connecting C with the tanks

; d, feed pipe for acid ; ;
a, gulley connecting tanks A, B ; L, discharge pipe for reduced liquor.
scrap-iron, itself gradually turning green, so that, at the end of

about i 2 hours, all traces of ferric sulphate will have disappeared
and the liquor ready for evaporation.
is
The process can also be effected on concentrated very hot

liquor and this plan is the better, although more difficult to
;
regulate and carry through.

C. CONCENTRATING THE LIQUOR. This is an operation of
great importance in the pyritic lignite industry. The liquors
measuring 27 to 28 Be. have tobe concentrated to 40 Be.
(measured hot) ;
and when it is remembered that a cubic metre
of cinder furnishes 600 litres of liquor, that this volume yields

about 200 litres of residual water at 31 Be., which has to be
again concentrated, and so on, an idea will be gained of the
volume of material to be treated, the amount of water to be
evaporated, and the considerable weight of coal required for the
operation. In fact the quantity of coal consumed in the pro-
FIG. 124. Reverberator}- evaporating furnace for reduced liquor.
duction of 1200 tons of alum and 2500 to 3000 tons of ferrous

sulphate is not less than 1500 tons,1000 of which are required
for the evaporation of the liquors.
Not many attempts have been made to secure the proper
utilisation of the fuel ; and, in fact, the nature of the liquors to be
treated, their acidity, the ease with which, under the influence
of slightly prolonged heat, they deposit coherent sediments of
FIG. 125. Double-bed evaporation furnace.
gypsum, basic ferric sulphate, and dehydrated ferrous sulphate, all
constitute difficulties hard to surmount.

The reverberatory furnaces adopted in England have also
been employed in France. In their simplest form they are very
long in proportion to the width, and the bed takes the form of a
dressed-stone basin to hold the liquor to be concentrated. The
arch is greatly flattened, in order to compel the gases to circulate
as near as possible to the surface of the liquid. In these furnaces
the fuel is utilised in a fairly advantageous degree, their main
drawback being the contamination of the liquors by ashes and soot.

Several improvements have been introduced, such as the
Cti'jJe /stumrtf EJ f
FIG. 126. Section along EF. Leaden evaporating pan viewed from above, and
showing the appearance of the bottom.
combination of two evaporating basins with only one fire (see

Fig. 125), the basin nearest the smoke-stack being on a higher
level than the other, and serving as a preliminary heater.
However, these furnaces have been superseded by leaden evaporat-
ing pans, which have the advantage of being inexpensive to keep

in order, of being worth nearly their full value when broken up,
and of keeping the liquors clean, though they waste heat in a
'.Sectionfalong GH.
FIGS. 127 and 128. Leaden evaporating pan. Plan and section
showing details of firegrates and flues.
deplorable manner, not more than 5 to 5i Ibs. of water being
evaporated for i Ib. of coal consumed.

This defect is due
(i) To the great thickness of lead necessary to preclude the
possibility of the walls getting out of shape under the influence

of heat and the internal liquid pressure ;
(2) To the low coefficient of conductivity of the metal ;
(3) To the formation of incrustations of gypsum, basic ferric
sulphate, and anhydrous ferrous sulphate ;
(4) To the viscosity of the liquors to be concentrated ;
(5) To the large superficial area of the liquor, favouring loss

of heat by radiation.
FIG. 129. Leaden evaporating pan. Longitudinal section along CD.
These leaden pans are of variable dimensions. Those at
Chailvet have an area of 25 square metres (270 square ft.),

and
are heated by naked
flame. The direct impact of the fire is
prevented by an arch, and the hot gases are led under the
bottom of the pans, where they make a triple circuit through flues
of masonry, the roofs of which flues are formed by undulations
of the bed of the pan. The concentrated liquors are run off
through gulleys, ordinarily closed by wooden plugs. The details

of these pans, which are made of jv-inch sheet-lead, are given in
Figs. 126 to 129.
At Chailvet an attempt was made aj continuous evaporation

in thin strata, the pans being arranged on the cascade system,
as shown in Fig. 130.
Fin. 130. Leaden evaporating pans. Continuous system.
The endeavour had, however, to be abandoned, since after

several hours' working there suddenly deposited as the result of
overheating a heavy white sediment, which increased very

rapidly, and set like plaster when removed from the pan. This
proved to be none other than dehydrated ferrous sulphate
salt
(FeSO 4 4H 2 O), which, as we have seen, can be readily formed

,
in the laboratory on subjecting a slightly acid, concentrated

solution of ferrous sulphate to continued boiling.
As soon as the liquor is concentrated it is run off into
crystallising pans, holding 30 to 36 cubic metres (6600 to

8000 galls.), where it is left to cool. With three evaporators
measuring 25 square metres (270 square ft.) in superficial area, and
i 20 metres (48 inches) in depth, about the above quantity of
1
concentrated liquor can be delivered in 24 hours. The evapor-

ators are kept in work for a period of 4 to 8 weeks at a time,
afterwhich they require cleaning out and repairing. As a rule
they have to be entirely rebuilt every two years.

D. COST PRICE. This, though very difficult to ascertain
with exactness, under such varying conditions, may be estimated
in an approximate manner as follows :
Receipts.
Ibs. ferrous sulphate at is 277*2 shillings.
527,720
5500 galls, of crude alum liquor 274 '8 ,,
Total . . .
552-00 shillings.
Expenses.
Oxidised mineral
Lixiviation ........ i68'oo shillings.
35 '20 ,,
Wear and tear of plant, tools
Pumping and upkeep of pumps

Coal, 5 tons at 1 4 '45
;
.....
upkeep, oil, supervision ii'2O
12 'So
72-00
,,
,,
,,
Cost of evaporation 32-00 ,,
Sulphuric acid, 16 cwt. at 2-1 is 33-60

Scrap-iron, 16 cwt. at i'5s. 24-00 ,,
General expenses and sundries 118-40 ,,
Handling ferrous sulphate, packing, cartage . .

44-80 ,,
Total . . .
552*00 shillings.
E. CRYSTALLISING, PURIFYING, AND STORING THE FER-

ROUS SULPHATE. The crystallisers receiving the concentrated
liquor are of dressed stone, coated externally with glaze and then
with powdered chalk. They are embedded in the ground, and
are provided with a lining formed, in the upper part, of an oak
frame with cross beams, and, vertically, of wooden uprights.

This arrangement is necessary to strengthen the walls, and, above
all, to support the ferrous sulphate crystals which are deposited

as the liquor cools. In order that the ferrous sulphate may
keep when stored, it is necessary that the crystals should be
deposited from a decidedly acid solution, since if the liquor is
neutral or too feebly acid the crystals will not remain in
merchantable condition, but oxidise and turn yellow owing to

the formation of an incrustation of basic ferric sulphate. When
the liquor is insufficiently acid, crystallisation proceeds in a very
Coupe |
AB
FIGS. 131 and 132. Plan and section of a dressed-stone crystallising vat.
Coupe AB = section along AB.
peculiar manner, the salt, instead of coming down in readily

detachable granules, then crystallising as coherent plates of con-
siderable hardness and very difficult to get out of the pans.
In practice, endeavours are made to keep the liquor in a state
of acidity corresponding to at least 10 grams of free H SO
2 4
per litre.
After a lapse of 20 to 25 days for pans holding about
8000 gallons the liquor will be cooled down sufficiently, and is

then drawn off from the crystals by the aid of primitive wooden
pumps, formed of two pieces, one fitting in the other. The lower
and smaller piece is the suction pipe, whilst the larger, the
a movable wooden
barrel, contains piston, shod with leather to
make a tight joint. The valves are also of leather, and are
weighted with lead ;

their general arrangement is shown in
Figs. 133 and 134. Pumps made of an alloy of lead and
FIGS. 133 and 134. Details of wooden pump.
antimony have also been used, and, though more expensive

in first cost, are
cheaper keep to in repair than the wooden
pumps, which soon get out of order.

The decanted mother liquor is delivered into vats of thin
sheet-lead,acting as refrigerators, and where a considerable
extra amount" of ferrous sulphate is deposited in the form of very
small crystals. At Chailvet the cooling process is completed by
running the liquors, as a thin layer, down a series of inclined
planes, after which they are stored for working up into alum by
the addition of ammonium sulphate.
The crystals are taken out by shifts of four men and trans-
Cou/* CD.
FIG. 135. Longitudinal section (CD) of washing tank (turbine).
ferred to a square receptacle fitted with a false bottom, on which

a layer of brushwood is 135 to 137).
placed These
(Figs.
"
receptacles are called turbines," not because of any resemblance
to the turbines or hydro-extractors used in sugar works, but
probably through the similarity in the results obtained, though
6 (jOuae A.B.
V'.
FlG. 136. Transverse section of turbine.
the real hydro-extractors are better. The crystals are washed

with a saturated solution of ferrous sulphate, and left to drain for
12 hours: in this way they are gradually purged of aluminous
mother liquor, and are soon ready for storage.

This manufacturing process furnishes three commercial

grades of the product :
(1) The ferrous sulphate deposited on the bottom of the

crystallising pans is in the form of very small grains, and is
known as smalls {petit-sel\ or by the letters PS. The weight

per cubic metre (220 galls.) of this grade is about 1050 kilos.
(21 cwt.) when loose, or 1250 kilos. (25 cwt.) when the heaps
have settled.
(2) The crystals deposited on the walls and wooden fittings

are larger, purer, and of a better colour. This grade is known as
PI*
\C
FIG. 137. Plan of turbine.
" "
ordinary copperas (couperose ordinaire}^ or more simply O, and
weighs, loose, 900 kilos. (18 cwt.) the cubic metre, or 1050
kilos. (2 i
cwt.) in the heap.
(3) The very finely divided salt deposited as sediment in the
cooling vats has to be left a very long time to drain, in the

course of which it sets into blocks of a fair degree of hardness.
To get it into merchantable condition it has to be carefully
broken down by stamping on a boarded floor, and the resulting
impure powder is known as crushed copperas (couperose ecrasce).
When drained the weight per cubic metre varies from 1350 to
1650 kilos. (27 to 33 cwt), according to the fineness of division.

All these grades are somewhat impure, containing a small
quantity of insoluble matter, calcium sulphate, ferric sulphate, a

little free acid, water, and, above all, aluminium sulphate, carried
down by the mother liquor disseminated among the crystals.
The PS grade contains an average of 86 to 88 per cent, of FeSO 4) 7H 2 O.

,, O ,, ,, 88 to 90 ,, ,,
, ,
crushed , , only about 82 to 85 , , , ,
Ferrous sulphate is placed on the market in bulk, bagged, or

(more rarely) packed in casks.
1>L L_J2L__ Jv| |xl tvl r*1
.9
Si/3.
FIG. 139. Longitudinal section along AB.

Re-crystallising vat.
F. RE-CRYSTALLISED FERROUS SULPHATE AND PSR.

Alum makers sell a purer grade of ferrous sulphate, containing
at least 96 per cent, of the pure salt, and mainly used in dyeing.
When in large crystals, this grade is termed re-crystallised copperas
(cuperose refonte) ; and, when in crystals the size of Indian corn, is
known as PSR (petit sel refonte), or re-crystallised smalls. These

latter are obtained by re-
crystallising the smalls in

a leaden vat (Figs. 138
to 140) about the same
size as the crystallisers,
fitted with a spigot for
running off the liquor, and

heated by a jet of steam.
The vat is first charged,
about \ full, with clear
water, or, better still, with
a saturated solution of
ferrous sulphate. Steam
FIG. 140. Re-crystallising vat.
is turned on, and when
Cross section along CD.
the liquid is hot the crude
crystals are shovelled in, the 42 to 44 Be. solution thus obtained
being run into a crystalliser. In order to obtain good results

and prevent loss, certain precautions are necessary, namely :
Although, at the outset, solution may be effected at boiling

heat, the temperature must be lowered in proportion as the
concentration increases ;
and the
injection of steam must be regulated

so as to produce a temperature of
90 to 92 C. at the close of the
operation. In the absence of this
precaution the solution will be turbid

as a result of the precipitation of
dehydrated ferrous sulphate. Again,

an interval of repose, from I to I \
FlG "
Hi.-Re-crystallising vats, show-
hours, Should be left between the rods
ing the arrangement of the
Completion of solution and the destined to serve as nuclei for the
transfer of the liquor, in order to crystallisation,
allow the heaviest impurities time to settle down. To obtain a
maximum of large crystals, the crystalliser is provided with a

large number of wooden rods, connected by bars, on which the
crystals form (see Fig. 141). The mass is left for 40 to 60

days, and, after the mother liquor has been run off, the salt is
broken out, washed, and screened to separate the large PSR

crystals. These grades are mainly packed in casks.
The residual mother liquor has a density of about 32 to
34 Be., and is fully saturated with ferrous sulphate, containing
also a notable quantity of aluminium sulphate, a little alum anc
free sulphuric acid, and traces of organic matter. In connection
FIGS. 142, 143, 144, and 145.
a, Mould collected on distillery waste ; b, mould formed on re-crystallisation liquor
c, laboratory culture obtained by inoculating b on same liquor with addition o
sugar ; d, preparation obtained by sowing /' on gelatinised Ineat broth.
with this liquor a curious circumstance occurring within the

author's experience may be mentioned here, namely, that when
the re-crystallisation liquor has been left in the vats for some
time, during the hot season, itbecomes covered with a large
number of small white spots, which gradually increase in size
and turn grey, becoming of a greenish
finally tinge, and covering
the entire surface of the liquid with a scum \ to | of an inch
thick. On examining
a portion of this film under the microscope,
it was found to consist of closely interlaced mycelial filaments
floating in a liquid containing numerous small oval corpuscles

resembling spores.
When re-examined after staining with Kiihne's blue and
being mounted in balsam, a number of sporiferous filaments,

more or less branched, could be detected issuing from the my-
celium, each branch carrying a cluster of sterigmata surmounted
by chaplets of spores.
These peculiarities correspond to those of the most widely
distributed mould known, namely penicillium glancum. Labor-
atory cultures of this mould were easily obtained on meat broth,
wherein it developed in 3 or 4
days. In re-crystallisation liquor,
with or without an addition of sugar, growth was more protracted,
requiring 15 to 20 days, and the resulting vegetation was in-
variably less vigorous and luxuriant than that obtained on meat

broth. Attempts made to cultivate on the ferrous sulphate liquors
the spores from a penicillium developing spontaneously on dis-
tillery waste resulted in failure, and it therefore seems as though

the organism requires acclimatising before it will grow in a medium
so rich in saline matter as the re-crystallisation liquor in question.
The same mould has also been encountered on media of very
different composition, water saturated with alum, fresh water
rich in ferric sulphate, crude alum liquor ;
but on none of them
in as vigorous condition as on re-crystallisation liquor. However
this may be, the author regards the circumstance as too curious
to be passed over in silence.
109. Alum Manufacture. A. FROM THE RESIDUAL LIQUOR

FROM THE FERROUS SULPHATE PROCESS (brevetage *). The
waste mother liquor from the crystallisation of ferrous sulphate
(termed in French, eau a breveter) is employed as raw material
in the manufacture of alum. As a general thing it has a density
of about 36 Be., and contains aluminium sulphate, ferrous sulphate,
a little ferric sulphate, and free acid, in the proportions indicated
in the subjoined table, as well as a minute quantity of alum.
The preparation of alum from this liquor can be effected with
*
The origin of this term, which is currently used in French alum works, seems to be
The process itself consists in treating waste ferrous sulphate liquor with
lost in
obscurity.
ammonium sulphate.
the aid of various salts, such as potassium chloride, potassium

sulphate, or ammonium sulphate. When, as at the present time,
the price permits, this last-named salt may be advantageously

used, being easier and more satisfactory to work with than
potassium sulphate. Potassium chloride furnishes very poor
results in point of yield, and, moreover, the mother liquors,
charged with hydrochloric acid,, have to be thrown away.
The quantity of ammonium sulphate required in each case is

determined by a laboratory experiment, conducted in the follow-
ing manner :
Fifty c.c. of the crude liquor are treated with 40 c.c. of pure
water and 2 to 3 c.c. of sulphuric acid, followed by 7 grms. of
ammonium sulphate, the whole being heated until complete
solution is effected, and then allowed to crystallise. On the
following day the mother liquor is decanted, the alum is washed

with a saturated solution of alum, and is then dried and weighed.
More frequently the reduction test (essai verdi) is performed.
This consists in treating 50 c.c. of the crude liquor with 40 c.c. of
water and 3 c.c. of sulphuric acid, dropping in a few nails, and
applying gentle heat, the evaporation of the liquid being pre-

vented by covering the vessel with a sheet of glass. The nails
are rapidly attacked, and as soon as the whole of the ferric
sulphate has been reduced the excess of iron is removed and the
liquid is treated with 7 grms. of ammonium sulphate, the remain-
ing procedure being the same as in the first test. This method
always gives results 0*5 togrm. of alum lower than the other.
i
The amount of ammonium sulphate to be added in practice

is deduced, by the aid of a special table, from the weight of alum

obtained in the tests. Another, though less exact, method is by
the cold precipitation in a graduated tube of a known volume
of the crude liquor by a constant quantity of a saturated solution
of ammonium sulphate, the precipitate being left to collect for
some time, after which its volume is read off on the scale.
The table referred to is given below :
In practice, if the liquors are rich enough, the indications on

Table I. are taken. These figures relate to ammonium sulphate,
and vary in the case of other crystallising reagents, as does also
the theoretical yield obtainable. Thus
looparts by weightof KC1 should theoretically furnish 636 parts
of alum from the decomposition of I 86*4 parts of ferrous sulphate,
or the saturation of a corresponding quantity of sulphuric acid ;
100 parts of K,SO 4 should produce 544 parts of alum ;
100 parts of (NH 4 SO 4 ought to yield 686 parts of alum.

).2
The practical yield is, however, different. Thus, in using

amounts of KC1 and K SO 2 4 corresponding to 670 parts of alum,

the quantities actually obtained were 451 with the chloride and
482 with the sulphate. The total alumina being represented by

56*6, the percentage recovered would be 86 per cent, in the
former case and 92 per cent, in the latter.
In treating liquor with 5 i per cent, of alumina the yield is as
follows :
Per 100 parts of pure potassium sulphate, 544 parts of alum
(theoretical yield).
Per 100 parts of pure potassium chloride, 597 parts of alum.
In dealing with 54 per cent, in the same liquor, the yield of
alum was 650 parts in the case of pure ammonium sulphate.
With potassium chloride 91 per cent, pure, the yield was
In recovering the 86 per cent, of the alumina, 496 parts alum.

97 ,, 465
,, whole ,, ,, 458 ,,
Since, as we working with potassium

shall see further on, in
chloride, the whole of the alumina has to be dealt with, it is easy

from these data to compile a table of the weights of chloride to
be added to the liquors, on the basis of the results obtained in
the small scale experiments.

A similar table may, with equal ease, be drawn up for
potassium sulphate, the following figures being taken as a

basis :
With 70 grms. of K,SO 4 , 380 grms. of alum were obtained.

,, 80 ,, 428
,, 100 ,, 510 ,, ,,
In the first case the 53 per cent, of the total alumina was
dealt with, and the yield from the potassium sulphate was
543 parts (kilos.). In the second, the 60 per cent, of alumina
was in question, and the yield amounted to 535 parts of alum;
whilst finally, in the third case, the 7 1
per cent, of alumina was
treated, but the yield was only 5 I o parts of alum.
For the alum recovery process the liquors are delivered into a
dressed-stone tank, heated by steam passed through a number of
leaden cylinders in the bottom of the tank, the general arrange-
ment being that shown in Figs. 146, 147, 148. When the
temperature of the liquid reaches 80 to 90 C. it is run off

into crystallisers,' ammonium sulphate being shovelled in during
the operation. Solution proceeds rapidly under the influence
of the heat, the baffles interposed for that purpose, and the use
FIG. 146. Plan of alum recovery tank.
.
;-iu ,
- .,, ,
' ' ' ' '* ' '

'' "*'' " ''' ' '
''
FIG. 147. Longitudinal section (CD) of alum recovery tank.
of suitable stirring paddles by the workmen ; and, in proportion

as the liquor cools, the alum crystallises out. Ammonium
sulphate by far the easiest reagent to use, since it is very
is
soluble, the alum crystallises readily, the quantity of sub-salts

formed is small, etc.; consequently this precipitant has much to
recommend it.
On the other hand, potassium sulphate is more troublesome,

owing to the formation of sub-salts, and consequent loss, during
the precipitation and purification of the alum. Moreover, the

relative insolubility of the precipitant causes difficulties, and it
often happens that a portion remains undissolved and comes

down with the alum, thus constituting another source of loss.
The best plan, when potassium sulphate is used, is to dissolve

it beforehand and add the solution to the crude liquor.
As for potassium chloride, this salt has little to recommend
it, the loss in manufacture reaching as much as 25 per cent.
Nevertheless, there are times when the use of this salt may prove
Cutuje AiU
FIG. 148. Alum recovery tank. Cross section along AB.
economical, namely, when it can be had at a low price and

ammonium sulphate is at prohibitive rates.
The mother liquor from the alum crystallisation is
residual
useless and has to be thrown away, the ferrous sulphate having
been converted into chloride. Hence, to diminish the loss of

alum, the liquor should be previously concentrated, so that its
volume is reduced by one-tenth.

In order to obtain at one stroke the maximum yield of alum,
the reverse of the procedure potassium or ammonium
with
sulphate is pursued, and the whole of the alumina in solution is

dealt with.
It is easy to account for the advantage accruing from this
method of working, the mother liquors being regarded as so much

loss.
Take the following series of tests with 50 c.c. of crude liquor
containing 80 grms. of alumina per litre :
Suppose the price of the cubic metre (220 galls.) of crude

liquor to be 16 frs. (i2'8s.) and the cost of KCl 11 frs. (8'8s.)
per cwt, the cost of the alum will work out as follows,
allowance being made for the working expenses :
The method of treating the whole of the alumina, though

irrational when potassium or ammonium sulphate is used, is
therefore justifiable in the case of potassium chloride.

B. YIELD. The insolubility of alum in its own mother
liquor is merely comparative, and varies considerably according
to circumstances. Of course it is a prime essential, in fact a sine
qua non y
for obtaining a good yield, and conversely a minimum
loss .of ammonium
sulphate, that the liquors treated should be
concentrated and as highly charged with aluminium sulphate as
possible. An equally important factor is acidity, and it is neces-
sary that the liquor should contain at least 10 to 15 grms. of

free H SO
2 4 per litre, the yield being deplorably poor when
neutral liquors are treated.
The author tried the effect of neutralising a quantity of crude
liquor with lime. After filtration, four samples, of 50 c.c. each,

were taken, one of them being then diluted with 40 c.c. of pure
water, whilst the others were mixed with 40 c.c. of acidified water
so as to obtain a free acidity corresponding to 5, 10, and

20 grms. respectively of H SO
2 4 per litre. On being after-
wards treated with 3 grms. of ammonium sulphate, representing
20*25 grms. of alum, the four samples gave the results set out in
the following table :
As we have seen, care is taken not to add sufficient ammonium

sulphate to convert the whole aluminium sulphate in
of the
the liquor into alum, an amount of free aluminium sulphate
equivalent to 200 to 250 kilos. (4 to 5 cwt.) of alum per cubic
metre (220 galls.) of liquor being always left.
Actually, the solubility of the alum in its mother liquor

decreases with the richness of the liquor in free aluminium
sulphate, as the following table will show :
The presence of a small quantity of ferric sulphate is not

injurious :
if, however, the amount increases, and attains, for
example, 30 to 40 grms. per litre, iron alum is formed, which
contaminates, the ammonium alum and entails a loss of
ammonium sulphate.
Hydrochloric acid is injurious, its presence immediately
reducing the yield to a considerable extent.
Two were made, one with 50 c.c. of pure water, the

tests
other with 50 c.c. of water containing 33 grms. of HC1 per litre,

each being employed to dissolve 20 grms. of pure dry alum, and
then left at rest for 1 2 hours at a temperature of 6 C. The
following results were obtained :
The same applies to chlorides, an experiment made, under

the same conditionsas the preceding ones, with 50 c.c. of water
and 20 grms. of alum, but with an addition of 10 grms. of NaCl,
having given only I S'77 g rms i> e a ss of 8*46 of alum per
-> - l
i oo of water.
This influence of hydrochloric acid explains the poor results
obtained in the manufacture of alum by the aid of chlorides.
Thus, if 50 c.c. of alum liquor be treated with equivalent quantities

of ammonium sulphate and ammonium chloride, the following
results are obtained :
In the same manner with potassium chloride :
The alum recovery process is therefore a delicate operation,

and requires care in its performance.
C. COST PRICE. The remarks made in connection with the
ferrous sulphate process are also applicable here. Nevertheless,
the cost of the alum recovery process may be approximately

determined as follows :
Receipts.
Alum in crude liquor .
7425 kilos.
Loss * .
825 ,,
Alum recovered . 6600 kilos. = 13 "2 cwt. at 3'i76s. = 419-20 sh.

15 cub. m. (3300 galls.) of liquor returned for evaporation 120 oo
-
,,
Total 539'2osh.
Expenses.
25 cub. m. (5500 galls.) of crude liquor
Ammonium sulphate, 22 cwt. at IDS.
Coal, I ton at I4'4s
Labour, pumping, maceration of alum, etc. .
Total 53 9 -20sh.
1 10. Purifying the Alum. A. TREATMENT OF THE CRUDE

ALUM. Production of Ordinary Alum. When the liquor in
the crystallisers has cooled down sufficiently, i.e. at the end
of 15 to 20 days, the mother liquor is drawn off and run
through a series of baffles, in order that it may finish cooling

and deposit the little alum it still contains ;
it is then returned
to the evaporators. This mother liquor has a density of about
32 Be., and, in addition to a little alum, contains ferrous
sulphate, aluminium sulphate, and a small quantity of ferric

sulphate, the composition being shown in the following table :
The crude alum, deposited as brownish crystals on the walls

of the crystallisers, is chipped out and wheeled off to a special
tank fitted with a wooden false bottom (see Fig. 149).
*
On comparing the recovered weight of alum with the theoretical yield of the liquor,
seen that a discrepancy exists, and that the loss is considerable.
it is This loss is due to
the solubility of the alum, part of which is retained by the crude liquor and part
removed by the mother liquor in the course of washing. The amount of loss varies, of
course, according as the work is well or ill done, and also according to the number of
re-crystallisations to which the alum is subjected. Thus, where half the product is to
consist of purified alum, and the remainder of ordinary alum (alun de glace], the loss
under favourable conditions fluctuates between 9 and 12 percent, of alum, referred to the
ammonium sulphate employed. In the above calculation the loss is taken as 1 1 per cent.
Here it is washed three times in succession with saturated

solutions of alum, the cleanest being used last, and is left to
drain after each washing. The solution employed for washing
FIG. 149. Washing and draining tank for alum.
is obtained from the re-crystallising process, and contains 80 to
90 kilos. (175 to 200 Ibs.) of alum per cubic metre (220 galls.),
together with a little ferrous sulphate. When it has been used

several times and becomes too impure to serve longer it is
returned to the lixiviation tanks, where it is mixed with weak
liquor.*
The washing process eliminates most of the mother liquor

adhering to the crystals, and the small amount of ferrous sulphate
* concentrated for the recovery, by crystallisation, of part of the

Sometimes it is
contained alum. Owing to the large consumption of coal involved, this plan has little in
its favour, though occasionally it

may be resorted to with advantage.
which has crystallised with the alum. It may be useful to
approximately determine the weight of pure alum corresponding
FIG. 150. Alum re-crystallising plant.
C, Vat ; A, steam pipe ; D, wooden platform ; B, trough delivering the alum

solution to the block moulds.
to a given quantity of alum washed and drained in this way.

This weight is, of course, variable, but within such narrow limits
that its empirical determination is not difficult. The preceding
FIG. 151. Plan of vat C.
figures are obtained from tests made with moist alum simply
drained.
It may therefore be considered that i oo parts by weight of I
moist alum, simply drained, correspond, on the average, to Si
parts of dry alum.

This alum, however, is not yet pure enough for sale as it
is, and, moreover, is not in a merqhantable form. It therefore
FIG. 152. Copper syphon.
must be re-crystallised a second time, and for this purpose is
re-dissolved by the aid of direct steam, in special vats, generally
FIG. 153. Copper vat with underneath fire.
of lead, slightly wider at the top than the bottom, and fitted with
a false bottom of pumice or thick sheet-lead.
The steam pipes extend nearly to the bottom of the vat,

and are bent upward at their lower extremity (Figs, 50,
slightly i
151). The solution is drawn off through a copper syphon, shown

in Fig. i
5 2.
Formerly copper vats, heated by a fire underneath, were used,

the steam jets being also employed (see Fig. 153), a plan which
enabled more highly concentrated solutions (43 to 44 Be.) to be
obtained.
PU
FIG. 154. Large alum tank. Plan.
The capacity of the vats is such as to nearly correspond to a

block of alum, i.e. about 440 to 550 gallons.
Sometimes the vats are replaced by large tanks of thin sheet-
lead, strengthened with wood, and of sufficient dimensions to
contain as much as eight blocks 16 to 20 tons- of alum. In
such event, the alum, instead of being thrown direct into the vat
itself, as is the usual practice the steam jets producing sufficient
agitation is placed in a kind of hopper discharging into a
perforated cylinder, in the interior of which a steam pipe sets up

an energetic agitation. This appliance is
generally mounted in
one corner of the tank (see Figs, i
54, i
5 4 A, 155).
The modus operandi in any case is as follows Enough :
alum is thrown in to cover the mouths of the steam pipes.
FIG. I54A. Large alum tank. Section along AB.
Steam is then turned on, and more alum is added in proportion

as solution progresses. When the vat is full, steam is shut off
and the mass is left at rest for about an hour, so as to allow the
FIG. 155. Apparatus for introducing the FIG. 156. Block mould for alum.
alum. Section EF.
insoluble matter to settle down. The density of the solution is
40 to 41 Be. in the case of leaden vats heated solely by steam,

and 43 to 44 Be. in copper pans with steam and fire heat.
16
When the liquor is sufficiently clear it is drawn off through a

copper syphon and delivered to the block moulds. The large
leaden tanks are emptied by means of an outlet pipe, about 8
inches from the bottom, and usually closed by a wooden plug.
The block moulds, which vary in size at different works
from 440 to 550 gallons, are in the shape of a truncated cone
(Fig. 1 5 6), and are formed of two or three sections, made of
oak staves joined together with iron hoops and lined with thin
sheet - lead. The joints are tightened by fastening the hoops
FIG. 157. Block of alum cut open to show the interior.
together by means of bolts and nuts and rubber plates. Around

the baser of the mould a luting of clay makes a tight joint with
the boarded floor of the room.
The mould thus prepared and filled with the alum solution is
left to cool. The alum rapidly crystallises on the sides and

bottom, and at the end of about a week the mould can be
taken apart, exposing the block of alum (Fig. 157), which is left
several days longer, 15 20 days being required to effect

to
thorough cooling. At the end of this period the walls of the

block will be 10 or 12 inches thick, the central cavity containing
90 to 100 gallons of mother liquor in a 2-ton block. This

mother liquor measures 5 to 6 Be., is drawn off by boring a

hole in the block, and is sent into storage tanks, from which it
is afterwards withdrawn for washing the crude alum. When too
impure used in the lixiviation process or returned to the

it is
evaporators, being preferably concentrated separately, and not

mixed with the fresher liquors.
The block alum is cut into large lumps with the axe, and these
in turn are broken down to about the size of a man's fist, the
product then constituting the ordinary alum of commerce. Only

the portion from round the sides of the mould can be regarded
as merchantable alum ; together with that part of the base which
is of a greyish colour, owing to the presence of impurities, and
which, under the name of " grey alum," meets with a ready sale
to curriers and the best of the broken smalls, which are passed
;
" "
through a mill and sold as crushed alum the rest, consisting ;
of the foot of block, which is laden with clayey impurities, and

of the dirty fragments, having to be purified to fit it for sale.
The block of alum obtained from 2200 parts by weight of
crude alum furnishes, on the average
Ordinary lump alum
Crushed alum
....... .
1000
260
parts.
,,
"\Yaste for re-purification ( AE) 600 ,,
Grey alum 300 ,,
Alum left in mother liquor . . . . . .

40 ,,
2200 parts.
The smalls can be crushed by hand with a heavy pounder on

a block of stone, or passed through a crushing mill consisting of a
core of fluted steel turning inside a fluted crown (see Fig. i
5 8).
Alum is also sold in the form of fine powder, ground in
special, mills.
B. MANUFACTURE OF PURIFIED ALUM. For certain
branches of the dyeing industry a purified alum almost exempt

from iron is required one, namely, that gives practically no blue
coloration with prussiate. Such a product may be obtained
by re-crystallising the ordinary alum in the same manner as in
preparing that quality from crude alum. It is also prepared from
block alum smalls, this dirty, greyish, and sometimes muddy
waste being re-dissolved by steam in a large leaden vat similar to
those already described as being used for dissolving crude alum
(8 blocks at a time).
The operation is continued until a 28 to 30 Be. liquor is
obtained, this being then covered up to prevent loss of heat, and
left until the next day. The clear liquor is run into a crystalliser,
whilst the turbid residue, which still contains a notable quantity of
FIG. 158. Alum mill.
alum chiefly as sub-salts is extracted by one or two washings
with hot water and thrown away. When potassium sulphate has
been used to form the alum, the loss in the form of insoluble sub-
salts thrown away with the turbid residue is much greater, but
may be diminished by a treatment with sulphuric acid.

The liquor is decanted and the alum drained, after which it is
re-crystallised into blocks of semi-purified (J AE) alum, in the

manner already described. These blocks are broken into masses

the size of a man's head, and, when re-crystallised in copper vats,
furnish blocks of purified alum (AE), which are broken into nuts,
any dirty pieces being set aside and the remainder washed to
complete the purification. With this object, the
alum, prepared
in the manner just described, spread out, as uniformly as
is
possible, in boxes fitted with false bottoms. It is then covered
with a very pure solution of alum and left for 1 2 hours, after
which the liquid is drained off into a receptacle underneath, and
the alum re-washed with pure water.
It is next taken out of the boxes, spread out to dry on slop-
ing tables freely exposed to the
air, or in shallow wicker sieves
(Fig. 159), and is then ready for

sale.
As will be evident, the pro- FIG. 159. Wicker sieve for drying
duction of purified alum is a very purified alum.
expensive process, the cost being considerably augmented by the

great amount of labour entailed in the successive re-crystallisa-
tions, and by the loss of material ensuing from these operations.
C. COST OF PRODUCTION. The following tables show the
mode of estimating the cost -of each set of operations comprised
in the purification of alum :
(i) Ordinary Block Alum.

Receipts.
Lump, crushed, and grey alum :
Lump and crushed alum .

25 '2 cwt. at 4-089 sh. = 103 '04 sh.
Grey alum . . . 6'o ,, ,,

= 2 4'55
Residue for re-crystallisation I2'O ,, 2*635
Total .
43-2 cwt. . . .
=159-20 sh.
Crude alum, 44 cwt.

Alum left in
at 3'i8i sh.
Expenses.
solution, o'8 cwt. (reckoned with the loss

.... = 140x10 sh.
in recovery)
Coal, 2-0 cwt. at 072 sh = 1-44

Wear and repair of pans, etc. . . . . .
i"j6
=
Labour in
Wear and
re-crystallising
repair of
Cartage, packages, labour, etc
moulds ...... =
=
2 'oo
2'oo
I2'oo
Total . . . = 159*20 sh.

(2) Re-crystallising for \ AE Grade.

Receipts.
Alum obtained, 88 cwt. at 3-882 sh =34i'6osh.
Total . . .
=34i'6osh.
Expenses.
Smalls for re-crystallising 12 cwt. at 2-636 sh.
Alum water, 1 760 galls
Coal, 14 cwt. at 0-72 sh
Loss of alum (reckoned with recovery)
Labour, upkeep, etc
Total
(3) Block Alum, \ AE Grade.

Receipts.
Alum to re-crystallise as AE, 30*0 cwt. at 3-883 sh. = 116-48 sh.
,, 4 AE, 13-2 3-540 ,,

= 4672 ,,
Total . .
43-2 cwt. = 163-20 sh.
Expenses.
Alum for \ AE, 32 cwt. at 3-883 sh. . = 124-16 sh.
Smalls . .12 ,, 2-636 ,,

= 3 '64 >.
Coal . . 2 ,, 0-72 ,, .
:
i'44 .
Labour, upkeep, etc = 5-96
Total = 163-20 sh.
(4) Block Purified Alum.

Receipts.
21 cwt. purified alum . . at 5-742 sh. .
= 120-56 sh.
1 6 ,, alum for re-crystallising ,, 4*035 ,,
= 64-56
4-2 ,, ,, ,, to ^ AE ,, 3-586 ,,
= 14-88
41 '2 cwt. alum Total = 200-00 sh.
Expenses.
Ordinary alum, 16-54 cwt. at 4-088 sh. = 67-68 sh.
Alum, \ AE 27-46 ,, 3-88 ,,

= 106-48 ,,
=
Coal
Labour, upkeep,
Crushing, washing, drying, etc
2
etc. ...... 0-72 ,,
= 6'oo
= 6-40
i
'44
,,
,,
Cartage, packages, etc = 12-00

Total = 2OO'OOsh.
D. GENERAL MANUFACTURING ACCOUNT. It is difficult to
draw up statements showing the cost of any one operation in

more than an approximate manner, though the general account
given below will furnish an exact idea of the total results of
working the alum recovery process, based on an output of 1500

tons per annum. Of course the balance will vary one way or the
other, according to the deviation from this figure, since some

of the factors, such as general expenses, horse-keep, etc., being
within a certain limit invariable for the whole year, will have to
be apportioned to a larger or smaller quantity of material treated.
Manufacturing Account, per cubic metre (3 5 '3 cubic feet} of

Mineral treated.
Expenses.
Horse-keep
Upkeep
......
Mineral (extraction, sundry expenses)
of plant
I '600 sh
0-360
0-800
Ammonium
......
Timber, cooperage,
Labour
sulphate
etc.
. . . .
0-304
3-040
3-600
Sulphuric acid .
0-560
Scrap-iron 0-320
Coal I -600
Bags 0-336
General expenses . I -880
Total . 14-400 sh.
Receipts.
Ferrous sulphate .
4-2 cwt. at 1-105 sh -
4-64 sh.
Alum, ordinary and purified, 2 "2 ,, "36 ,,
Total . i6'oosh.
Balance.
Receipts i6x> sh.
Expenses i4'4 ,,
i-6sh.
iii. Construction and Upkeep of Plant. The treatment

of lignites, as also the bauxite, alunite, and many other chemical
industries, entails the use of numerous leaden vessels and appli-

ances, which need frequent repair. In works dealing with the
treatment of lignites a lead worker's shop is an indispensable
part of the establishment. Here are moulded the large sheets of
lead required for constructing the various pans, the necessary
soldering is performed, and other repairs executed.
The production of leaden plates of a certain thickness is com-
paratively easy. The plant is simple, consisting of a cast-iron
melting pot fitted with pouring spout (see Figs. 160 and 161)
closed by a stopper and of a shallow bed, or table with raised
edges, to contain the layer of sand on to which the molten metal

is poured. The method of working is as follows The old metal :
to be re-cast is melted down in the iron pot, the casting bed being
meanwhile prepared by spreading over the table a uniform layer
FIG. 1 60. Cast-iron pot for melting lead.
of wet sand, which is pressed down to a suitable degree, smoothed

by means of copper trowels, and allowed to dry slightly. When
the lead has been melted down, the pouring spout is opened
the stopper has been kept cool by a stream of water so as to
form a leaden plug in the mouth
and the molten mass is poured into
a sheet - iron pot, fitted to the
casting bed, and capable of being

tilted up at one end by means of
suitable levers.
The lead to be cast must be
neither too hot nor too cold, and it is
in this second pot that the metal is
left to attain the right temperature,

FIG. 161. Front view of pouring
which is determined in an empirical
spout.
manner namely, as soon as the
metal begins to solidify round the sides it is considered ready

for casting; whereupon the pot is tilted and the metal flows
over the sandy bed, the raised edges of the table preventing it
escaping at the sides.

The metal is distributed uniformly over the bed by means of

a wooden levelling bar, whose ends slide along the table edges,
and the breadth of which enables the thickness of the cast sheet
A
D
B
FIG. 162. Blowpipe for autogene soldering.
to be regulated according to requirements. All that is then
necessary is to leave the sheet to cool down, and cut it

up as
required.
The joints are soldered by the autogene method invented by
Desbassyns de Richemond, a process which, when performed by
FIG. 163. Leaden hydrogen generator for the autogene soldering process.
good workmen on clean surfaces, furnishes joints more solid,
by reason of their great thickness, than the sheets of lead
themselves.
The work is done by the aid of a blowpipe (Fig. 162)
supplied with air and hydrogen through two caoutchouc pipes
fitted with stopcocks A and B. The gases are mixed in the part
CD, which carries a movable ajutage E; and by means of the
cocks A and B the dimensions of the flame can be controlled
by the workman, and an excess of hydrogen maintained so as to
preserve the reducing character of the flame.
The hydrogen is furnished by a leaden generator (Fig. 163),
the lower chamber of which (A) is charged with scrap-iron
through the capped tubulus B. The upper chamber C, which is
covered with a loose leaden plate M, contains dilute sulphuric
FIG. 164. Bellows.
acid, and communicates with A by means of the pipe D, which

dips into a cup L. The pipe D is provided with a branch E, which
is closed by a plug F while the apparatus is in work. The
hydrogen generated in A escapes through the neck G into a pipe
H, which discharges it through the water in the bottle I, the neck

of which (J) communicates with the blowpipe supply tube. The
bottle is interposed to prevent any flashing back of the gas from
the blowpipe to the generator.
On ceasing to use the blowpipe the workman closes the stop-
cock of the hydrogen pipe, whereupon the pressure of gas in A
increases and forces the acid up through the pipe D, away from
contact with the iron filings, and consequently the evolution of

gas is discontinued automatically.
To empty the generator, the plug F is taken out, the blowpipe
cock being kept turned off.
The air blast required to support the hydrogen flame is
supplied by the bellows shown

in Fig. 164, the lever A being
worked by an assistant seated on
the bellows case. The blast is dis-
charged from the bellows through

the neck B.
Whenever possible the work
should be done on the flat, the
ends of the two sheets to be
joined being lapped over about
if to 2 inches (Figs. 165, 166), FIGS. 165, 166. Soldered lapped butt
the contact surfaces a and b joint in leaden sheets.
scraped clean, and the metal of .
the upper sheet melted by the

blowpipe flame and united with the
under sheet. A simpler method
is tosimply put the two edges
(butts) of the sheets together
(Figs. 167, 1
68) and run the
blowpipe jet along the space

between a and b, so as to melt
the metal and join the two
sheets ;
this joint, however, is not
so strong as the lapped joint. In
both cases it is advisable to hold
in the blowpipe flame a stick of
solder, which fuses and increases
the thickness of the joint.
FlGS l67 l68
-
'
- Butt J oint -
The work of soldering lead sheets is a delicate operation, and
requires skilled labour. If the blowpipe jet be directed too long

on the same spot, the sheet is liable to melt through and form a
hole ; consequently the flame must be shifted the moment the

solder is sufficiently hot to begin to melt and fuse with the

metal of the under sheet. In the case of thin sheets the task
becomes particularly delicate, and great dexterity is required to
ensure success.
Again, the soldering of upright sheets is very difficult. In
FIG. 169. Scraper for brightening the parts to be soldered.
this case use is made of the small wrought-iron tool, shaped like
a gouge, shown in Fig. 172. The work of soldering is begun at
the bottom, and, a stick of solder being laid on the tool, the latter
is held against the edges of the two sheets, the flame being then
directed alternately against the solder and the parts to be joined.
FIGS. 170, 171, and 172. Soldering a vertical joint.
The solder melts, runs down to the lip of the tool and there
solidifies, thus joining the edges of the leaden sheets. The tool
is about -^ or xV of an inch higher up, and the

then raised
same process is repeated until finally a ridge is formed all the
way up uniting the sheets (Figs. 170, 171).
A good workman can solder sheet-lead of about | an inch
thick at the rate of 40 to 60 inches an hour on the flat, or
12 to 1 6 inches of upright work.

In the case of thin sheets, a practised hand can solder at the
FIG. 173. Jointing two horizontal pipes.
rate of 6| to /| yards run on the flat, or 40 to 80 inches of

vertical work in the same time.
The soldering of the convex under side of a horizontal pipe is
an almost impossible task for the blowpipe. Consequently, where
the jointing of two horizontal or slightly inclined pipes (A, B,
FIG. 174. Fitting a leaden pipe to FIG. 175. Fitting a leaden pipe to a vertical
a vertical wall, accessible on the wall, inaccessible from the back,
rear face.
Fig- 173) is in question, they cannot be soldered all round from

the outside ;
and in such event the one pipe (A) is slightly en-
larged at the mouth so as to receive the end of the other pipe
(B). A hole C is then made at the top, through which the

blowpipe is introduced, and the soldering is effected on the inside
of the pipe, which done, the hole C is covered with a leaden plate
readily fastened on by soldering.

If it is desired to fasten a pipe A to a vertical sheet B (Figs.
174, 175), and access to the rear of the latter is possible, a
circular hole, of rather smaller diameter than the. pipe, is cut in
the sheet. The metal round then turned up outwards
the hole is
so as to form a neck large enough to admit the pipe without too

much play. The latter is next fixed in position in such a manner
that the edge rests on the turned-up part at a, and the work of
soldering is begun, the blowpipe attacking the edge of the pipe
in order to form the ridge. This is continued as far as />,
FIG. 176. Bolted loose-flange joint for pipes.
from which point onwards the sheet B is attacked until c is
reached.
When the wall cannot be got at from the back, or when it is
desired to have the soldered joint on the same side as the pipe,
the latter is first fitted with a collar C (Fig. 175). Then, in
addition to the opening necessary for the reception of the pipe, a

slit a b is cut in the wall, and, after the edge of the collar has
been set in this slit, soldering is begun along the straight line a b,
and continued upwards all round the collar.

Occasionally a bolted loose-flange joint is required for pipes.
In this case the two adjacent ends of the pipes are flanged after
the loose flanges have been slipped in position, and, the ends
being put together, the loose flanges are fastened with bolts and
nuts (Fig. 176), which squeeze the lead flanges together and
make a perfectly tight joint.
112. Possible Improvements in the Treatment of Pyritic
Lignites. The method of manufacture already described is
costly, and, although under proper management it is still pro-

fitable, the small margin of profit left is sufficient justification for
the endeavour to find more economical methods of procedure,
apart from all other considerations.
The prospects of success in such endeavour have been con-
sidered by the author, and, in collaboration with A. Vivien of
St. Quentin, he has made a special study of the preparation and
lixiviation of the ore.
A. ENRICHMENT OF THE ORE. When prepared in the
ordinary manner the ore furnishes a poor raw material, expensive

to handle, and varying in yield according to the weather. This
poverty necessitates the accumulation of enormous stocks,
which cannot possibly be protected in a satisfactory manner
from the lixiviating action of rain, considerable losses being
the result.
The high temperature generated during the oxidation
process causes the formation of insoluble sub-salts, and there-
fore a portion of the sulphuric acid produced is left unutilised.
Moreover, the work is slow, costly, unhealthy, and difficult to

control.
An investigation of the sequence of operations during the

oxidation process will readily show that the oxidation develops a
considerable volume of heat. Even after a lapse of three months
the temperature of the large heaps still remains about 1 00 C. ;
and the author has endeavoured to utilise this heat for attacking
the excess clay in the mass, by means of sulphuric acid, without

expense. The fear that the presence of organic matter in the
mineral would lead to a loss of sulphur dioxide, resulting from
the decomposition of part of the sulphuric acid, has been proved
groundless by the result of these experiments.

The first trial was conducted as follows :
A
4 5 -ton heap of the mineral was treated with 52 cwt. of
60 Be. sulphuric acid, which was left to react for about a fort-
heap adjoining being left without acid as a check.
night, a similar
Samples were taken with great care, pulverised, and subjected to

analysis, with the following results :
(i) Lixiviation of 100 grms. with 500 grms. water
(2) Comparative Analysis of Cinder ; results referred to dry

matter
Acidified Check
Cinder. Cinder.
+ 4'20
-I-OS
+ 6-82
+ 574
The quantity of acid used was 4*260 kilos, per cubic metre,
and therefore more was recovered than the amount initially
present.
This first test showed that the attack proceeds fairly rapidly
and without loss ; but, owing to the great difficulty experienced
in sampling, it was felt desirable to repeat under conditions of
greater accuracy. Again, a difficulty having arisen in distributing
the acids to the small heaps in a practical manner, it was thought

advisable to wait until the large-heap stage before adding the
acid. In order to ensure identicity of conditions, the work was
performed as follows :
A certain quantity of the oxidised lignites was taken at the
time of making the large heaps, and sifted to render it homo-
geneous. An accurately weighed amount of this sample was then

placed in boxes and treated with a known quantity of sulphuric
acid and, after the addition of a little water, the closed boxes
;
were re-weighed and placed in the heap in course of building, a

note being taken of the weights in each case. When the attack-
was deemed to have sufficiently progressed the boxes were taken
out of the heaps and weighed again, the difference in weight
noted and, the contents having been reduced to powder, the

;
samples for analysis were taken.

A preliminary test carried out on this plan gave the following
results :
j
Temperature on opening the boxes, 90 C.
>
Duration of experiment, 20 days.
I
N.B. No. 2 sample, having been placed in a damp part of the heap, had absorbed
The second trial, performed under identical conditions, came

out as follows :
*
Sludge acid from petroleum refining, containing 850 grms. H SO
2 4 per litre.
The time occupied in this case was ten weeks, and the
temperature of the material at the time of opening the boxes
= 100 C.
From these experiments it follows that the added sulphuric
acid attaches itself mainly to the alumina; that it is completely
utilised ;
and that a larger quantity is recovered than was added
in the first place, a result evidently due to the sub-salts having
been rendered soluble.
*
4-13 per cent. f 4"75 per cent. J 5-34 per cent. |< 4'ii per cent.
would therefore seem advantageous to treat the ore in this

It
fashion the more so because the earliest consequence of the

;
considerable enrichment of the material is to appreciably diminish

the cost of labour, consumption of coal, waste, etc.
B. LIXIVIATION. I. Theory of Systematic Lixiviation. In
studying this stage of the process it is highly necessary to be able

to follow up all the phases by calculation. We will therefore, in
the first place, trace out the

simple connecting the
relations
different quantities such as volume of liquid to be drawn off,
weight of material lixiviated, density of the liquors, etc. coming
into play in the process of lixiviation.
Let us take a battery of apparatus composed of a series of

units, i, 2, 3 in i, 1/1, in which the direction of circulation
. . .
is from i towards m and assume that the liquor stays long

;
enough in each unit for the concentration to be identical through-

out the series.
A constant volume v of liquor is retained by the insoluble
matters.
Then, let
V/ be the volume of liquor to be drawn off;
V ,
the volume of water fed to the battery for each operation,
and consequently the volume of liquor passing from orie unit to
another ;
P, the weight of material placed in the last unit ;
TT, the weight of soluble matter in P ;
TT I , 7r 2 , . . . 7r n , 7r
;i+i ,
the weight of soluble matter per unit of
volume in the intermediate or final liquors ;
i + </!,
i +</2 ,
. . . i +dn ,
i
+d,l+1 ,
the densities of these
liquors.
The liquids and an invariable, though
solids are introduced in
intermittent, manner, and the tendency is towards the establish-

ment of a permanent regime. Let us suppose this to be accom-
plished, and the apparatus in work.
Take three units in series, n i , n, n + i
;
then n + i becomes
n, losing one step, on the addition to the series of a freshly
charged unit forming the final member.

This unit n, previously + i contains the residues and the ,
liquor impregnating same, representing an amount of soluble salts
corresponding to
On the other hand, the

*>x^,
newunit n receives from its immediate
predecessor a volume V of liquor, representing a quantity of
salts equivalent to
Consequently, at a given moment n contains a weight of

soluble salts equal to
In the next turn, however, n becomes n i, n+ i becomes n,

and so on ;
the unit n loses a quantity of soluble salts represented
by the amount of water impregnating the residues, i.e. v X TT W , plus

that contained in the liquor passing into the unit n -\- i ,
i.e. V TT H
O ,
or in all
v x TT W +V x TT
U .
The weight of soluble salts entering this unit is evidently the

same as the amount leaving it, and is equivalent to
Or
If we apply this relation to all the vats or units, and make in
succession n= I, 2, 3, . . .
;//, we shall then have
Unit i TT., TT^

= V, X '
7r x
- 7T, -
V
- - ITj
Unit 2 7T 3 (7T 2
(A)
V
Unit ?// I
On multiplying these equations one upon the other we have
~ ^l) fa -ITt) " fau ~ T^-,) =

'
-(^2 - Wl) '
( l)
and on dividing by
fa - î) fa -
obtain
V.
--,=(;) X 7T,
(0
If we now add together the equations A we obtain
V V
+ fa ~ ^2) + + fa,< ~ ^-J = + (^ -
-
fa î) î
Or
from which can be deduced
(3)
Let us substitute this value of 7r>>l _ 1 in equation (i)

whence _
1=11 X 7T, 7T
V
and hence
(I)"-
*V = y- X.7T, (B)
^ T
From this can be deduced
V
>"( \
= ~(~- + =- '"'
( *)
1
^r (4)
If we apply the primordial formula to the m vat, we have

TT +V O (TT W_ I )
= z> X TT
OT + V, X TT ;/; ,
and, by applying the value already found for TT,,,.,,
-"w
1
= v x TW + V, x TT W
V X 7T...
-"
V. X 7T,
= tr m (v + V,)
TT+
rt
'
- = 7; x TT W + V, X ir m
v
V
-(~ ) + V, X 7T W - V, X 7T,
= ^( V +
V,)^'
V. X 7T ;;/ -V X VT, = (t, X ^+ V,7TW ) ^ - TT^

VTT )n -f V,7r,,; - 7T
(C)
Let us assume that the water throughout the system is con-
stant. The volume entering is V, therefore an equal volume of :
water should leave the series
V, = Z< + ^) - OTT! + V,( + <) - V,7T,,,

I I
V,= t<I + 4-^) + + <,,-7T,,,) ^ I

(D)
To sum up, we obtain three ratios between the values TT, v,
V V
ot t,w ir lt d^ dm and m. These values are for the most part
7r , ,
arbitrary, and dependent on the requirements of the manufacturing
d,n
process: thus -r- = TT,,,
: -iris known; v can be determined by
d l IT,
I + d the density of the final liquor, will vary accord-

experiment ; llt ,
ing to the conditions of manufacture and the result in view irm ;
is known I + d, or TT, is the

;
result of the final washing and P ;
(from whence comes the values TT and i>) is a fixed quantity : so

that there only remain to be determined V,, V/, and in.
O . .
(i)
(2)
(3)
U It i
These three ratios comprise all the factors of systematic

lixiviation, and enable all the problems of this operation to be.
solved.
II. Hot Extraction. The usual method of extraction is
attended with numerous inconveniences in practice, since the
liquors obtained are very dilute and have to be concentrated,

which entails considerable consumption of fuel, much labour,
etc. In consequence of the large area of the apparatus the
extraction is often defective, tedious, and does not properly

exhaust the mineral, especially in winter.
The work is very troublesome, and considerable loss by

infiltration occurs in consequence of the leaks formed in the
masonry.
AXI) SULPHATES OF IRON 263
The author has had the idea of a process of extraction in

closed vessels under pressure, with small charges, and at a
temperature of 100. In fact, the mineral to be treated consists
essentially of an insoluble porous skeleton, containing a mixture

of soluble salts, for whose solution a temperature of 100 is
the best. It is a priori evident that by causing hot liquor to
circulatethrough this mineral a sufficient number of times a hot

saturated solution will be formed, i.e. one that does not require
concentration. If it proves that this result can be obtained with
a smaller expenditure of fuel than the concentration process, the
advantage of the new system will be evident. In the ordinary

method the liquor measures 28 Be. only, and must be concen-
trated by evaporation to 42 Be., ie. by applying the formula
*'-4
V= I OOO ;;
d> i
.
About 420 litres of water must be removed per cubic metre of

liquor. The amount of heat theoretically necessary for this
evaporation taking the specific heat of the liquid as unity
is given by the formula O=P (6o6'5 + 0^305 x / 0), that is
to say, in the present case about 250,000 calories. To these

calories must be added the heat required for raising the residual
volume 00,to 49,000 cal.,

1 i.e.
assuming the
initial temperature to
be 15, or a total quantity of heat represented by 306,000 cals.
By the hot -extraction method the consumption of heat is

represented merely by the number of calories necessary to raise
the temperature of the concentrated liquor from I
5 to 100, i.e.
49,000 cals., volume of

since this liquor will be equal to that
furnished by the evaporation process. That is to say, we have
in round numbers a saving of 250,000 cals. per cubic metre of
28 500 metres of concentrated liquor; i.e.

Be. liquor, or per each
a littlemore than t of the total quantity. The advantage
is therefore more than appreciable. As regards the means of
performing this operation, the first idea that presents itself is
that of an apparatus similar to that of the diffusion batteries used

in sugar works. This apparatus can be pictured as lined with thin
sheet-lead, and somewhat flat in shape, provided with a filtering
surface of asbestos cloth or glass wool, leaden conduits, etc. The

water would be turned on, but, in order to avoid loss of heat in

the spent mineral, only the last members of the series would be
heated, and that, too, after the liquor was already in a state of
cold saturation. In this manner the heat stored up in the spent
mineral would be recovered by the subsequent cold liquid, and
each unit would not be emptied until thoroughly cooled down.
At this moment, i.e. when the cold saturation had been effected,
the residual liquors from the alum process could be introduced,
thus effecting an economy of fresh water. From the trials made
T
FIG. 177. Hot extraction. Diagram of a unit of an extraction battery.
by the author the thickness of the charge should not exceed 20

to 24 inches in each unit, in order to prevent undue resistance to
the passage of the liquor. Perhaps, however, by arranging more
favourable conditions this thickness can be increased, and would
correspond to an increase in the volume of liquid obtained.

The number of units in the battery would be easily calculable
for each particular case by means of the formulae already given,
and would always be small consequently the cost of the installa-
;
tion would not be very high.
The concentrated hot liquors would be caught in a reservoir

fitted with baffles, where the insoluble matters would settle down ;
from those they would pass to the reduction process (which of course
would be effected in the warm), and finally to the crystallisers.
Other improvements are also possible in the treatment of

lignites such, for example, as the filtration of the saturated alum
;
liquors before casting the blocks, which treatment, by removing

the insoluble matters usually present, would increase the quantity
of merchantable alum produced. For this purpose a filter, of the
Philippe type, employed for filtering syrups in sugar works, but

fitted with heating apparatus to prevent a crystallisation of a
concentrated alum solution, might be used.
It is evident that in this case it would no longer be possible
to lute the bottom joint of the mould with clay, but that in order
to ensure proper working this joint would have to be made of
caoutchouc, or some other suitable material.
Another improvement that may be introduced applies to the
manufacture of purified alum direct in crystallising the crude
alum by agitation, in order to secure the deposition of very small
crystals. This mass of crystals, when drawn in the hydro-
extractor, clarified, macerated with alum water, drawn off, and

clarified anew, furnishes an alum which, the author is satisfied,
will give purified alum after a single re-crystallisation.
Concerning the crystallisation process generally, both for
ferrous sulphate and alum, it is evident that the crystallisers set

in the ground are very defective. Wooden crystallisers, lined
inside with thin and raised above the ground, such
sheet-lead,
as those described in dealing with the treatment of alunite, would
be much more practical. In addition to the fact that on de-
molishing the crystallisers the old lead retains its value, and
that consequently an installation of this kind, although costly,
always represents a portion of the capital expenditure, with

this system leaks can be easily detected and repaired, and a
considerable saving of labour is effected. In fact, the mother
liquor can be drained off by a single process of syphoning, which

saves the expense of pumping a serious matter in view of the
enormous volume of liquor. Furthermore, the crystallisers can be
arranged to serve as washers, thus avoiding a double handling of
the salt.
So as not to go beyond our subject, which is chiefly con-

cerned with describing the industries forming the object of the
present work, we will not further enlarge on this point, but will
now pass to the manufacture of ferric sulphate.
3. MANUFACTURE OF ORDINARY FERRIC SULPHATE.
113. Introduction. Until within the last few years ferric
sulphate was generally looked upon as a mere laboratory product,

or, at any rate, was only manufactured in small quantities indus-
trially. Nevertheless, it has long been known that this salt,
already used in dyeing,* was useful for purposes of sanitation,
by reason of its property of combining with organic matters and

preventing their putrefaction. Among the numerous patented
processes for manufacturing ferric sulphate we need only mention
those of Marguerite and Rohart, which are now of merely historic
interest ; and, above all, the elegant and practical method invented
by Buisine, the distinguished professor of science at Lille and the
Institut Industriel du Nord.
i 1
4. The Marguerite Process. This process was devised
for manufacturing ferric sulphate from oxide minerals, pyritic
cinder, etc., which substances, under ordinary conditions, are
difficult to attack with sulphuric acid.

The modus operandi claimed by the inventor consists in]
treating oxide of iron presence of a small
by sulphuric acid, in
quantity of hydrochloric acid, which facilitates the reaction. The.
hydrochloric acid, which acts the more energetically, forms at
first ferric chloride, according to the equation
Fe 2 3 + 6HC1 - Fe 2 Cl 8 + 3H 2
0.
This ferric chloride is produced in presence of an excess of
sulphuric acid, which acts upon it in turn
Fe 2 Cl + 3 H S0 4 *
2
Fe 2 (SO 4 ) 3 + 6HC1.
The small quantity of hydrochloric acid is thus constantly re-
*
Ferric sulphate was employed in dyeing, in consequence of the researches of Raymond,
i.e.early in the nineteenth century. It was first used for blue, and for this purpose was
prepared from ferrous sulphate by moderate calcination.

AND SULPHATES OF IRON 26;
generated, and the cycle of operations continues as long as there

is any ferric oxide and excess of sulphuric acid remaining.
115. The Rohart Process. Although the inventor of this
process, Rohart's principal aim in connection with ferric sulphate
was to investigate its disinfectant properties, and it was only
subsequent to the date of his patent (1882) that the importance
of this application of the salt in
question began to be properly

appreciated.
The Rohart process is based
on the conversion of ferrous sul-
phate into ferric sulphate, under

the influence of nitric acid in
presence of the necessary amount

of sulphuric acid. The apparatus
for this purpose consisted of a
wooden trunco-conical vessel C
(Fig. 178) suspended over a group
of five glass carboys D D, the
necks of which, E E, projected
through the bottom of C.
To obtain ferric sulphate with
this apparatus, 36 Be. nitric acid
was poured into the carboys.
first
Meanwhile a mixture was pre-

pared by heating and stirring
suitable proportions of sulphuric
acid, ferrous sulphate, and water FIG. 178. Manufacture of ferric
sulphate (Rohart process).

in a cast-iron pan ;
this mixture
being poured into the vessel C as soon as it had become homo-
geneous, and without waiting for it to cool. The sediment left
in the pan was afterwards broken up and filled into the flasks
D through the necks F.

The reaction commenced at once, and proceeded unaided.
To decrease the considerable consumption of nitric acid entailed
by the method, the inventor, in his specification, recommends

injections of air into the carboys.
The resulting, ferric sulphate was acid, and had to be neutral-
ised with sodium carbonate or ferric hydrate.

Ordinary Peroxidation Process with Regeneration
1 1 6.
of the Nitrous Products. This process will be described later

on in dealing with the basic ferric sulphate known as Rouil
mordant, in the manufacture of which it is still employed.

1 1
7. The Buisine Process. This method consists in
attacking roasted iron pyrites with sulphuric acid. The very

simple reaction is represented by the equation
3 H,S0 4 + Fe 2 3
= Fe,(S0 4) 3 + 3 H 2 O.
Iron pyrites, the actual raw material employed, furnishes the

two products necessaryin this method of preparing ferric sulphate,
namely, iron peroxide and sulphuric acid, the sulphur dioxide

formed by roasting the pyrites being converted into sulphuric
acid in leaden chambers. The method is therefore specially
adapted for use in large chemical works possessed of the
necessary plant, and producing, on the one hand, roasted pyrites,

and, on the other, 60 Be. sulphuric acid in fact, the reaction ;
goes on most actively with this strength of acid, and at a

temperature of 120 C. that at which the acid leaves the
Glover tower.
The operation is extremely simple. The hot acid is run
direct from the Glover tower into a cast-iron pan, heated from
below, which pan is then charged with roasted pyrites, in powder,
as it leaves the furnace, but cooled and sifted if necessary.
On stirring the mass the reaction commences, and is stimu-

lated and carried to completion by the aid of heat, the tempera-
ture being raised to 250 to 300 C. Steam alone is liberated,
and the iron oxide
almost entirely consumed, the product
is
generally containing not more than 5 per cent, of insoluble

residue. The ferric sulphate forms 75 to 95 per cent, of the
total.
In practice, 45 to 50 parts of roasted pyrites are taken for
every 100 parts of acid, according to the composition desired for

the product, which may be either normal ferric sulphate or ferric
sulphate containing a larger or smaller excess of free sulphuric

acid. This has its advantages, because in certain cases the treat-
ment of waste liquors may require a neutral ferric sulphate or one
of known acidity, according to circumstances. The temperature
of the reaction also affects the composition of the product, as is
shown by the following table compiled by Buisine :
The following analytical values of another ferric sulphate
prepared by the Buisine process were obtained by M. Vivien

of St. Quentin :
Ferric sulphate . 60 -oo

Free sulphuric acid 9H9
Ferric oxide . .
11-40
Ferrous sulphide .
0-56
Sand 2-04
Moisture ....
Volatile matter .
Sundries and undetermined .

1-16
11-64
3-7I
Total 100 'DO
The Buisine sulphate is a greyish dry powder, easy to pack
and transport. It is anhydrous, and in that condition is very

sparingly soluble in water, but after hydration which occurs
gradually in cold, though more rapidly in the warm

the it
becomes exceedingly soluble.

When mixed with i 5 to 20 per cent, of water, ferric sulphate
sets slowly, like gypsum. As we shall see later on, this property
has been utilised for the production of ferric sulphate briquettes, a

very suitable form of this salt for many uses. Briquettes have
also been made containing phenols and other antiseptics for use
in certain special cases (see Part III., USES).

2/O MANUFACTURE OF ALUMINIUM SULPHATE
4. MANUFACTURE OF BASIC FERRIC SULPHATE, OR

*
ROUIL MORDANT
i I 8. Introduction. The preparations known by the name of

Rouil mordant consist mainly of concentrated solutions of a basic
ferric salt, largely used in dyeing, especially for silks. They
form the object of an important industry, mainly located at
Lyons, which at the same time is the principal centre of con-

sumption of the products.
This industry was founded by Raymond, and the first
manufactory was started at Lyons early in the nineteenth
century ;
it was still in existence at about 1830.
In 1876 the daily output of the Lyons factories was 25 to 30
tons of this product. The amount now produced is difficult to
estimate, considerable quantities being made in Rouen, Amiens,
Paris, Lille, Chailvet, etc., as well as at Lyons.
The preparation most used in dyeing is that known as rouil
sulphate. When first Raymond, who was professor of chemistry

at Lyons, proposed to use ferric sulphate for producing blue with
potassium cyanide, the salt employed was prepared by calcining
ferrous sulphate but subsequently, when working on a manu-
;
facturing scale, he modified the process and employed nitric acid
for peroxidising the ferrous sulphate. At first the operation was
conducted, without any attempt at recovering the nitrous pro-

ducts, by mixing nitric acid, sulphuric acid, and ferrous sulphate
together in casks. The resulting product was costly, and neces-
sarily imperfect, and it was only at a later date that the idea
arose of working in vats, and recovering the nitrous products.
A. ROUIL SULPHATE. This preparation is, in the liquid
form, dark reddish brown by reflected light, rusty by transmitted

light, and contains in solution a ferric salt, which should prefer-
ably approximate in composition to the formula (Fe.2 )o(SO 4 )5 .
The liquid shouldmeasure 40 to 46 Be.

At one time two kinds of this sulphate were prepared that
for blacks (Rouil pour noirs) containing an excess of ferrous
sulphate, whilst that for blues (Rouil pour bleus) was completely
*
According to Littre, this word rouil is a corruption of rouille rust.
peroxidised. This distinction has now been abolished, and

endeavours are confined to producing a mordant containing a
minimum of ferrous sulphate.
Other classes of rouil are known, but being of limited em-
ployment need only brief mention here.
/>'. ROUIL NITRATE. Deep red liquor, generally home-made
by the dyer, by gradually adding scrap-iron to nitric acid until an
ochreous deposit of ferric sub-nitrate is formed.

C. ROUIL ACETATE. This is also a dark red-brown liquor of
20 Be. density,, and is prepared by the double decomposition of
ordinary rouil and lead acetate.
D. ROUIL CHLORIDE. A
reddish-yellow liquor. Despite
numerous trials, this has always been abandoned on
variety
account of the difficulty with which it forms insoluble sub-salts on
contact with water, the production of which salts is a characteristic
property of the other rouil preparations, and one inter alia that
justifies their employment in silk dyeing.
E. ROUIL ACETO-NITRATE. This is dark red in colour. It
is prepared in the same manner as rouil nitrate, except that the

addition of scrap-iron is continued until the whole mass sets firm.
The mass of sub-salt is then treated in enamelled cast-iron
pans with hot acetic acid, the sub-salt being kept in excess
throughout.
Except this last one, these different rouils present little of
interest.
119. Rouil Sulphate Manufacture. A. NITRIC ACID

METHOD. This, the process in general use hitherto, consists in
oxidising commercial ferrous sulphate with nitric acid in presence

of a certain proportion of sulphuric acid, and is based on the
following reaction, which represents the production of normal

ferric sulphate
6[FeS0 4) 7H 2 0]+3H 2 S0 4 +2HN0 3
m 3[Fe 2 (S0 4 ) 3 9 H 2 0]+ 2NO+ 9 H 2 0.
,
I
The process appears exceedingly simple, but, as we shall see
later, is in reality difficult, and entails skilled labour.
(i) Plant. This is simple, and comprises a peroxidation vat,

a recuperator for the nitrous products, and storage vats for the rouil.
The peroxidiser is of lead or cast-iron, the former being
preferable on the score of economy, since it is more durable,

easily repaired by the hydrogen blowpipe ;
and when the vats are
pulled down the old metal is worth a good deal of its original
price. The vat is fitted at the bottom with a discharge pipe
which is closed by a wooden plug. The lead used is to i inch 'i
thick. Towards the upper edge the vat widens out suddenly, so
as to be able to cope with the effervescence produced in the mass
by the violence of the reaction.
FIG. 179. Rouil mordant process, Peroxidation vat.
On this widened part rests a wooden cone, surmounted by a

pipe for the escape of the gases, and also pierced by three open-
ings one, generally closed, for inserting a stirring rod ;
the
second and smaller one admitting the steam pipe, which terminates
below in a coil whilst the third and largest opening is traversed
;
by an earthenware pipe extending to within 4 to 6 inches of the

bottom of the vat. Into the mouth of this pipe fits a leaden
funnel for introducing the charge. All the joints are luted with
brick earth.
The gas-escape pipe leads to a series of condensers for the
removal of moisture, the gas then passing into a battery of

divided carboys and thence through a set of three coke scrubbers
into a chimney shaft of good draught. The joints are luted
with a mixture of -J
Portland cement and f brick earth
with sufficient melted pitch to make a plastic paste. The
mixture must be used whilst fresh, as it will not keep.
The installation is completed by a series of lead-lined wooden
reservoirs placed over against the peroxidising vat, and destined
to store the liquid product.
(2) Manufacturing Process, The vat shown in Fig. 179

furnishes about i 2 cwt. of merchantable product at each charge.
It is charged with about 4|- gallons of water, or saturated solution
of iron sulphate, followed by 2\ gallons of 60 Be. sulphuric acid
and 3-j- gallons of 36 Be. nitric acid. Steam is then turned on,
and, when the contents are hot, commercial ferrous sulphate, in
the state of small crystals, is shovelled in, a little at a time.
Each shovelful produces strong effervescence owing to the
abundant liberation of nitrogen dioxide, a small portion of which
escapes as red fumes through the charging pipe, and enables the
progress of the reaction to be followed. When the reaction
slackens, 9 to i 2 gallons of weak (20 to 22 Be.) nitric acid from

the recuperation plant are run in, followed by a further addition
of ferrous sulphate. When the red fumes cease to escape
through the charging pipe, and no particular effervescence can be
heard on the addition of more ferrous sulphate, the peroxidation
is complete. Steam is then turned on full, so as to superheat the
mass and cause the rouil to assume its characteristic colour, after
which the liquid is run off into the storage reservoirs.
At the end of several days the liquor deposits an abundant
sediment of insoluble sub-salts, which constitute a considerable
amount of waste.
Fire heat may be used instead of steam, but is not to be
recommended. In this case the vat is first charged with about
30 gallons of water instead of 4^ gallons. As the final weight
of product is unchanged, 242 Ibs. of steam, corresponding to
35 1 Ibs. of coal, are consumed in the steam -heating process, i.e.
the cost per ton of product taking the coal at 203. per ton at
18
the works is under sevenpence. With fire heat about 80 Ibs. of
coal are required, which works out at the rate of is. 2d. per ton
of product, the saving by using steam heat being therefore
8d. per ton to say nothing of the reduction in the quantity of

;
waste sub-saltsproduced in the final

superheating stage, the
greater ease in working and controlling the operation, and the

diminished wear and tear of the vat.
the Nitrous Products. Throughout the
(3) Recuperating
operation large volumes of nitric oxide are liberated, which by

reason of the chimney draught are conveyed into the battery of
FIG, 180. Manufacture of rouil mordant. Recuperation of the nitrous products.

Marche des gaz = course taken by the gas ; Marche des liquides
= course taken by
the liquors ; Chaudiere = peroxidation vat ; Colonnes a coke = coke scrubbers ;
Soutirage = outflow.
carboys already mentioned. So far from being hermetically

closed, the stoppers of some of these vessels are pierced with
holes to facilitate admission of air, so that the nitric oxide, in
passing through the vessels, becomes mixed with an increasing

quantity of air, and is converted into nitrogen peroxide.
On the other hand, the first of the coke scrubbers is charged
with fresh water, the second receives the (0-5 to i Be.) liquor
from the first, and the third receives the 6 to 8 Be. liquor from
the second, and in turn discharges a 10 to 14 Be. liquor, which
is returned to the first carboy A of the battery ;
whilst the acid is
drawn off from one of the carboys of the middle set B, which
receives the gaseous products from the peroxidation vat. This
acid has the density 16 to i 8 Be., and in turn is delivered into
the third series of carboys C, theweak (20 to 22 Be.) acid to

be returned to the vat being drawn from the middle row of
carboys D, which receives the gas from the first carboy A. The
course taken by the gas and liquors is sketched in Fig. 1 80.
The nitrogen peroxide being in continual contact with water,
the regeneration of the nitric acid proceeds according to the
equations
2H O = 4HNO 3 +N O
2 2 2>
etc.
Theoretically, the whole of the nitric acid should be recovered

in the weak liquor ;
but in practice a considerable loss occurs
through leakage,secondary reactions, and the solution of a

fraction of the nitric oxide in the liquors, in consequence of which
it
escapes oxidation.
Theory indicates that to peroxidise 75 parts of ferrous
sulphate (equivalent to 100 parts of rouil} requires 5*70 parts of

nitric acid, which should be recovered in the waste liquors. As a
matter of only about 4 parts of 36 Be. acid, equal to 2'io of
fact,
pure acid, are recovered, the loss being therefore 36*8 per cent, of
the initial acid introduced.
On tracing the course of the gases, it will be found that they
consist of about f nitric oxide on entering the battery, but
merely traces of this oxide on their exit to the chimney stack.

The liquors collected in B are of a greenish colour, and are
highly charged with nitric oxide. If stirred, numerous bubbles of

gas are disengaged, and make their escape as red fumes.
This percentage decreases rapidly in the other vessels, whilst
the amount of HNO 3 continually increases under the influence of

progressive aeration.
This explains why the liquid has to be drawn off at the
centre of the battery instead of at the same end as the gases, as
would appear more rational. Another reason for the change is
that the gases carry over a large quantity of water vapour, and,
though the greater part of this is recovered on the way, a consider-

able proportion condenses in the first carboys of the battery, and

thus dilutes the acid liquor there.
Even when air is blown into the battery by a Korting
injector, to establish a regular circulation of the gases and liquor,
the degree of acidity is always greater at the middle of the
battery than in the end units.
This experiment was made with a view to ensuring more
complete condensation and a consequent increase in density of

the recovered acid. The results were very insignificant, the
increase being only i to 2 Be.
To ensure favourable recuperation and reduce the losses to a
FIG. 181. Manufacture of rouil mordant. Recuperation carboys.
minimum, there must be no back pressure in the battery. This

necessitates large outflow pipes and regularity of the reaction in
the vat. If the temperature gets too high, or the ferrous sulphate
is thrown in too quickly, there will be a sudden and enormous
liberation of gas, which results in an increased pressure, loss of
nitric oxide, momentary obstruction of the air supply, etc.
If the ferrous sulphate be added .too quickly when the vat is
too cold another accident may arise, i.e. the fixation of the nitric
oxide by the excess of ferrous sulphate, and the production of a
brownish-black compound, which is difficult to decompose even by
prolonged boiling: when this decomposition is effected it occurs

suddenly with great violence, and forces part of the charge out of
the vat. Hence it is
necessary that the reaction should be looked
after by skilled workmen.
External climatic conditions also exercise great influence
on the course of the recuperation process. Dull moist weather
lessens the chimney draught, and consequently increases the
pressure in the apparatus, and causes loss by leakage ;

on the
other hand, in bright dry weather the draught is better, and the
operation goes on more successfully.
(4) Insoluble Basic Sediment. This sediment, which has
already been mentioned, consists of a basic salt, insoluble in
water but soluble in acids, which is deposited in the storage

reservoirs as a viscous, ochreous magma.
The analysis of this salt in its crude condition, merely
drained, shows the following composition :
Sulphur trioxide (SO 3 ) = 24/43 P er cent.
Ferric oxide (Fe 2 O) 3

= 35'9O '
It also contains a considerable proportion of substances insoluble

inHC1, such as silica, earthy matter, lead sulphate, etc.
The sediment retains about 30 per cent, by weight of rouil.
When washed and dried it contains

Sulphur trioxide (SO 3 ) = 37*80 per cent.
Ferric oxide (Fe 2 O 3) =43-20
When the operation has been properly conducted the amount of
sediment does not exceed 8 to 10 per cent, of the total product,
but if badly conducted may attain as much as 20 per cent.
If it be remembered that 100 parts by weight of this
sediment, as taken from the reservoirs, are equivalent so far as
concerns its content of iron oxide to 240 or 250 parts of
rouil) and that it is generally wasted, or at least very difficult to

get rid of, it will be evident that the loss attains the enormous
proportion of 20 to 25 per cent, of the finished product. Later

on we shall see how this can be remedied.
(5) Cost Price. A staff of 2 men is sufficient to work the size
of plant we have described one man to look after the operation,
the other taking charge of the recuperation and the packing of

the products. They will be able to finish 4 charges a day. The
rouil is packed in carboys or petroleum barrels. The latter
must first be steamed out, and then carefully washed in order to
get rid of the traces of oil. The cost per cwt. of the rouil
product, packed in casks, amounts to
Nitric acid (36 Be. ), 4j Ibs = sd.

Ferrous sulphate, 76 Ibs 9k
Sulphuric acid (60 Be. ), 5 \ Ibs
= li
Labour = 3i
Lead, coal, etc 2
Management expenses, interest, etc I
Packing = 10
Total . . . .25. 8d.
The sale price averaging 33. 2d., the nett profit is therefore
6d. per cwt.
B. GESCHWIND PROCESS EMPLOYMENT OF SODIUM NI-

TRATE, AND RECOVERY OF BYE-PRODUCTS. This process, the
original idea of which is due to M. Gaillot, manager of the
Aisne Agricultural Station, is described in the author's (French)
Patent Specification, dated 4th August 1897.
It has been in use for more than I 2 months at the Chailvet
works, with excellent results.We have already seen that the

formation of sediment in the reservoirs entails a loss of about
20 to 25 per cent, of the finished product; consequently it is of
great interest to be able to prevent the formation of these sub-
or at any rate to use them up in the manufacturing process.
salts,
This has been successfully accomplished in a very simple manner

by dissolving the sediment in sulphuric acid, and using up a
fraction of the resulting ferric sulphate liquor in each operation.
The saving by the use of sodium nitrate is also

effected
considerable, and easily expressed in figures. Commercial 36 Be.

nitric acid contains 52*80 per cent, of HNO 3 and may be ,
reckoned worth zos. per cwt, the HNO

3 being therefore worth 2d.
per Ib. Commercial nitrate of soda contains 69'8o per cent, of

HNO 3 and costs about 75. 6d. per cwt., consequently the
,
3 HNO
in sodium nitrate costs a little over i d. per Ib., a saving of about
one-half. It is therefore advantageous to employ this method,
the more so that it is an extremely simple one.
The requisite apparatus is exactly the same as that for the
nitric acid process, except for an additional boiling pan made
of lead and heated by direct fire or steam, a lead-lined wooden
sodium nitrate tank, and tanks for the acid solution of ferric
sulphate.
(i) Dissolving the Sediment. This is a very simple operation.

About 66 gallons of the slimy sediment are placed in the supple-
mentary pan, which holds about 1 80 gallons, and, after adding
FIG. 182. Manufacture of rouil mordant. Treatment of sediment.

Section of boiling pan.
22 gallons of water and 20 gallons of 60 Be. sulphuric acid, the

whole is raised to boiling, and
kept constantly stirred.
is The
sediment gradually dissolves, and at the end of 2 or 3 hours the
liquor is run into tanks to clarify.
The solution has a density of 47 to 48 Be., is greenish
brown in colour, and exhibits the following composition per
litre :
In the manufacture of rouil 100 vols. of this liquor represent

I 2 of 60 Be. sulphuric acid.
It may also be employed for other purposes, and prepared

either in the aforesaid manner or by peroxidising ferrous sulphate
with nitric acid or sodium nitrate, in presence of the necessary

amount of sulphuric acid is utilised for coagulating blood from
FIG. 183. Manufacture of rouil mordant. Treating the sediment.

Section of boiling pan.
slaughter-houses, and converting the same into a non-putrefactive
manure.
(2) Dissolving the Sodium Nitrate. This operation is con-
ducted in a leaden pan, the salt being stirred up in hot water
and left to cool, thus furnishing a saturated 40 to 42 Be.
solution containing about 680 grms. of sodium nitrate per litre,
FIG. 184. Manufacture of rouil mordant. Treating the sediment.

Section through boiling pan and fire-place.
and serving to replace nitric acid in the peroxidation of ferrous
sulphate.
(3) Manufacturing Details. The peroxidation vat is charged
with 22 gallons (about 330 Ibs.) of the acid solution of ferric
sulphate, prepared from the rouil sediment as just described, together

with about 5 gallons of the nitrate solution (equal to 33 Ibs. of

sodium nitrate) and enough sulphuric acid (2'6 to 2^9 gallons of
60 Be. acid) to form sodium bisulphate with the base of the latter
salt. Heat being then applied, the ferrous sulphate is added by
degrees, and the operation is conducted in exactly the same
manner as in the nitric acid process, namely, adding part of the
recovered liquor when the reaction slackens, and stopping the
supply of ferrous sulphate as soon as the evolution of nitric
oxide ceases. The recuperation process is also the same as
before.
The rouil so obtained contains a little sodium bisulphate

about 46 Ibs. from a charge of the above dimensions, but in-
sufficient to affect the quality of the product.
Owing to the employment of the recovered ferric sulphate

from the sediment, a greater weight of product is obtained for a
given consumption and ferrous sulphate

of nitric con- acid ;
sequently the cost of manufacture is reduced, and works out as

follows per cwt. of product :
s. d.
Sodium nitrate, 2-65 Ibs. at 7s. 6d. per cwt. . . .=02

Ferrous sulphate, 64 is. od. . . .
=07
Sulphuric acid, 8i
,,
,, 2s. 6d.
,,
,, . . .=02
Labour 03
Coal, lead, etc. 02
Packing . . . . . . . . . . oio
Management expenses, interest, etc o i
Total
Since the cost in the nitric acid process is 2s. Sd., we have
here an extra profit of 5d. per cwt., i.e. I id. instead of 6d. a
decided advantage.
C. CHARACTERISTICS OF ROUIL. The colour of the rouil
liquor is
deep reddish brown by reflected light, rusty by trans-
mitted light. A blackish, greenish, or yellow tinge indicates

defective manufacture, being due either to fixation of the nitrous
fumes by ferrous sulphate, or to an excess of the latter or of
sulphuric acid.
In the first-named case, and w hen the defect r
is considerable,
it
may be remedied by adding sulphuric acid in larger excess and
applying heat. Red fumes and a characteristic effervescence will
282 MANUFACTURE OF ALUMINIUM SULPHATE, ETC.
be suddenly produced, and when the liquor is again quiescent the

black coloration will have disappeared.
In the second case, the liquor, after acidification with H SO 4
2 ,
evaporation to almost dryness, and abundant dilution with water,

will decolorise potassium permanganate. When the excess of
ferrous sulphate is considerable, the liquor will give off red fumes
on being treated with nitric acid in the warm.
When diluted with a large excess of distilled water rouil
liquor throws down a precipitate of an insoluble and highly basic

ferric salt, leaving a more acid ferric salt in solution, the reaction
being more pronounced if the water contain calcium carbonate.
It is on this property that the fixing of the ferric oxide by the
fibre in mordanting silk (j-ouillage) is based.
Commercial rouil is of 40 to 46 Be. density. It is of merely
relative stability, and tends to separate into an insoluble basic salt

and a soluble acid salt when stored for some months. It often
contains organic matters introduced by the ferrous sulphate and ;
these substances, incompletely destroyed by the nitric acid during

the peroxidation process, are gradually oxidised by the ferric
sulphate, which is thereby reduced to the ferrous state. This

reaction is accentuated by light.
A good quality should not contain ferric chloride, this
reuil of
salt being of no use in mordanting silk. The liquor should there-
fore give no precipitate with silver nitrate.
The following table shows the percentage composition of
several varieties of commercial rouil Nos. I, 2, and 3 having been
,
prepared by the sodium nitrate process, the others by the nitric
acid method :
PART III
CHAPTER V
USES OF ALUMINIUM SULPHATE AND ALUMS
I. APPLICATION TO THE ART OF DYEING
I 20. Introduction. It is very evident that the two most essen-

tial elements in and the dye stuffs with
dyeing are the materials,
which they are to be treated. There is also, however, a whole
series of substances the mordants of considerable importance
from the part they play in fixing the dye stuff on the fibre, or in
modifying the shade of colour obtainable. Chief among them

are the aluminium mordants, which have been from time im-
memorial, and still are, employed for all kinds of fibre.
The different alums, with ammonium, potassium, or sodium
as their base, have been the most widely used in dyeing, not only
because they are themselves mordants, but also because they
serve for the production of other aluminium mordants aluminium
acetate, sulpho-acetate, etc. They are still largely employed, the
best qualities being in the form of large vitreous crystals entirely
free from iron.
Alum
is, however, becoming more and more displaced every-
where by aluminium sulphate, which is now obtainable fairly pure

in commerce and in a state suitable for the preparation of all the
other aluminium mordants. It is besides more economical than

alum, the latter containing barely 10 or i i
per cent, of the really
283
284 USES OY THE SULPHATES OF ALUMINIUM AND IRON
active ingredient, alumina, whereas the well - made sulphate,

exempt from iron, contains 1 6 to 17 per cent, without being
any dearer.
When a solution of normal aluminium sulphate is partly

neutralised by adding sodium carbonate or bicarbonate, chalk,
etc., solutions of basic alumiimim sulphates are formed.
These new salts vary in composition according to the degree
of neutralisation, as the following equations will show :
(1) Al 2 (S0 4) 3 +2NaHC0 3
= A1 2 (HO) 2 (SO 4) 2 + Na S0 + 2CO,,

2 4
(2) 2[Al 2 (S0 4 ) 3 ] + 6NaHC0 3
= (A1 2 ) 2 (HO) C (S0 4) 3 + 4Na S0 + 6CO

2 4 2,
(3) Al 2 (SO 4) 3 + 4NaHC0 3

= A1 (HO) 4 (S0
2 4) 4 + 2N a;,S0 + 4C0 4 2.
The first of the foregoing basic sulphates is probably the one

most widely used.
When solutions of basic aluminium sulphates are boiled a
still more basic and insoluble salt is thrown down, especially in
presence of textile fibres, and a normal, or even acid, salt remains

in solution. Similar changes evidently occur when the fibres
impregnated with these solutions are dried ;

and it is upon these
facts that the employment of basic salts in mordanting is founded.
Experience teaches that the more basic the solution the more
readily is it decomposed, whether by heat or dilution with water,
and the larger the proportion of alumina fixed upon cotton fibre
by immersion and subsequent drying at a low temperature.

When caustic alkalis, or carbonates of the alkalis or alkaline
earths, are added to normal solutions of alum, products known as

neutral or basic alums are obtained. These are analogous to the
basic aluminium sulphates just mentioned, and their solutions
when heated and diluted decompose and furnish analogous pre-
cipitates (Hummel and Dommer). The manner of using alums

and aluminium sulphate as mordants is the same, and both com-
pounds should be free from iron.
121. Application to Cotton. The best method is that of
precipitation, the being impregnated uniformly with basic

fibre
aluminium mordant, dried, and entered in a solution of some salt

USES OF THE SULPHATES OF ALUMINIUM AND IRON 285
capable of fixing the alumina on the fibre, either by precipitation

in the form of oxide or by combination to form an insoluble
compound. A number of substances can be employed for this
purpose, such as ammonium carbonate, sodium phosphate, sodium

arsenate, sodium silicate, soap, ammoniacal sulphoricinate, etc. In
every case the fixing agent, degree of concentration, temperature

of bath, and duration of exposure must be accurately determined
by experiment.
122. Application to Wool. Normal aluminium sulphate
alone used for mordanting wool, the basic salt being too readily
is
decomposed, the result of which would be superficial mordanting,

dulness of colour, incapacity to stand the effects of friction, and
harshness of touch.
The solution must be boiling hot in order to expel the air in
and around the wool-fibre, as also to soften the fibre and render
it thoroughly permeable. It is also desirable to add a certain
quantity of potassium bitartrate, since this increases the depth

and brightness of the subsequent colour, prevents the ready and
superficial precipitation of alumina by the ammonia proceeding
from the wool, and increases the amount fixed on the fibre.
To mordant 10 grms. of wool with aluminium

successfully
sulphate, O'8 grm. of this salt and O'7 grm. of potassium bitartrate
(cream of tartar) are dissolved in i litre of water. The wool is

entered into the cold liquor and the temperature is raised to
boiling point within i to 1

1 hours, and, after being maintained
thereat 30 to 60 minutes, the
for fibre is carefully washed
(Hummel and Dommer).
123. Application to Silk. The aluming of silk may be per-
formed anterior to or during the operation of dyeing. In the
former event the alum bath may be kept going continuously,
whereas in the latter case it generally has to be thrown away
after use.
The silk being made up into batons, is put through three or four
stretchings and steeped for several hours in the alum bath, being
generally entered in the evening and left over night. The bath
should be cold-saturated, and is replenished from time to time with
a boiling concentrated solution of alum or the same result may
286 USES OF THE SULPHATES OF ALUMINIUM AND IRON
be obtained by keeping a bag full of alum crystals in one end of'
the bath and stirring up well after each passage of the silk.
For this, as in all the other operations of dyeing, the silk,
whether raw or boiled, should always be properly moistened

beforehand, i.e. should contain about its own weight of water, a
result obtainedby wringing it well. If introduced dry, the silk
dyes badly, and in some cases absorbs the bath liquor with,
difficulty. It follows that this degree of moisture causes the
permanent baths to undergo corresponding dilution ;

hence the
necessity for replenishment with concentrated liquor in order
to keep up their standard strength.
The alum bath should be cold. On leaving the bath, the silk
should not be allowed to dry or it will become harsh to the touch
and difficult to moisten again ;

in another passage through
fact,
the alum bath will be necessary. After being well drained the
silk is rinsed slightly with running water and, if necessary, beaten
(coarse silks).
Only a very little alumina is fixed on the silk by aluming,
and even this amount is so by the action of the rinsing water,
which should preferably be calcareous, calcium bicarbonate
assisting to precipitate alumina on the fibre (M. Moyret, Traitc

de la teinture des soies}.
Silks that have already been dyed are alumed in the same
way ;
the bath may perhaps be warmed up a little, and is gener-
ally used but once.
Aluminium sulphate is used in the same manner, the alumina
being usually fixed by a slight rinsing with water and a brief

sojourn in a cold bath of sodium silicate (density, roo5), followed
by careful washing. The use of basic aluminium sulphate may
spoil the brilliancy of the resulting shades.
1
24. Preparing and Using Aluminium Acetates. Normal
aluminium acetate may be obtained in solution by dissolving
alumina in acetic acid, or by adding lead acetate solution to dis-
solved aluminium sulphate in the proportion indicated by the
equation
A1 2 (S0 4)3 ,
i8H 2 + 3 [Pb(C 2 H3 2) 2 , 3 H 2 O]
= A1 2 (C 2 H 3 2)6 + 3 PbS0 4 + 2 7 H 2
0.
From this normal salt a series of basic aluminium acetates

can be obtained by treating the solution with increasing quantities
of an alkali carbonate.
The solutions of these basic acetates, containing sodium
acetate, are precipitated by heat, the higher the basicity the
lower the temperature required for dissociation.
Curiously
enough, however, this temperature is higher the more dilute the
solution mere dilution alone will not cause precipitation.
;
Freshly prepared solutions of pure aluminium acetate (equiv-

alent to 200 grms. of ordinary sulphate per litre) are not
precipitable either by heat or dilution ;

but when left at rest
for a certain time they decompose spontaneously, alumina being
deposited.
All solutions of the various aluminium acetates, whether
normal or basic, are precipitated by heat when diluted, if they
contain sulphates such as potassium or aluminium sulphate, etc.
This is always the case with the basic acetates, made from alu-
minium sulphate, when a portion of the lead acetate is replaced by

alkali carbonates
A1 2 (S0 4 ) S ,
8H 2 + Na 2 C0 3 + H O + 2 [Pb(C 2 H 3 O 2 ) 3 H 2 O]
1
2 2,
= A1 2 (C 2 H 3 2) 4 (HO), + Na.2 SO 4 + 2PbSO 4 + CO 2 + 2 4 H 2 O.

The result is the same, whether the sodium carbonate is
added before or after the lead acetate. When a solution of

normal aluminium acetate containing sulphates is precipitated
by heat, the precipitate re-dissolves on cooling; but under no
circumstances does this happen with the basic acetates. The
precipitate formed in presence of sulphates is an aluminium
sulphate containing a large excess of the base.
Experience has shown that when cotton is impregnated with
a solution of normal aluminium acetate (
= 200 grms. of normal
sulphate per litre), and then dried at a low temperature, about
50 per cent, of the alumina present is fixed on the fibre; and
an equivalent solution of the basic salt A1 2 (C 2 H 3 O 2 ) 4 (HO) 2 con- ,
taining sodium sulphate, will, under the same conditions, give up
nearly the whole of its alumina.

Aluminium acetates (especially the normal salts) prepared
with lead acetate are liable to contain a little lead sulphate.
For this reason, lead acetate may be advantageously replaced
by an equivalent quantity of calcium or barium acetate when the

presence of this sulphate would be injurious.
It has long been known that no practical advantage accrues
from using enough lead acetate to decompose the whole of the

aluminium sulphate. According to Koechlin, this is explainable
by the assumption that the actual mordant fixed on the fibre is
not pure alumina, but probably in most cases an insoluble basic

aluminium sulphate.
An excellent mordant may be prepared by dissolving in-
soluble basic aluminium sulphate in hot acetic acid. The basic
sulphate is easily obtained by carefully neutralising a solution of

alum by sodium carbonate, until the precipitate first formed
ceases to re-dissolve.
This method is due to Koechlin. Aluminium sulphate
may also be used, and the resulting mordants are known as
aluminium sulpha-acetates, their formation being shown by the
following equations :
(1) A1 2 (S0 4) 3 ,
iSH 2 + 2[Pb(C 2 H 3 2)2 , 3 H 2 0]
= A1 2 SP 4 (C S H S 2 ) 4 + 2PbS0 4 + 2 4 H 0, 2
(2) A1 2 (S0 4 ) 3 i8H,0+ 3 [Pb(C 2 H 3 2 ) 2 3 H 2 O] + 2 NaHCO 3

, ,
= A1 2 SO 4 (C 2 H 3 O ) 3 HO + 3?bSO 4 + Na 2 SO 4 + 2CO 2 + 45 II
2 ,
A
Experience has shown that the more basic these sulpho-
acetates the lower their decomposition point, whether by heat or
dilution, i.e. their sensitivity is increased.
Aluminium sulpho-acetates up nearly all their alumina

yield
and drying.
to cotton fibre after impregnation In this particular
they act more strongly than aluminium sulphates, and almost the
same as basic aluminium acetate
A1 2 (C 2 H 3 2) 4 (HO) 2 .
The technical name applied to the various acetates and

"
sulpho-acetates of aluminium employed in dyeing is red
mordant," because they are universally used for printing and

dyeing alizarine reds on cotton. Commercial red mordant is
prepared by the double decomposition of normal aluminium
sulphate and commercial calcium acetate. It contains a certain
amount of undecomposed aluminium sulphate, and is an impure
" "
sulpho-acetate ;
the variety known as red tin mordant is one
where the been effected as completely as
decomposition has .
possible, and which consequently represents an impure normal

aluminium acetate.
These mordants are chiefly used for cotton, and especially for
calico printing. The mordant solution is thickened with flour,
starch, dextrin, etc., and is then printed on the cotton and dried.
The cloth, in a more or less open and stretched condition, is
afterwards exposed to the air under suitable conditions of tem-
perature and humidity.

Next follows fixing or dunging, an operation consisting in
passing the goods through hot liquors containing cow's dung,
sodium arsenate, sodium phosphate, sodium silicate, chalk, etc.
The object of this treatment is threefold, namely

(1) To more thoroughly fix on the fibre that part of the
mordant which has escaped the influence of the air during the
stretching process.
(2) To prevent the subsequent staining of the unprinted
portions through the running of the soluble mordant.
(3) To remove the thickening materials.
"
Aluminium acetates are largely used for the so-called steam
colours," and frequently serve to replace basic aluminium sul-
"
phates in Turkey-red dyeing." On the other hand, they are
rarely employed for common fabrics, since under the ordinary

conditions of fixation they offer no advantage over the basic
sulphates, and are more costly. They cannot be used for
mordanting wool, owing to their low stability and are but ;
seldom employed for silk, except in printing (Hummel and

Dommer).
125. Employment of Aluminium Sulphate in Carbonising
Wool. Wool is frequently contaminated with vegetable im-
purities, which are very difficult to entirely remove by
mechanical
means, and are a source of great trouble in the dyeing process

when present in piece goods.
Itwas proposed by R. Joly, of Elbeuf, to destroy these
impurities with aluminium sulphate, and the method was
after-
wards adopted by many cloth manufacturers of Elbeuf, Sedan,

19
Chateauroux, Romorantin, Mazamet, etc., it having been found

possible by this means to carbonise fabrics dyed with fugitive
tints (Rev. Ind. et Sciences Chim., 1879, p. 69).
Aluminium chloride can be prepared from aluminium sulphate
by simply treating the latter with calcium chloride, which is

cheap
and easily procured. The dissolved aluminium chloride is easily
separated from the precipitated calcium sulphate by filtration,
alone or assisted by pressure (filter-press). The solution em-

ployed in carbonising has a density of about 5 Be. for delicate
tints, or f Be. for darker shades. The fabric is immersed in
and thoroughly impregnated with the solution, and is afterwards

drained in the hydro-extractor whether loose wool, yarn, or cloth
dried at 60 to iooC, and carbonised at 120 to I35C.
Under the influence of this temperature the chloride reacts on the
vegetable impurities, and decomposes them without altering the

dyes or the animal fibre in the least. All that is necessary is to
shake, stir, and beat the material, and the carbonised matter will
come out as dust. The operation should be followed by a
thorough scouring ;
and the material should be carefully washed
before entering the aluminium chloride bath (Pommier, article on
" "
Alum in Fremy's Encyclopedic}.
2. EMPLOYMENT IN THE MANUFACTURE OF PIGMENTS
126. The Manufacture of Lake Pigments. A '"lake"

"
pigment consists of a solid material, or base" generally white,
tinted by some colouring matter.
Sometimes the base is coloured direct, as if the dyeing of a
fabric were in question ;
but generally the base and pigmentary
matter are precipitated together, so as to produce the most
intimate combination possible between them.
The production of lakes is a delicate operation, and a matter
of great importance.
Artists employ several handsome and durable lake colours
(madder lake, weld lake, etc.).
Paper stainers use a large quantity of lakes, often rather
fugitive (redwood lakes, aniline lakes, etc.).

Cloth printers are also large consumers of fustic lakes, alizarine

lakes, etc., the colours being dissolved in acetic acid, and the
solution, after being thickened, is printed in the ordinary manner.
The cloth is afterwards steamed to drive off the acetic acid and
fix the colouring matter on the fabric.
The base most frequently employed in the production of lake
pigments is alumina, either alone or in combination as various

salts, mostly of a basic character.
Alumina is often employed as gelatinous alumina, precipitated
by a slight excess of ammonia from a solution of alum or alu-
minium sulphate.
Gelatinous alumina readily absorbs pigments, and is stained
directly by a decoction of cochineal, redwood, weld, etc. ;

but
more often the resulting lakes are deficient in brightness, and
moreover, when dried they become hard, horny, and difficult to
thin down with water or oil.
In manufacturing lake pigments the basic aluminium sulphate
corresponding to the formula A1 2 O 2 SO 4 is most frequently used.

This salt is insoluble in water it is pure white and
; opaque,
instead of being transparent like gelatinous alumina.
It is easy to collect and wash, and when dried furnishes a
very white friable product, not hard or horny.

This basic sulphate is prepared by saturating a solution of
alum or aluminium sulphate with sodium carbonate until a light
persistent precipitate is formed. is kept Constant agitation

up
during the operation, and the clear liquid is separated from the
precipitate. This liquid when boiled deposits the basic sulphate,
which is then washed by decantation.
In order to obtain a product of known composition, the
solution ofalum or aluminium sulphate may be precipitated
with sodium carbonate until the reaction becomes alkaline, in-
dicating that the whole of the alumina is precipitated. This

operation gives the quantity of sodium carbonate necessary for
the complete saturation of the sample. The operation is then
repeated, taking only two - thirds of the quantity of sodium
carbonate thus indicated. The reaction is as follows :
A1 2 (S0 4) 3 + 2Na,CO 3 = 2CO + 2

2Q2 USES OF THE SULPHATES OF ALUMINIUM AND IRON
Generally the precipitation of the basic sulphate is not effected

separately, but is combined with the incorporation of the pig-
ments.
Sometimes alumina, or the basic salt precipitated from alum
or aluminium sulphate by metallic zinc at boiling temperature, is
used.
Sodium aluminate is also largely employed. The salt is
mixed with a decoction of the pigment, and the product is

thrown into a solution of aluminium sulphate, the precipitated
alumina carrying down the colouring matter.
Various other insoluble salts of aluminium, such as phosphates
and, above all, the borate, are used as bases for lake pigments.
The advantage of this is that the borate, for example, can be
prepared from aluminium sulphate and borax. The latter salt

having only a feeble alkaline reaction, does not affect the pig-
ments that are sensitive to alkalis, such as cochineal, redwood, etc.
Insoluble aluminates, and notably magnesium aluminate, also

serve for the preparation of lake pigments.
Magnesium aluminate is obtained by gradually adding

ammonia to a solution composed of
Potassium alum 45 grms.
Magnesium sulphate 13 ,,
Ammonium chloride .
'
. . . . . 6 ,,
dissolved in 250 c.c. of water. The aluminate precipitated carries

down nearly all the magnesia. By adding to the solution some
pigment, such as a decoction of cochineal, a handsome lake will
be produced, provided an excess of ammonia is avoided.
Stannic acid combines readily with pigments, and forms the
basis ofmost lakes employed in cloth printing.
Sodium stannate may be used to prepare lakes on a stannic
acid basis. The method is similar to that used for sodium
aluminate, a solution of the pigment in sodium stannate being
precipitated by dichloride of tin. Sometimes aluminium sulphate
isused to precipitate the sodium stannate, in which case a true
aluminium stannate, representing the base of the lake, is formed.
Antimonic acid, antimony oxide, tungstic acid, oxides of lead,
zinc, chromium, magnesium, calcium, etc., also serve as bases for

certain lakes, as also chalk, albumin, gelatin, and even starch or

flour. This need not be further discussed.
For paper staining and cloth printing the lakes are sold in
paste forms, and are thus easy to use. These generally contain
33 per cent, of water.
For use as artists' colours, the lakes are generally supplied in
lozenges. For making these on a small scale the paste is put in

a funnel, into the stem of which is inserted a glass rod. By
pressing on this rod the paste is forced out in the shape of small
conical heaps, which are then placed on sheets of glass and dried
in a stove at a low temperature. The dried blocks separate
easily from the glass.
The
lakes are also frequently supplied in the form of dry
powder, which is more simple and is free from inconvenience

when they have to be ground in oil or water (Guignet, article on
" "
Colour Making in Fremy's Encyclopedic].
127. Yellow Lakes. A. WELD LAKE. Weld (Reseda

hiteola] an indigenous plant which was formerly grown on a
is
large scale for dyeing purposes, but is now almost gone out of use.
The pigmentary principle of weld is luteoline, discovered by
Chevreul. Luteoline is almost colourless, but turns deep yellow
under the influence of a powerful base ;
it crystallises in beautiful
needles, and behaves as a weak acid. only sparingly soluble

It is
in boiling water, but dissolves in considerable quantity in water

at 200 under pressure. For the production of weld lake, well-
harvested and dry plants not those browned by exposure to
rain, air, and light are selected. Plants that remain slightly
green when dry are just as good as those of a pure yellow colour.
The plant is cut into small pieces and left in water for i 2
hours. It is then boiled and a weight of alum equal to that of
the weld is added, the liquid being then boiled up for a few
minutes, filtered through a cloth, and afterwards precipitated by
sodium carbonate solution so as to throw down a basic aluminium
sulphate. The pigment is carried down with the precipitate,
which has merely to be collected, washed by decantation, and
dried at gentle heat.
Another process consists in preparing a white base by boiling
I kilo, of pure chalk in I litre of water and adding I oo grms. of

powdered alum. Brisk effervescence ensues the mixture is ;
stirred and a decoction of weld is added by degrees until no more
of the pigmentary principle is absorbed. The mother liquor

separated from the lake serves for treating a fresh quantity of
weld.
Weld lake is the most durable of all the yellow lakes, and is
the only one suitable for use as an artist's colour (Guignet).

B. YELLOW (STIL DE GRAIN} LAKE. This is a lake of
somewhat complex composition, and is only used for theatrical
decorations, floor-staining, etc. It is not very stable.
"
The chief ingredients of this lake are " French berries (grainc
" "
d'Avignon, the fruit of Rhavmus infectorius] and Persian berries
(from Rhamnus saxatilis], to which are added quercitron, weld,

fustic, safflower, curcuma all freshly gathered.
The decoction is treated with alum or aluminium sulphate,
and filtered, the filtrate being then mixed with finely powdered
chalk and the whole stirred briskly to facilitate the liberation of
carbon dioxide.
C. OTHER YELLOW LAKES of fine appearance, but deficient
in permanence, are prepared from quercitron, the bark of an

American oak (Quercus nigrd] (Guignet).
128. Red- and Rose Lakes. A. MADDER OR ARTIFICIAL
ALIZARINE LAKES. A great variety of tone can be obtained
from madder lakes, ranging from light rose-red to deep violet,
almost black, through the entire scale of reds.
The lighter shades can be easily prepared by adopting the
following precautions :
When madder is used it is extracted with cold water, in order

to remove all the extraneous substances (gums, sugars, albumin,
etc.) likely to injure the preparation of the lake. Most of the

methods in use are based on the property exhibited by "alizarine
of dissolving in a hot solution of alum, in which particular the
artificial alizarine is
especially distinguished. For rose-red lakes
the variety known as alizarine for reds is used, alizarine for violet
being taken for violet and purple-brown lakes. Both substances
are obtainable in the form of yellow-brown liquid paste, very
sparingly soluble in water but soluble in alcohol. Alkaline

solutions dissolve alizarine and furnish a fine red liquid ;
alum
gives a slightly yellowish solution, and if the operation is con-
ducted at boiling temperature a portion of the alizarine deposits
on cooling. Besides, it is better not to boil madder or alizarine
in presence of alum solution; a temperature of 40 to 5oC. is
quite sufficient for the saturation of a solution of I

part alum in
10 to 12 parts water with alizarine.

After cooling the liquid down to 35 to 40, a solution of
sodium carbonate is gradually added, with continual stirring, not
more than f as much sodium carbonate as would fully saturate
the alum being used. Bytime the liquor will have become
this
a deeper red in colour, and when heated to boiling will throw

down basic aluminium sulphate, which carries the alizarine down
with it and forms a fine dark rose-red lake, even when dried.
According to Persoz, this lake offers the advantage of com-
plete solubility in acetic acid, on which account it can be used in

cloth printing. The same author also gives another method of
preparing this lake, namely, by adding sub-acetate of lead to a
solution of alum saturated with alizarine at 30 or 40. An
abundant precipitate of lead sulphate is formed, and on filtration
is separated from the dark red liquor, which when boiled deposits
the lake in question. The most suitable proportions to use
appear to be equal weights of alum and (solid) sub-acetate of

lead. The residual mother liquor will serve for dissolving a
fresh quantity of alizarine.
A handsome lake is obtained by dissolving alizarine in water
containing a very little ammonia, and by adding gradually thereto
a i o per cent, solution of alum. This lake is of a dark red colour.
In the same manner a very dark violet, or even nearly black, lake
can be prepared by adding ferric sulphate to the alum, or by

using ferrous sulphate by itself.
has described a very ingenious process consisting in

Kopp
treating madder with a solution of sulphurous acid. This gives
a solution of alizarine, which when heated with saturated alum
solution furnishes a lake of good quality.
Nowadays madder lakes are very little used, their place

having been taken by lakes made from artificial alizarine and

purpurine.
These lakes are often adulterated, the red kinds often contain-
ing cochineal, redwood, fuchsine, cosine, safranine, etc. and the ;
violet or black lakes, campeachy, archil, aniline violet, etc.
(Guignet), constituting adulterations difficult of detection.

B. COCHINEAL LAKES. The mother liquors from the manu-
facture of carmine are often used for making these lakes, being
.employed to thin down gelatinous alumina or basic aluminium

sulphate, or mixed with alum and boiled after saturation with
sodium carbonate.
It is,however, preferable to work with fresh materials, and to
boil the ground cochineal in water containing potassium bitartrate.
The extract is filtered and treated with powdered alum, a little
tin protochloride being added drop by drop when solution is
complete. After a while a very fine quality lake is deposited,

and, when this has been collected, a second lake, of inferior quality
and lighter colour, can be recovered by precipitating the mother
liquor with sodium carbonate (Guignet).
The cochineal lakes, known as carmine lakes, are often
adulterated with chalk or starch.
Very handsome rose-red lakes are easily prepared by dissolv-
ing ammoniacal cochineal in water, filtering the solution, and pre-

cipitating with saturated alum.
Ammoniacal Cochineal
in tablets is also a lake prepared in a
special manner. Three parts of ammonia and I of cochineal are

macerated for a month in a closed vessel, the clear liquid being
then drawn off and mixed with o 4 part of gelatinous alumina.
-
The whole is evaporated in a copper vessel until all smell of

ammonia has disappeared, whereupon the thickish mass is cut up
into tablets and dried (Wurtz's Dictionary).
C. LAC LAKE. The raw material for this product is stick lac,
the thick, hard, adherent incrustation surrounding the twigs of

certain large fig trees or mimosae, and consisting mainly of a
mixture of resins enclosing cells wherein are imprisoned certain
gall insects (Coccus laced) which yield a red pigmentary matter
(carminic acid).
To prepare lac lake, a decoction of stick lac in weak caustic

soda is precipitated with alum.
Lac lake contains
Pigmentary matter .
50 parts,
Resins . . . . . . . . .
40 ,,
Alumina . . . . . '. . . .
9
Extraneous matter i , ,
For use, this aluminous lake is dissolved in hydrochloric or
sulphuric acid (Wurtz's Dictionary}.

D. REDWOOD LAKES. There are several varieties of red-
wood, namely, Pernambuco wood (Cczsalpinia crista] ;

Brasil wood
(C. brasiliensis) ; Sapan wood (C. sappati] ;
Brasilette (C. vesicarid],
the latter being the least valuable ; and, from these woods, lakes
are prepared on a base of stannic acid, antimony, oxide, etc.
Venetian Ball Lake is obtained by incorporating gelatin and
gelatinous alumina in Brasil extract, the latter being renewed

until no more colouring matter is taken up. The colour is then
brightened by the action of alum, or turned violet by means of
soap solution. Italian Lake is prepared by mixing a decoction
of redwood with alum, followed by chalk to partly neutralise the
latter and throw down alumina, which fixes the colouring matter.
Basic aluminium sulphate or previously saturated alum, which
will throw down the sulphate when heated, can also be used.
Starch paste is sometimes added to redwood lakes, especially
when they are to be used in making fancy papers.

Although not very fast colours, the redwood lakes are largely
used by paper stainers for marbling fancy papers, etc., as well as
for theatrical decorations (Guignet).
E. ANILINE RED LAKES. Several very handsome and fairly

durable lake pigments of this class are prepared from various
artificial dye-stuffs.
129. Green Lakes. These are merely mixtures of yellow

and blue lakes, so as to produce transparent greens ;
fustic lake
and Prussian blue, for example, furnishing very handsome green

shades, though not very fast.
1
30. Violet Lakes. As already stated, violet lakes are
prepared from madder and very fine ones can also be obtained
;
from campeachy and tin dichloride.

Very good violet lakes for coloured and fancy paper are now
made, from aniline violet, by employing an aqueous solution of
this violet to colour a white base formedof basic aluminium
sulphate combined with gelatin. Sometimes, also, small quantities

of tannin and starch are added.
The finest compound violets are obtained with Prussian blue
and madder or cochineal lakes (Guignet).

131. Application of Aluminium Sulphates to the Manu-
facture of Prussian Blue. Prussian blue is made by a very
simple process, namely, precipitating a solution of potassium
ferrocyanide, or yellow prussiate, with a salt of iron, under suit-

able conditions.
Prussian blue in the pure state is inapplicable for most
purposes in painting, and consequently the commercial varieties

contain extraneous substances, not always with intent to defraud.
Thus the addition of an aluminium compound at the moment of
precipitation seems to improve the product. For this purpose

alum is mixed with the iron sulphate used, and the resulting
aluminium ferrocyanide, which resembles alumina, remains inti-
mately mixed in the mass.

For best quality Prussian blue, I
part of alum is used to
every 7 or 8 parts of iron sulphate, whilst for the lower grades

the proportion is increased to i 123; and for the lowest of all,
equal parts are used. The alum may be advantageously replaced

by an equivalent quantity of aluminium sulphate (Guignet).
Mineral Blue or Antzverp Blue is a kind of Prussian blue
adulterated in the process of preparation, magnesium sulphate
and zinc sulphate which form a white precipitate with potassium
ferrocyanide being added in addition to alum.
132. Application of Aluminium Sulphates to the Manu-
facture of Thnard Blue. This pigment has now almost
entirely gone out of use ; nevertheless, it is of considerable historic
interest, being the first cobalt blue pigment ever used as an

artist's colour.
It is prepared by precipitating a solution of cobalt chloride

or nitrate by tribasic sodium phosphate, which gives a somewhat
violet-tinged, rose-red, gelatinous precipitate of tribasic cobalt
phosphate. After careful washing, the phosphate is

intimately
mixed with gelatinous alumina prepared by adding an excess of
ammonia to a solution of alum, or aluminium sulphate free from
iron, and washing the precipitate.
The mixture is dried in the oven and calcined at cherry-red
heat in a closed crucible. The proportions given by Thenard
are : i
part of tribasic cobalt phosphate, in the condition of paste
(with 30 per cent, of moisture), and 8 parts of gelatinous alumina
(Guignet).
133. Employment in the Preparation of Mars Yellow.
Bourgeois employed alum in the preparation of Mars yellow by
precipitating a mixture of ferrous sulphate and alum with sodium
carbonate. The handsome golden yellow - brown precipitate
assumes various tints under the influence of a longer or shorter
calcination.
i
34. Employment in the Manufacture of Indian Yellow.
Analysis having revealed euxanthic acid, alumina, and magnesia
as the essential constituents of Indian yellow, attempts have been
made to reproduce this compound by artificial means. With this
object a solution is prepared of

Potassium alum 45 grms.
Magnesium sulphate 13 ,,
Ammonium chloride . . . . . . 6 ,,
in 250 c.c. of water, and to this solution is added euxanthic acid

dissolved in a minimum quantity of ammonia. A yellow pre-
cipitate is formed of inferior brightness to the natural Indian
yellow.
3. VARIOUS APPLICATIONS OF ALUMINIUM SULPHATES
135. Hide and Leather Industry.

Employment in the
Attempts have been made tanning with aluminium salts with

at
or without soap, but the results were not very satisfactory. The
method, which was based on the fact that alum or aluminium
sulphate will, like tannin, form insoluble compounds with gelatin,
gave merely imitation leathers, and, despite numerous attempts,
no one has yet succeeded in producing good saddle leather by
this means.
fi.,U. b. L.H.
3OO USES OF THE SULPHATES OF ALUMINIUM AND IRON
On the other hand, alum is successfully applied to the pre-

paration of leather by ordinary and Hungarian tawing, the last-
named process being practised on the thick hides of buffaloes,

oxen, and horses to produce white leather for saddlery and
harness making. For this purpose the hides are scraped with
knives and placed in a soak of alum and brine, and are then
beaten to expel a portion of the coriin extracted by the brine.
The alum acts as a plumping liquor, by virtue of its acid properties
and its astringent, antiseptic qualities. On leaving the soak the
hides are dried, heated in an oven, and greased with tallow.
If the proportion of common salt exceeds 3 molecules to 2 of
alum the latter isdecomposed into aluminium chloride, which
remains in the hides, and into sodium sulphate, which diffuses in
the bath liquor.
In the Hungarian tawing process the alumina whether
present as sulphate or chloride does not combine with the
animal matter ;
and a washing with water is sufficient to dissolve
it and regenerate the hide, which is then readily gelatinised by
boiling in water (F. Jean).

Tawed skins are mainly used for boot and glove making,
those of the goat, kid, sheep, and lamb especially being treated
for the latter purpose.
The dry skins to be tawed are soaked for a period depending

on their thickness and
degree of dryness. After removing
adherent flesh they are unhaired either by lime or sodium
sulphate then scraped and rinsed in a tub. The next stage

consists in immersing the skins for 6 to 1 2 hours in water
containing the putrefied excrement of dogs or pigeons, in order

any lime they may have
to dissolve out retained, as well as to
plump them, render them supple, and fit them for receiving
the dressing. After this follows steeping for 3 days in a vat
containing water at 30 to 35 C. with bran and flour, the skins
being subjected every day to a fulling process, rinsed, and scraped

to remove particles of flesh. The dressing, which corresponds to
the tanning process in other leathers, by fulling the
is effected
skins in a lukewarm mixture of egg yolks, alum, and

brine, flour,
water until they are uniformly impregnated and of equal thick-
ness throughout. They are next doubled, flesh-side inwards,

dried as quickly as possible, and packed in bundles. Finally,
they are streaked and pared to supple them and remove residual
traces of dressing paste and flesh and when rinsed and air-dried
;
are ready for dyeing.

In the German method of dressing skins, which differs from
the French process in employing stronger limings, dispensing with
the bran soak, and by employing a supplementary treatment with
the softening iron and fulling mill, the following soak is used for
IOOO skins :
Flour 27^ Ibs.
Alum 27^ ,,
Common salt n ,,
Fresh eggs 10 galls.

Milk 0-9 ,,
with sufficient water to form a stiff paste (F. Jean).

136. Employment in Paper-making. Paper made from
rags or the various other materials employed cannot be used for
writing unless the pulp is mixed with certain substances to bind

the fibres together, stop up the pores, etc. The paper has there-
fore to be glazed. Formerly gelatin was employed for this
purpose, particularly in England ; but, in addition to the incon-

venience exhibited by the papers so treated, the operation was
delicate, expensive, and had to be performed on paper already in

sheet form.
Attempts were then made to glaze the paper in the vat, and
D'Arcet was the first to propose a practical formula for the use of
vegetable glues. His mixture had the following composition:
Starch . . . . . . . . . 12 parts,
Resin (dissolved in half part of sodium carbonate) . I
part,
Water .
.315 parts,
these proportions being employed per 100 parts of dried pulp.

The papers made in this manner were deficient in tenacity, and
D'Arcet altered the formula to
Flanders glue
Resin soap
........ 4 parts,
8 ,,
Alum 8 ,,
per i oo parts of dried pulp.

3O2 USES OF THE SULPHATES OF ALUMINIUM AND IRON
According to Payen, the resin soap is prepared by crushing

and sifting 150 parts by weight of resin, which is then treated
with a hot caustic

lye obtained by mixing 75 parts of soda
crystals,375 parts of water, and 12 parts of lime. The amount

of water is increased, by the washing water and the steam used
for heating, to I
50 parts, and, after boiling for half an hour, 750
parts of resin soap are obtained.
As this soap would not mix very easily with the pulp, 75
parts are dissolved in 500 parts of lukewarm water containing 20
parts of starch, the granules of which swell up considerably in the
solution when raised to boiling temperature by a jet of steam.
This liquid is added to the pulp and, after about a quarter of
an hour, is stirred up well and mixed with a solution of alum,
which forms an insoluble impermeable glue. The following
proportions are often employed To each cwt. of fine paper and
:
210 gallons of water are added about 82 gallons of agglutinant

(prepared as above), and the whole is precipitated with 4-1 Ibs. of
alum.
According to Planche, 210 parts of water, 16 parts of 80

soda, and 8 parts of lime, boiled for 3 or 4 hours, are required to
dissolve 100 parts of resin. After leaving to clarify, the clear
liquor is drawn off, and the caustic lye is run into soap-making
pans. The resin is thrown in bit by bit, the mass being kept
stirred and raised to boiling point until the whole is dissolved,
which takes about 4 or 5 hours. In the earlier stage the heat
must be applied with caution, in order to prevent the resin soap
from boiling over. In order to use this soap without any addition
of starch, a portion is then thinned down in 20 parts of hot
water, the solution being left to settle for I or 2 hours, and

afterwards drawn off as required. To mix starch with this, the
soap solution is run off into a pan, and incorporated with starch,
previously mixed with warm water and passed through a fine
sieve. As soon as the mixture is complete it is boiled for half

an hour, with continued stirring. Usually 2 parts of starch are
taken to every 3 parts of resin.
When the pulp is well impregnated with the agglutinant it
precipitated by alum, as already stated. Liesching states th :

better results are obtained by adding alum first and the resin
agglutinant afterwards, the alum apparently penetrating the pores

of the paper in a more complete manner.
Aluminium sulphate may be advantageously used in place of
alum, but should not contain any free acid. For white papers, or
those to be coloured in light tints, the alum should not contain
"
iron (P. Charpentier, article on Paper" in Fremy's Encyclopedic}.
If the paper is to be blued with ultramarine, it is essential for the
alum or the aluminium sulphate to be perfectly free from uncom-

bined sulphuric acid.
Aluminium sulphate and alum are also employed in paper-
making as mordants for fixing colours, just as in the dyeing
industry.
137. Application for hardening- Plaster. It has long been
known that plaster prepared with solutions of certain salts sets
much harder than when mixed with water alone. The use of
alum for this purpose was proposed by Pauware, the process being
afterwards improved by Greenwood, and thoroughly investigated
by Eisner (Knapp). In Pauware's original process the plaster

articles were treated with alum solution after casting, by steeping
them for a month in a solution consisting of I
part of iron-free
alum and water at a temperature of I 5 per cent.
I 2 parts They
were then washed and dried in a current of hot air. After this
treatment the plaster was found to have increased in hardness and
no longer soiled the fingers at the same time, it could only be
:
scratched with difficulty by the finger-nail ;

but after a time the
articles proved incapable of resisting the influence oT moisture,
and, in addition, assumed an irregularly distributed greyish
coloration. Moreover, plaster treated by this process softened to
such a degree as to easily take the impress of finger-prints. In
the second process the block plaster heated in the ordinary
manner is
plunged for several minutes into a solution containing
8 to 10 per cent, of alum, and is then calcined over again at
a dark red heat the temperature must be uniform and constant.
;
The resulting plaster is dull, and has a milk-white colour, or faint

Isabella tint ;
and
can easily be reduced to powder. If the
temperature in the second baking has been pushed too far, the
edges of the blocks are as hard as stone they can only be ;
powdered with difficulty, and are really scorched.

Articles manufactured of alumed plaster set much more
slowly than those of ordinary plaster, but finally attain a degree
of hardness resembling alabaster or marble ; and, besides, exhibit
at the edges and thinner places a kind of translucence which
further increases this resemblance. Slabs of a certain thickness
can only be broken with difficulty under the hammer, and when
left exposed to the weather for several months they remain intact
without loss of hardness. According to Eisner, this alumed

plaster will stand immersion for several hours in boiling water
without its resistance being appreciably impaired.
Different explanations have been advanced to account for the

hardness of this plaster. Payen ascribed it to the formation of a
double salt of lime and potash, the crystals of which are enveloped
in a precipitate of alumina. Landrin, who examined several
specimens of alumed plaster such as are used for stucco work in

France and England, stated them all to be almost perfectly pure,
free from alumina and potash, and well baked ;
and he was led to
conclude that their slow rate of setting could only be ascribed to

chemical reaction set up between the aluminium and potassium
sulphates and the plaster, resulting in the conversion of all the

calcium carbonate into sulphate.
According to this view, the action of the alum is entirely due

to its sulphuric acid, and Landrin sought to verify this hypothesis
by reacting on plaster with a number of soluble sulphates, such as
those of sodium, potassium, ammonium, etc.
By restricting the additions to the quantity absolutely neces-
sary to saturate the calcium carbonate, he obtained about the same

results as with alum. He afterwards found that sulphuric acid by
itself is able to play the same part, and was thus led to a simple
and method of preparing alum or stucco plaster.

practical
This process consists in steeping the raw plaster for about i
5
minutes water containing 8 to 10 per cent, of sulphuric acid,

in
and then baking it in the ordinary manner. The stucco produced

in this way is not only of the best quality, but also, thanks to the
dissociation of a small excess of sulphuric acid, the organic matter
always present to a small extent in gypsum, is burned away,

so that the resulting plaster is of exceptional whiteness instead of
being grey like ordinary stucco.

Care must, however, be taken to heat the plaster sufficiently
to drive off all the free sulphuric acid, since the least trace of
residual acid will alter the properties of the product

by rendering
it moreover, the fritting temperature of the
very hygroscopic ;
plaster must not be exceeded. The best baking temperature

lies between 600 and 700 C.
After having demonstrated that the effect of alum on plaster
is solely due to the action of the sulphuric acid on the calcium
carbonate therein, Landrin investigated the retardive influence of
alum or sulphation on the setting of ordinary plaster, and put
forward the following explanation:
"
If it be admitted," he says, "that by baking gypsum at a
fairly high temperature the affinity of this body for water is
partly removed, immediate combination between the sulphated

plaster and water is prevented and, the chemical action being
;
very slow, the same will apply to the desiccation, and the
setting will be delayed. It is not until afterwards, when the
water has been partly dissipated into the atmosphere, that the
solution can become supersaturated and then only will the ;
plaster set hard."

If this explanation be accurate, one ought to be able to
cause the plaster to set at once by heating it gently when the

water has been added and this is precisely what does occur.
;
The same can be obtained by mixing slow-setting plaster

result
with ordinary plaster, the latter commencing to set and imparting

the same tendency to the rest of the mass. Again, by employing
hot water in making the plaster, the more rapid evaporation of
the liquid hastens the setting. Consequently the analogy
between the phenomena of setting in ordinary and sulphated
plaster is complete ;
the sole difference consists in the loss of
chemical affinity produced by an excess of warmth a difference
that is found at a maximum in the case of anhydrite, which will
not set with water at all (Knapp).
The alum plaster or stucco is chiefly employed for articles of
indoor decoration, on account of its hardness when set and its
resemblance to marble a likeness that can be heightened by

;
employing plaster of various shades to produce marbled effects.

In such event recourse is had to pigments :
minium, chrome
yellow, colcothar, terra di Sienna, lampblack, etc., added to the
water, mixed with glue, used in making the plaster. By placing
several layers of differently coloured plaster one above another a
mass of striped appearance in section can be obtained, which will
imitate the aspect of marble when applied so as to expose por-

tions of these different layers.
This class of stucco can also be polished.

138. Application to Lime Washes. The extent to which
lime washes are employed to coat the external surface of houses
in country districts is well known ;
and the same preparations
are also largely used for indoor work, particularly in stables, etc.
In addition to being cheap and enabling the appearance of walls
to be improved and their materials protected from the weather
at a small outlay, this method also exhibits the advantage of
disinfecting insanitary premises.

Lime wash, prepared by mixing fat lime and water, does not,
however, adhere very well to the surfaces to which it is applied,
and rapidly peels off. This inconvenience may be remedied by
the addition of a little alum at the time of use, the precipitate of
gelatinous alumina thus produced enveloping the particles of lime

and helping them to stick. The coating of lime is then much
more firm and durable than usual.
139. Application to the Preparation of Non-inflammable

Wood, Fabrics, etc. The extreme inflammability of the
materials used in building has led to many disastrous fires
notably that at the Charity Bazaar in Paris not very long ago ;
and many fatalities could undoubtedly have been prevented had
the fabrics and wood used in building been impregnated with

some metallic solution to render them less inflammable and
thereby prevent the rapid propagation of fire.
The use of alum for this purpose has often been recom-
mended, and the author's personal experience speaks in favour
of such a course, he having found that wood steeped for several
hours in a hot solution of alum becomes perfectly incombustible

after drying. And if we may give credence to the statements of
ancient writers, this salt was used for the same purpose at remote
periods, it
being recorded by Aulus Gellius that, during the siege
of Athens by Sylla, Archelaus constructed a wooden tower
which could not be set on fire, the wood having been impregnated
with alum.
140. Application to Bleaching. A bleaching preparation,

recommended by Orioli, is obtained by decomposing a solution
of chloride of lime with aluminium sulphate. The product being
very unstable, no acidis required. Its bleaching action is due to
decomposition into aluminium chloride and oxygen.

141. Application to Photography. Alum is the salt prin-
cipally used in this connection.

After developing, the (gelatino-bromide) plate is well washed,
and then immersed in a 5 per cent, alum bath, whereby the
pellicle hardens and loses its tendency to detach or wrinkle.
Plates that have turned yellow on exposure may be bleached by
5 minutes' immersion in a bath of
Water 1000 parts,

Alum 100 ,,
Hydrochloric acid . . . . 20 ,,
and can be then washed immediately and fixed.

The alum treatment is not indispensable, but is nevertheless
useful in preserving the plates.
142. Employment in Medicine. Here again alum is
mainly used. Calcined, it is employed as a caustic ;

in the
ordinary condition it serves for the preparation of certain
gargles, etc.
143. Application to the Purification of Waste Waters.

The waste waters from various industries, sewage water, etc.,
contain larger or smaller quantities of fats, organic and mineral
matters in solution or suspension, the more dangerous from a
sanitary point of view being the organic substances, since they
begin to putrefy after a while and contaminate the water-courses
into which they are discharged. The necessity of chemically
purifying these waste waters has long been recognised, and
aluminium sulphate is certainly one of the best agents to which

recourse has been had for this purpose.
When this product is added in small quantity to an alkaline
water, or one that has been rendered alkaline by lime, an
abundant gelatinous precipitate forms and carries down with
it all the matters present This precipitate is
in suspension.
aluminium hydrate, a body which, as we have already seen, has
a great affinity for certain organic matters in solution and forms
lakes with the same.
Aluminium sulphate has also been used for treating the
liquids furnished by various processes for dealing with sewage.

Thus in the Lencauchez process the liquids freed from am-
monia and boiled with an excess of lime are delivered into
decantation tanks, where they are treated with a small
quantity of aluminium sulphate (about 1

1 ozs. per cubic yard)
to facilitate the deposition of suspended matters and hasten

decantation.
In the Hennebutte and De Vaureal process the total sewage
is treated with aluminium sulphate (5 parts per mil.) and zinc
sulphate (2 to 3 parts per mil.), the mixture being left to settle
and the clear liquid afterwards decanted off and sent to the
ammonia recovery plant. The sediment is again treated with
the same 'reagent, and is delivered, by the aid of compressed air,
to a filter- press which furnishes firm cakes easily dried by

exposure to air and a clear liquid which is added to that first
obtained.
The addition of aluminium sulphate and zinc sulphate de-
sulphurises the matters present, and the gelatinous alumina

precipitate carries down the bodies held in suspension. The
cakes obtained in this way contain, when dry, 3 to 4 per cent,
of nitrogen and about 3 per cent, of phosphoric acid (C.
Vincent).
Alum is very well adapted for use in purifying waste liquors,
and may be obtained from the makers in a crude form, which is
just as good for this purpose as the commercial grades and far
less expensive. In use the alum crystals are put into a bag,
which is then placed in the channel through which the liquors to
be purified are discharged. The alum is thus gradually dissolved

and mixed with the flowing liquid, the resulting precipitate of
alumina carrying down the matters in suspension. The pre-
cipitate is collected in the settling tanks.
It is thus evident that the uses of alum and aluminium
sulphate are both numerous and extensive.
CHAPTER VI
USES AND APPLICATIONS OF FERROUS SULPHATE AND

FERRIC SULPHATES
I. USES OF FERROUS SULPHATE
144. Ferrous Sulphate in Dyeing. A. As A MORDANT.

Ferrous sulphate is known by the name of green vitriol and
green copperas, and is prepared in the manner already described.

Its uses as a mordant are somewhat limited.
(1) On Cotton. Ferrous sulphate is generally used to dull the

shades after dyeing. The cotton is boiled in a decoction of the
dye stuff, the excess of liquor being eliminated and the cold
ferrous sulphate solution then used. This method is only suitable
for light tints. A better plan is to impregnate the cotton with a
tannin principle and then immerse in ferrous sulphate solution :
for this process, however, ferric sulphate is to be preferred.

Ferrous sulphate is used in the same manner as ferric nitrate
for the production of chamois tints on cotton.
(2) On Wool. For this purpose ferrous sulphate has been
largely superseded by potassium bichromate, but is still used in
certain cases.
Wool may be mordanted by boiling in a suitable mixture of
ferrous sulphate and cream of tartar, a fairly large proportion of
the latter being required.
In certain cases (sandal-wood, etc.) it is better to boil the
wool first in a decoction of the dye until the greater portion of
the latter has been absorbed, the ferrous sulphate being then
added to the same liquor, or in a separate bath, in the proportions
of 5 to 8 per cent, of the weight of wool taken, boiling being
continued for | an hour or longer (Hummel and Dommer).
USES OF THE SULPHATES OF ALUMINIUM AND IRON 31 I
(3) On Si/k. Ferrous sulphate is not very much used in this
particular case. It is employed as a mordant in paper staining.

B. APPLICATION TO THE MANUFACTURE OF OTHER IRON
MORDANTS. Ferrous sulphate be utilised
in making ferrous
may
acetate, which is employed in dyeing and is
somewhat largely
prepared by double decomposition between ferrous sulphate and
lead acetate or calcium acetate. The method of treating ferrous
sulphate for the preparation of normal ferric sulphate or of rouil
mordant has already been described.
C. APPLICATION TO INDIGO DYEING. The principal method
FIG. 185. Indigo dyeing. Ferrous sulphate vat.
of indigo dyeing is based on the property of this pigment of

undergoing conversion, under the influence of reducing agents,
into indigo white- which is soluble in alkaline solutions, can be
fixed on the fibre, and then under the oxidising influence of the
air is transformed into insoluble indigotin firmly fixed on the
fibres.
The vats used in indigo dyeing may be classed, according to

the reducing agents employed, as ferrous sulphate vat, zinc vat,
and hydro-sulphite vat. These vats are mainly used in cotton
Our is confined to the ferrous sulphate vat, or,
attention
dyeing.
as it is
generally termed, the lime and copperas vat. These
vessels are rectangular in shape, and are constructed of wood,
stone, or cast-iron. The size varies according to the material to

be dyed.
For calico dyeing the usual size is 40 x 40 x 20 inches ;
for
hank dyeing they are made a little smaller. In order to
economise the indigo, the vats are arranged in series.
The bath liquor for dyeing calico consists of

Water
Crushed indigo
Ferrous sulphate
....
. . . .
880 gallons,
88 Ibs.
154 ,,
Quicklime 165 ,,
For yarn dyeing, proportions are

Water 165 gallons,
Indigo 8'8 Ibs.
Ferrous sulphate . . . . 1
5 '4 , ,
Quicklime 17 "6 ,,
The reactions in the bath are very simple : lime reacts on the
ferrous sulphate toform very unstable ferrous hydrate, which
latter, in presence of indigo, reacts on the water and is converted
into ferric hydrate, nascent hydrogen being liberated and im-
mediately reducing the indigotin to indigo white. This latter

then combines with the excess of lime and enters into solution.
The reaction may be expressed by the following equations :
(1) FeSO 4 +CaO+H = CaS0 4 +Fe(HO) 2

2 ,
(2) 2[Fe(HO) 8 ]+2H 2 O = Fe 2 O 3H 2 O + H 2 3> ,
(3) C 16 H 10 N 2 2 +H 2 = C 16 H 12 N 2 2
.
A freshly prepared vat can be considered in proper condition if
the liquid, on being stirred, exhibits numerous deep blue veins at

the surface, which is covered with a thick scum. The bath liquor
should be clear and of an amber-brown colour.
It makes little difference in what order the various substances
composing the bath are added, but it is highly necessary that
the ferrous sulphate should be as pure as possible. An excess
of this salt or of lime should be avoided.
At the end of the day's work the baths should be stirred up
vigorously, and should receive slight additions of lime or ferrous

sulphate according to their appearance.
Before dyeing, the scum should be taken off with a skimmer,
to prevent it spotting the stuff or yarn.
This bath mainly used for cotton. The fabric is first boiled
is
in water to enable it to take the dye uniformly.

For dyeing pale blue, only a few hanks are treated at a time,
and the operations must be conducted with the greatest regu-
larity ;
but such great precaution is unnecessary when dyeing
dark shades. The length of immersion varies from I to 5
minutes and more, according to the shade required ;
and after
wringing the hanks they are set aside to oxidise completely.

The most economical plan is to dye systematically, the cotton
being entered into the weakest baths first and afterwards into
progressively stronger ones until the desired shade is attained.
In this manner each bath becomes completely exhausted in turn.
After dyeing, the lime deposited on the fibre is removed by a
bath of sulphuric acid (density, roi to i'O2). This operation
removes the grey tinge and brightens the colour. A final wash-
ing is then given, but not too energetically, as otherwise the
indigo may partly run and the shade will be deficient in uni-
formity and intensity.

For dyeing calico, the piece goods in a dry state are suspended
on a square wooden frame and immersed in the bath for I 5 to
20 minutes they are then taken out of the bath and exposed to
;
the air for a similar period. The continuous machine of the kind
shown in Fig. 185 is often used for calico dyeing, the pieces
being passed over a series of rollers mounted on wooden frames
in the bath. On issuing from the bath the goods are passed
between wringers and then over other rollers on the outside,
where oxidation occurs, the operation being repeated several
times according to the shade required. The pieces are then
rinsed in pure water, then in dilute sulphuric acid, and are finally
washed and dried (Hummel and Dommer).
145. Application of Ferrous Sulphate to the Manufacture
of Pigments. A. PRUSSIAN BLUE. Prussian blue is a ferric
ferrocyanide
(Fe"Cy ) 3 (Fe/') 2 + 1 8H 2 O = Fe 7 Cy 18 + 1 8H 2 O.
,
It was discovered by accident as long ago as 1704, and was

prepared at Berlin by Diesbach, a colour maker, and Dippel, a
pharmacist, who kept their process a secret. The first process
3H USES OF THE SULPHATES OF ALUMINIUM AND IRON
for making this pigment on a large scale was described by

Woodward before the Royal Society of London in 1724.
Up to the present time the only known method of obtaining
Prussian blue of good quality is by precipitating ferrous sulphate
with ferrocyanide. The potassium ferrocyanide solution must be
run by degrees into the slightly acidified ferrous sulphate liquor,
the converse procedure being inadmissible owing to the retention,
in that case, of a large proportion of ferrocyanide by the pre-
cipitate.Furthermore, the washing from the precipitate should
be examined for traces of ferrocyanide (blue precipitate with
ferric salts).
The best proportions are
Ferrous sulphate 6 parts,

Potassium ferrocyanide 6 ,,
each dissolved in I
5 parts of water.
After mixing, an addition is made of I
part concentrated
sulphuric acid and 24 parts fuming hydrochloric acid. This
forms a white precipitate of ferropotassic ferrocyanide, which,
on oxidation, furnishes Prussian blue
6(FeCy 6 .Fe"K 2 )+30 = Fe 7 Cy 18 + 3 K 4 FeCy 6 +Fe 2 O 3 .
This precipitate can be oxidised either by contact with air or by

the action of nitric acid, chromic anhydride, chlorine, bleaching
chlorides, etc.
In the above-mentioned case a clarified solution of chloride
of lime is added, by degrees, several hours after the addition of
the sulphuric and hydrochloric acids. The precipitate is then
left for several hours, and afterwards washed and dried. It is
purified by digestion with hydrochloric acid followed by washing

with water. It has been already stated that a certain quantity
of alum is precipitated along with the ferrous sulphate in order to
improve the quality of the blue; consequently this need not be

further dilated upon.
B. MANUFACTURE OF MARS, OR MARTIAL, PIGMENTS.*-
These pigments are artificial ochres of handsomer colour than the
natural pigments they are used to replace.
*
So called from the ancient alchemical name of iron (namely Mars), e.g. martial pyrites.
(1) Mars Yellow. This is prepared by treating a pure solu-

tion of ferrous sulphate with sufficient milk of lime to completely
saturate the sulphuric acid. A precipitate of ferrous hydroxide

intimately mixed with calcium sulphate is formed, and this is
agitated in contact with air until the oxidation is complete. The

product is a yellow ochre of very pure shade and highly trans-
parent (Guignet).
When ammonia is used as a precipitant the product is darker
and less pure in tone.
(2) Mars Orange. This is obtained by moderately treating
ferrous sulphate, the products being basic ferric sulphates varying
in colour according to the temperature of calcination.

(3) The Capuchin Reds, Flesh
Colours, etc. used in painting on
porcelain may also be obtained in this manner. It is necessary
to wash these products thoroughly in order to remove the soluble
sulphuric acid.
(4) Mars obtained by calcining ferrous sulphate at a
Violet is
very high temperature. The pigment is very hard to grind, and

is somewhat dull, though very durable (Guignet).
C. Colcothar. This residueis obtained on decomposing ferrous
sulphate by heat in manufacture of fuming (Nordhausen)

the
sulphuric acid. It should be washed with great care in order to

remove all traces of sulphuric acid. The shade obtained varies
according to the calcination temperature employed.

146. Application to the Manufacture of Writing Inks.
A large number of recipes have been put forward for the pre-
paration of writing ink. This ink has a basis of iron tannate,
and entails the use of three principal materials, namely gall nuts,
gum, and ferrous sulphate.

The gall nuts (of the best quality) are crushed, I
part of the
product being infused for 24 hours in 14 parts of pure (preferably
distilled) water. It is then boiled for half an hour and filtered
through a cloth.
On the other hand, i part of gum arabic or Senegal gum is
dissolved in I
part of pure lukewarm water and added to the
decoction of gall nuts.
Finally, J part of pure ferrous sulphate is dissolved in I

part
of hot water, filtered, and run by degrees, with continued stirring,

into the previous mixture.
This ink turns very dark in time, but afterwards gradually

and assumes a yellow tinge.
loses its colour Ink made from gall
nuts rapidly becomes infested with mould fungi, a defect which
can be corrected by a small addition of phenic acid or salicylic
acid.
To convert this ink into copying ink, it is merely necessary to

add a little sugar and glycerin.
147. Employment in Microbiology; Staining the Cilia of
Bacteria. The vibratory cilia of the motile bacteria are difficult
to stain, and special methods have employed in order to

to be
facilitate their examination. One of the best methods is that of

Lceffler. When dried and fixed, the plates are subjected to the
action of a mordant bath composed as follows :
Cold saturated aqueous solution of ferrous sulphate . .

5 c.c.
Aqueous solution of tannin (20 grins, to 80 grms. of water) . 10 ,,
Saturated solution of fuchsine in absolute alcohol . . i ,,
They are then stained with a saturated solution of fuchsine in

aniline water.
148. Application to Photography. Ferrous sulphate has

been largely used in photography as a developer. On the one
hand, a solution is made of
(1) Potassium oxalate 250 grms.

Water 1000 ,,
and another of
(2) Ferrous sulphate .100 grms.

Water 300 ,,
Sulphuric acid 5 drops.
Solution No. i is stable and will keep indefinitely, but No. 2
solution oxidises in the air, and should only be prepared in small

quantities at a time.
For use, the ferrous sulphate solution is poured into the
oxalate solution and the plate is developed in the resulting bath.
It is advisable to add the ferrous solution in small quantities at a
time, and according to requirement, as revealed by the progress

in developing. For example, 80 c.c. of the oxalate solution are
measured into the dish, 2 5 c.c. of ferrous solution being measured

out, but only -il- added at first. The plate is then immersed, and,
according to the way the image comes up, the second or even
third portion of the solution is added afterwards.
149. Application to the Manufacture of Nordhausen Sul-

phuric Acid. This process will be dealt with in treating of
ferric sulphate, the raw material employed being a mixture
of ferrous sulphate, ferric sulphate, and aluminium sulphate
obtained by treating shale.
150. Application of Ferrous Sulphate for Disinfection.

Ferrous sulphate is, with justice, largely employed for disinfec-
tion. It is precipitated by ammoniacal and sulphide products,
which are thereby fixed. For example, with ammonium sulphide
the following reaction occurs :
FeS0 4 + (NH 4 ) S = (N H 4 ) 2 SO 4 + FeS.

2
It is also used in domestic hygiene for disinfecting cesspools,

etc., several pounds of the being thrown in at intervals.
salt
Again, it is employed for treating waste waters and sewage in

the manufacture of ammonia salts and fertiliser cakes, its action
being to destroy the sulphides and fix ammonia.

Ferrous sulphate has likewise been utilised for disinfecting
mud, street sweepings, and other decomposing material likely to
prove injurious to the public health.
Rabot's method has proved satisfactory wherever tried. It
consists in steeping the matters to be treated with a saturated
solution of ferrous sulphate at the rate of I Ib. per cubic yard,

and then covering them with double that quantity of milk of lime.
This method was adopted during the cleaning out of the Versailles
Canal and the lake at St. Mande.
151. Application in the Metallurgy of Gold. This applica-
tion is based on the precipitation of gold, in the metallic state, by
a solution of ferrous sulphate, a reaction also utilised in analysis.
The auriferous mineral is roasted and chlorinated, the gold being
converted into a soluble chloride. The mass is then extracted,
and the yellow liquor is treated with ferrous sulphate solution.
After several hours' repose the clear liquor, is drawn off and the
muddy precipitate of metallic gold is collected.
1 8 USES OF THE SULPHATES OF ALUMINIUM AND IRON
152. Application to the Purification of Lighting Gas.

The necessity for chemically purifying lighting gas has been
apparent ever since it began to be made and as soon as the gas ;
leaves the scrubbers it is treated to remove the tar. There,
FIG. 1 86. Laming purifier. Original form.
nevertheless, always remains a certain quantity of injurious or

malodorous gases, which cannot be got rid of except by chemical
reagents. These impurities comprise H 2
S ;
CO 2 ;
SO 2 ;
CN ;
HCNS; CS 2 ;
NH 3 ;
etc.
At first the gas was simply passed over slaked lime ;

but as
FIG. 187. Laming purifier. Present form.

Arrivee du gaz = gas inlet ; Sortie = gas outlet.
this gave but a very deficient purification, metallic solutions were

afterwards trjed, ferrous sulphate in particular. As the purifica-
tion still remained incomplete, and inconvenience arose through
the passing the gas through the liquid,
pressure produced in
further attempts were made, and finally the reagent known as
Laming' s was prepared, in which ferrous sulphate plays a principal
part. This is in the form of a powder containing ferrous sulphate,

calcium hydroxide, slaked lime, and sawdust, the first-named"
being dissolved, mixed with the slaked lime, and the product
thrown up into heaps in admixture with the sawdust.
The following reaction occurs :
FeSO 4 + Ca(HO) 2 = CaSO 4 + Fe(HO) 2 .
The mixture thus containing at first, Fe(HO) 2 CaSO 4 Ca(HO) 2 in , ,
excess, and sawdust. By exposure to air, the ferrous hydroxide

is converted into Fe 2 (HO) G Equal proportions of the ingredients
.
are taken to form the mixture, the result being that the quick-
lime is in excess.
This mixture is placed in the purifiers, which at one time were
made in the shape of boxes containing several layers of trays
charged with the mixture, intermediate spaces being left for the
circulation of the gas (Fig. 186).
At the present time the Laming mixture is used in the form
of a single layer 20 to 40 inches in thickness.
The apparatus consists of a large sheet-iron tank (Fig. 187),
12 to 24 feet square, set on the ground and provided with a gas-
inlet pipe projecting from below nearly to the top ;
another pipe,
leading from the bottom, serving to draw the gas away. The
mixture placed on a perforated
is false bottom fixed at a certain
distance from the real bottom of

the tank.
The purifiers are arranged in
sets, generally four, three of them

being always in use. The opera-
tion should be carried on system-
system of pipes being

atically, a
provided so that each purifier

can be put in communication
with any of the others in the
set. The arrangement is very FIG. 1 88. Distributor bell for a set of
simple,
.
111
all the pipes
IT
leading to
Laming purifiers,
or from the purifiers opening into a central tank filled with

water and containing a bell divided into compartments as shown
in diagram, Fig. 188 the central one receiving the gas from the
32O USES OF THE SULP?IATES OF ALUMINIUM AND IRON
scrubbers. To change the direction it is only necessary to turn

'the bell round through an angle of 45.
The first stage of the action of the Laming mixture is the
absorption of CO 2 by the lime, CaCO 3 being formed. The H 2 S
is readily absorbed by the Fe 2 (HO) G according ,
to the equation
The lime also absorbs the SO 2 present ; and, in addition,

forms Ca(CN) 2 with the cyanogen, and Ca(CNS) 2 with the
HCNS.
CS 2 is sparingly absorbed by the lime, but is taken up by cal-
cium sulphide, whereas a little H 2 S is

always fixed by the lime
CaO + H 2 S - CaS + H 2 O,
CaS + CS 2 = CaCS 3 ,
calcium sulphocarbonate being formed.

The ammonia is mainly in the form of carbonate, which, in
presence of CaSO 4 , gives CaCO 3 and (NH 4) 2 SO 4.
The gas is thus purified, but at the end of a certain time

the Laming mixture ceases to act, its composition then being a
mixture of CaCO 3 Fe(HO) 2
, , S, Ca(CN),, Ca(CNS) 2 CaS, ,
CaCS 3 ,
(NH S0 4)2 4.
It may, however, be regenerated, for which purpose it is taken

out of the purifiers, mixed with a little slaked lime, and exposed
to the air, whereby the Fe(HO) 2 is re-converted into Fe 2 (HO) c ,
and the mass ready is use

After a certain
for over again.
number of times the mixture gets into such a condition as to
be incapable of further regeneration, and must then be replaced
by a fresh batch.
The spent mass, which contains 30 to 45 per cent, of sulphur,
ammonia salts, and cyanides, is treated for the recovery of these
bodies.
153. The Uses of Ferrous Sulphate in Agriculture are
very numerous, and many of them highly interesting. The chief

of these will now be discussed, special mention being made of
one of the most recent, but most original, namely, the destruction
of wild mustard or charlock (sinapis arvense) in cultivated crops
by solutions of ferrous sulphate.

USES OF THE SULPHATES OF ALUMINIUM AND IRON 32 I
A. DESTRUCTION OF Moss IN PASTURE LAND. Damp

pastures are generally infested with moss, which hinders the
growth of grass and reduces the quantity and quality of the

forage. To destroy this moss, successful experiments have been
made by dressing the surface with about 300 to 500 Ibs. of
powdered ferrous sulphate per acre, applied by hand or in a drill.
The work is generally performed in the early spring, in damp
weather, before vegetation re-commences. February and March
are also suitable months.
A still more effectual method is to water the pasture with a
5 to io per cent, solution of the ferrous sulphate.

In about 8 or i o days the moss turns quite black, and should
then be broken up (by cross-harrowing, etc.), gathered in heaps
and carted away. Should the first treatment prove insufficient,
the work should be repeated without hesitation.
DESTRUCTION OF DODDER IN FODDER CROPS.
B. Ferrous
sulphate has yielded certain results in this case. The clover or

lucerne attacked by the parasite is mown close and watered with
ferrous sulphate solution, a 2 per cent, solution being sufficient if
applied as soon as the parasite appears ;

but if left later, the
strength must be increased to 3 to 4 per cent.

C. EMPLOYMENT IN TREATING CHLOROSIS, ANTHRACNOSE,
ETC., IN VINES AND FRUIT TREES. The distinctive signs of
chlorosis in vines and other plants are well known, and consist
in stoppage of growth, the leaves turning yellow, the twigs re-
maining thin and the plant stunted and barren. The causes are
still somewhat obscure. In some cases the disease has been
traced to poverty and lack of aeration of the soil ;
but generally
it is attributed to an excess of lime. Some plants are more
susceptible than others, but nevertheless the amount of damage
done to the vineyards by this complaint was very great until
Rassiguier discovered a simple and practical method of coping

with it, the means now generally employed and involving, in the
aggregate, the consumption of enormous quantities of ferrous
sulphate.
Rassiguier's method is perhaps best described in the words of
his contribution to the Bulletin de la Societe des Agriculteurs de

21
France (ist January 1896) on the treatment of chlorosis in vines
by washing with ferrous sulphate :
"
The treatment with ferrous sulphate, as an antidote to
chlorosis, which I invented in 1891 and tried on my own
property, has furnished such results that the method has spread,
and experience has taught its value to both scientists and prac-
tical wine-growers.
"
For the benefit of those who are still unacquainted with the
details of the matter, briefly review the conditions to be
I will
followed as to the time, method of operating, and quantity of
dressing to apply ;
and recount the influence of a single annual
'
washing on chlorosis, anthracnose and short node (court nouc}

'
in vines, fruit trees, and roses.

"
To produce the full effect, washing should be performed in
autumn, the vines most afflicted with chlorosis being treated
first, as soon as the first leaves begin to fall ;

in fact, I think that
such as are very much stunted should be treated before any of
the leaves come off. Both are washed immediately after each
stock has been pruned.
"
All the wounds made in pruning should, without exception,
be drenched with the ferruginous solution and, in order to ensure ;
the curing of the disease, the drenching should extend over the
whole surface of the trimmed shoots (not excepting the buds,
these being sufficiently protected by their downy envelope), the
branches, and even the stem, as will be explained below.
"
There is no need to be afraid of a more or less deep colora-
tion of the trimmed shoots, and if any of these insufficient!]
ripened, and therefore liable to perish should succumb to tl
washing process their place will shortly afterwards be found take

by vigorous buds beside or below the dead shoots which will
bear fruit the next year. All vines, well or diseased, may be
washed with advantage, as the treatment strengthens growth.
"
If postponed until the cold weather sets in, the washing
will have little effect, and spring washing is less efficacious
against chlorosis than autumn washing.

"
An active woman, armed with a wooden pail and a brush
or, better still, a woollen rag tied up in the shape of a brush
can wash after three pruners. During use the liquid should be
stirred up at intervals to keep it fairly uniform in density. The
solution should be a saturated one, i.e.
containing 40 to 45 per
cent, of ferrous sulphate, and may be prepared
very simple in a
manner by placing 80 to 90 Ibs. of ferrous sulphate in a wicker

basket slung on a stick through the handle, and thus suspended
in a vessel large enough to hold 200 gallons of water without
overflowing when the basket is immersed. After leaving over

night the sulphate will be dissolved and the liquor ready for use
by next day.
"
Generally the results of the treatment are remarkably bene-
ficial, and in many places a complete cure is effected the first
year. However, some soils are less favourable to viticulture and
require the treatment to be repeated. Chlorosis has also been

cured in fruit and rose trees by washing the pruned surfaces with
the same solution.
"
Moreover, when the dressing is applied over the entire
surface of the stock, it is capable of destroying the germs of
oi'dium, anthracnose, mildew, and insects lodged in the interstices
of the bark.
"
Three years' consecutive treatment of my own vines cured
the stocks suffering from short node, i.e. those where the nodes
on the sickly branches were only a few centimetres apart. These
formerly unproductive stocks now yield a large crop, and the
internodes are of ordinary length.
"
First year's grafts may be treated with a 20 to 30 per cent.
solution, the fulldose being repeated the third or fourth year.
"
Thus all the foregoing maladies are curable by a single
annual operation.
"
I recommend the primer to cut through the middle of the
bud just above the one destined to bear fruit, so as to leave
intact the protecting septum existing at this point, and which,
when cauterised at the surface by the action of the ferrous
sulphate, preserves adjacent internode from the effects of

the
frost, insects, or wet, which might otherwise penetrate the pith :
this internode remaining healthy, the fruit bud will be rendered
more vigorous."
324 USES OF T-HE SULPHATES OF ALUMINIUM AND. IRON
The importance and value of this method is confirmed by the
report drawn up by M. Guillon (teacher of Viticulture at the

National Agricultural School, Montpellier) on the experiments
instigated by the Herault Agricultural Society with reference to

the treatment of chlorosis.
"I. At present, without taking into consideration the lime-
resisting properties of the grape stocks, the best and most
efficacious preventive against chlorosis of the vine is a thorough
washing of the stocks with ferrous sulphate by the Rassiguier

process.
"
2. Ammoniacal iron citrate also restores stocks afflicted with
chlorosis; but in addition to the fact that the action of this

salt is unknown in the case of certain maladies curable by
ferrous sulphate it is much too dear for its employment to be
advocated.
"
3. The best results ensue when the washing is performed at
the time the leaves are beginning to fall, i.e. end October to
early November in the south. Spring washing produces less
decided results.
"
4. The application of ferrous sulphate to the pruning cuts
alone is nearly as efficacious as when the whole stock is dressed,
which shows the importance of not neglecting these cuts when
applying the dressing.
"
5. The ferrous sulphate solution should be of 40 to 50 per
cent, strength.
"
6. In vines badly afflicted with chlorosis the remedy is not
always completely successful the first year, and, even if apparently

so, it is advisable to repeat the process for several seasons."
The action of ferrous sulphate in the treatment of chlorosis
is somewhat difficult to explain. According to Coste-Floret,
however
"
The buds and wood still continue to grow after the leaves
have fallen ;
and the only way in which the plant can now
procure the carbon dioxide necessary to its growth which
though small is continuous is by decomposing the carbonates
in the sap, and it is at this moment that the accumulation of
lime salts increases in the young wood to such an extent as

to endanger the previous year's growth. This being so, the
Rassiguier process is readily explained, namely, the ferrous
sulphate acts by paralysing the cells still active at the end of

the season, and, by retarding this slow continuous vegetation
subsequent to the fall of the leaf, it prevents the gradual and
dangerous accumulation of lime salts in the plant. This is the
reason why the process is not thoroughly efficacious except
when applied immediately the leaves have fallen, because later
on the mischief will have been already done."
Sahut recommends the following formula as a preventive
against anthracnose :
Ferrous sulphate
Copper ,,
...... 20
12
parts,
,,
Fat lime 6 , ,
Water 100 ,,
Ferrous sulphate has also been recommended as a remedy
against fruit dropping off, when due to mildew. Coudercq found

the best results were obtained by spraying during the winter with
a solution containing 3 per cent, of ferrous sulphate and 5 per
cent, of
copper sulphate, or the latter salt by itself.
At the beginning of winter, and again in January, it is well to
wash the trunks and branches of fruit trees with a 20 per cent,
solution of ferrous sulphate in order to destroy insects and their
eggs, flies, and moss.

As a remedy for canker, Prillieux advises excision of the
diseased portions and washing with a 10 per cent, solution of

ferrous sulphate. It is also well to scatter about 2 pounds of
the powdered salt about the foot of each tree, for a distance
varying with the size of the trees.

Ferrous sulphate has also been used as an insecticide, and
employed, with more or less success, against aphides, caterpillars,

etc. Again, G. Croquevieille recommends it for treating oi'dium,
mildew, black rot, etc. in the vine, and ergot, anthracnose, caries,
etc. incereals but, in the author's opinion, it is pushing matters
;
to extremes to claim universal curative powers for ferrous sul-

phate, as such a course will probably only lead to disappointment
in a number of cases.
D. DESTRUCTION OF CRUCIFEROUS WEEDS. These chiefly
belong to the Raphanus and Sinapis species the first-named, ;
which is rare, being represented by only a single variety, namely

the wild radish (Raphanus RapJianistruin, L.), a plant 4 to 8
inches in height, bearing white blossoms veined with brown or
violet, and an elongated fruit which divides, when ripe, into
portions containing only a single seed each.

The mustard tribe is more general, three varieties being found,
namely white {Sinapis alba), black {Sinapis nigrd}> and wild
FIG. 189. Portable spraying apparatus.
R, Receiver ; A, bottom wall traversed by the pump P ; D, circular rubber diaphragm

acting as piston ; J, metallic joint supporting D
; E, piston rod connected to the
diaphragm by two D
convex discs 1 , and actuated from the shaft B ; C, handle for
working the shaft B and pump ; l>, l>, apertures admitting liquid to the pump, and
closed by discs during the compression of the diaphragm I, orifice admitting the
;
liquid in the pump to the air chamber in P, closed during the back stroke of the
diaphragm ; K, discharge pipe.
mustard (Sinapis arvense), all of which bear yellow flowers, and

vary in height from 8 to 48 inches.
Apart from these types there are numerous hybrids of
variable height and ramification, with yellow flowers more or less
bright in colour.
All these plants produce large quantities of seeds that
germinate readily. In some years they invade cereal crops so
rapidly, and their growth is so luxuriant, that the wheat, oats, etc.
are stifled and killed, or at any rate greatly enfeebled, the great loss
caused by these weeds making them greatly dreaded by the farmer.
Weeding being a very expensive task, other means of

eradicating these pests have been sought. Topping is the one
generally pursued, but this is attended by the disadvantage of
leaving the bulk of the plant intact; consequently the recent

discovery of a rapid, simple, and cheap method of totally destroy-
ing the weeds was readily welcomed by farmers.
Copper sulphate was first used, in the condition of a 5 per cent,

solution, applied, at the rate of 100 to 150 gallons per acre of
by a spraying engine similar to those generally
the infested area,
used for copper solutions. This liquor destroys the cruciferous
weeds, and leaves the cereal plants intact, their glaucous surface,
with its thin overlying layer of fat, preventing them from being
wetted by liquids. The copper solution therefore merely runs
FIG. 190. Spraying engine.
down the leaves of the cereals and falls to the ground without
any injury. On the other hand,
the leaves, stems,
doing them
in the
and flowers of the cruciferous weeds are unprotected
described manner, and consequently the copper solution adheres
to their surface and acts as a caustic poison. couple of days A
after spraying, the weeds look as though scorched,
turn yellow,
and commence to shrivel up and in about a fortnight they will

;
have entirely disappeared, leaving the cereals growing with vigour.

Copper sulphate being dear, especially for small consumers,
cheap substitute was sought
in
who buy only a little at a time, a
to 20 per cent.)
ferroussulphate. True, a stronger solution (15
with the
of the latter is required to produce the same effect
above-named volume of dressing per acre but the treatment is
;
thoroughly effective, and, in view of the lower price of ferrous

sulphate, expensive than the copper sulphate method.
is less
The action of the two salts is not quite the same, ferrous sulphate
acting mainly as a caustic, being transformed into a strong
oxidising agent, ferric sulphate, in the tissues of the impregnated
plants.
The difference in action is shown by the appearance of
magnified sections of treated plants. Thus with copper sulphate
there is hardly any exterior zone of dissociation, the epidermis
remaining just as distinct as if no treatment had taken place.

Only the cell contents have been altered, the protoplasm having
contracted and adhered to the cell walls, although the section be
taken from a green undried plant.
still
On the other hand, with ferrous sulphate, besides the
coagulation of the protoplasm, there appears around the edge

of the section where the plant has come in contact with the
solution a brown zone wherein the detailed structure is no
longer perceptible. This zone has a scorched look, and extends
more or less towards the centre.
In any event, the weed
is' destroyed the main thing this
having been placed beyond doubt by the experiments made by

the author and M. Vivien of St. Quentin. Other weeds, such as
thistles, camomile, though rather more resistant, are also destroyed
or greatly damaged.
The treatment should be applied when the cruciferae have put
forth their first leaves, though good results are still obtained
during the flowering time.

This is a very important application of ferrous sulphate.
E. PRESERVATION OF STALL MANURE. It has been pro-
posed to employ ferrous sulphate to fix the ammonia in stall
manure, and thus prevent the losses always occurring in manure

heaps. Theoretically this should act all right, but in practice the
result is the formation of a mixture of excrement and litter,
which does not constitute stall manure.

F. FERROUS SULPHATE AS A FERTILIS-ER. Iron, in various
stages of oxidation, is found in most arable soils, and is the cause

of their brown or reddish colour. It is also found, though in
very small proportion, in the ash of most cultivated plants ;

the
following table, compiled by P. Gontier, showing the weight of

ferric oxide per acre removed from the soil by different crops :
An examination of the table shows that the iron is localised
rather in the herbaceous parts than in the seeds. Nevertheless, it
is none the less of great utility in plant life, as was shown by the
labours of E. Gris in 1840, Knop in 1859, Dr. Sachs in 1860,
and Boussingault in 1872.
The part played by this substance in vegetation has been
mainly established by the researches of Dr. Griffiths, who carried
out a large number of culture experiments with iron sulphate and
phosphate, from which he drew the conclusion that not only do

ferruginous manures increase the yield of most crops, but that
they also exert manifest influence on the quality, particularly as
concerns the increase of the albuminoids, carbohydrates, and fats,
at the expense of water and fibre. Two examples referring to
potatoes and beet are given below.

It results from experiments made by the same author that
ferruginous manures in excess have an unfavourable influence on
vegetation, and even a decided sterilising action.
The classes of soil requiring iron are, in the first place, all
such as are deficient in organic matter, since, even if these soils
contain sufficient quantities of iron, the latter would probably be
33O USES OF THE SULPHATES OF ALUMINIUM AND IRON
inassimilable ; secondly, siliceous soils containing iron in the

condition of sparingly assimilable silicate ;
and thirdly, calcareous
soils.
For manurial purposes iron may be employed in the form of

a compost of lime and ferrous sulphate, previously oxidised by
aeration. To prepare this compost, the ferrous sulphate is dis-
solved in water, and the lime is added in powder, i

part of
slaked lime being taken to 2 parts of ferrous sulphate.
The dissolved salt is converted into an ochreous pulp, with
which the remainder of the lime is then mixed. Ferrous sulphate
may be also used by itself, in quantities from 50 to 200 Ibs.
per acre, according to the class of soil for sandy soils from 50 to:
I oo Ibs. is advisable, but for calcareous soils a

larger quantity may
be taken. Uniform distribution being desirable, it is a good plan
to mix the fertiliser with soil or sand previous to sowing.
The dressing should be applied in the autumn, preferably on
a warm day, immediately after rain ;
in default of rain, the best
plan is to work after a good watering or on a dull day, the

dressing being applied in nearly equal portions.
Great importance is attached to the conditions in which the
ferrous sulphate is applied, and lack of care in this respect may
lead to failure. A negative result will certainly follow if the salt
be not sufficiently pulverised, if it be applied in dry weather, or if
the temperature be too low, E. Grieg having found in his experi-
ments that no effect ensues when the temperature is below 10 C.
(A. Larbaletrier).
Ferrous sulphate is very frequently used in admixture with
other substances, as a compound manure for pot and ornamental
USES OF THE SULPHATES OF ALUMINIUM AND IRON 33!
plants in the garden or the house. For foliage plants the follow-
ing mixture may be used :
Sodium nitrate 3 parts,

Superphosphate . . . . . . .
4 ,,
Potassium chloride I
part,
Calcium sulphate 4 parts,
Ferrous sulphate . . . . . . . 2 , ,
applied at the rate of about I o ozs. per square yard.
For flowering plants the proportions are as follows :
Sodium nitrate 2 parts,
Superphosphate 10 ,,
Potassium chloride 2 ,,
Calcium sulphate . . . . . . .
4 ,,
Ferrous sulphate . . 2 , ,
applied at the same rate as above.
2. APPLICATIONS OF FERRIC SULPHATE

i
54. Dyeing. A. COTTON DYEING. Normal ferric sulphate
is but -very little used in cotton dyeing, the principal mordant
employed, particularly for dyeing blacks, being the basic sulphate
(rouil), the preparation of which has already been described.

The fabric is first entered in a cold bath of tannin material,
and is then, or after passage through lime water, immersed for an
hour in a bath of iron mordant diluted to a density of I'oi to
i'O2. The material is then washed, either in ordinary water
or water rendered alkaline by powdered chalk, in order to
in
complete the precipitation of the basic salt on the fibre and

to remove all traces of acid. The cotton is then dyed in a bath
of campeachy.
In this operation the tannic acid, which is attracted by the
cotton, mainly serves to fix the iron mordant, although incidentally
it
produces a bluish-black (inky) colour by combining with the
ferric salt.
The passage through milk of lime after the tannin bath
evidently causes the formation of calcium tannate, and the lime

by taking part in the reaction facilitates the decomposition of the
ferric salt.
This iron mordant may also be employed for dyeing chamois

iron colours, for which the normal sulphate is still used (Hummel
and Dommer).
B. WOOL DYEING. Ferric sulphates are not generally used
for mordanting wool, although they might be if properly applied.
C. SILK DYEING. In this, again, the basic sulphate (rouif)
is the most frequently used, the silk being mordanted in the con-
dition of grege or as boiled silk. To mordant grege, the silk is
first entered in a lukewarm bath (40 to 5oC.) of sodium car-

bonate. It is then washed, wrung, and entered into a cold
solution of the mordant, diluted to a density of ro75, where it
is worked for 30 minutes to an hour, then drained, wrung,
FIG. 191. Mordanting silk.
washed, wrung again and worked for an hour -J- in a lukewarm

bath of Na 2 CO 3 followed by wringing and washing.
,
These opera-
tions are repeated 3 or 4 times according to the object in view.
For boiled silk the material is worked for 30 to 60 minutes

in a solution of the mordant (density, 1*25). After rinsing it is
washed, first in cold water, then in hot. These operations are

repeated 7 or 8 times, the silk is afterwards boiled in an old soap
bath, the soap used being generally the same as employed for
boiling the silk, plus the addition of I 2 parts of soft (olein) soap
and 2 parts of soda crystals per I oo parts of silk. This soaping
is continued at 100 for an hour in order to obtain a maximum
fixing effect.
The mordanting is completed by a final washing. It being

essential that silk mordanted with rouil should not be allowed to
dry, the material must either be left in the mordant or else

covered with damp cloths after washing.
Silk impregnated with ferric oxide gradually perishes if left
in that condition, owing to the slow oxidation of the fibre. The

differences in the method of fixing rouil mordant in these two
kinds of silk are theoretical as well as practicable.
In the case of grege silk, for which a comparatively weak

solution of mordantemployed, the grege itself causes the
is
decomposition and precipitation of an insoluble basic salt within
FIG. 192. Washer employed for silk.
its own mass, fixation being completed by the washing and the
rinsing in Na" 2 CO 3.
In the case of boiled silk, the fibre merely absorbs the mordant
solution, and there is no decomposition or precipitation of basic salt
until the solution is diluted by washing. The use of water con-
taining calcium bicarbonate facilitates the fixing of the absorbed

mordant, and the operation is completed by boiling in a soap bath.
Mordanted in this manner, the silk has a deep orange-brown

colour and an improved lustre. The weight is increased 4 per
cent, by a single mordant and 25 per cent, after six operations.
After seven or eight repetitions there is a gain of about 8 per

cent,on the original weight of grege silk.
The apparatus employed for mordanting silks is very simple,

and consists of a rectangular vat to hold the mordant, the silk
being hung on rods which are worked by hand in the bath

(Fig. 191).After draining, the excess of liquid is removed by
passing the hanks through a wringing machine.

For washing, the machine shown in Fig. 192 is
employed.
This contains a double row of glazed, fluted porcelain bobbins on
which the hanks of silk are suspended and worked. The washing
is effected by means of perforated pipes placed laterally under-
neath and between the bobbins (Hummel and Dommer).

D. USES OF FERRIC NITRO-SULPHATES. These mordants
are known as nitrates of iron, and are prepared by oxidising
ferrous sulphate with nitric acid, which entirely or partly replaces
the sulphuric acid. Their principal application is in dyeing cotton
black, and they are used in the same manner as the ferric
sulphates.
E. APPLICATION OF IRON ALUM, FE 2 (SO 4 ) 3 ,
K SO 24H
2 4, 2 O.
This salt may be employed in the same manner as ordinary
alum. Up to the present it has not been very largely used, its
sole application being for mordanting wool previous to dyeing

with alizarine colours (Hummel and Dommer).
155. Ferric Sulphate as a Disinfectant and Antiseptic.
A. INTRODUCTION. The utilisation of the disinfectant and
antiseptic properties of ferric sulphate forms one of the most
important applications of this salt. The matter was investigated
some twenty years back by Rohart, but we are indebted to
Messrs. Buisine, of Lille, for the main of our knowledge on the
subject ;
these last-named workers having devised the already
described method of preparing the salt, namely that pursued in
the Kuhlmann works at Lille.
Ferric sulphate forms with animal organic matter certain

insoluble, non-putrefactive compounds of high stability, which are
precipitated from solution and protected from subsequent decom-

position under the action of air.
Urea, uric acid, mucus, gelatin, and albuminoids in fact, all
nitrogenous organic matters are precipitated as non-putrefactive
compounds.
When treated with ferric sulphate, fresh urine gives a precipi-

tate containing nearly all the nitrogen and phosphoric acid, and the
clear liquid will keep for a very long time without decomposing.
Human egesta, solid and liquid, can be preserved free from
any trace of fermentation or liberation of gas by treatment with

this reagent.
Animal remains, viscera, etc., will keep unchanged if im-

mersed for some days in a I
per cent, solution of ferric sulphate,
and then washed and dried in the air.
In the same manner, small animals can be mummified whole,

the flesh preserving its colour but being hardened to such a
degree that it can with difficulty be scraped with the finger-nail.
In fact, in the presence of animal matters, ferric sulphate behaves
exactly like tannin and prevents putrefaction.

The foregoing results show the extent to which ferric sulphate
modifies the character of organic substances, and the energy with

which it retards or opposes putrefactive fermentation in fact, the
whole of its value as an antiseptic.

Its disinfectant properties are also easily explained. The
action of ferric sulphate on solid organic matter has just been
described ;
and this action is equally complete in the case of
organic matters in solution, e.g. albuminoids, these being pre-
cipitated in the form of unalterable, non-putrefactive compounds
of ferric oxide. Moreover, in the case of liquids on the way to
putrefaction, ferric sulphate eliminates the decomposition products,
especially sulphuretted hydrogen,ammonia, etc., the former being

thrown down as iron sulphide, and the ammonia fixed as am-
monium sulphate, so that all odour is entirely dissipated.
The organised germs themselves are enveloped in the pre-
cipitate of ferric oxide, and are to a large extent carried down
in the deposit and rendered innocuous the importance of which
fact will be admitted.
Thus, presence of certain substances,
in
ferricsulphate behaves as an oxidising agent, the ferric oxide

being reduced to ferrous oxide, which rapidly absorbs oxygen
from the air. In view of these properties, ferric sulphate is
suitable for a variety of uses.
B. DISINFECTING CESSPOOLS. For this purpose ferric

sulphate may advantageously replace the zinc chloride, copper

sulphate, and ferrous sulphate generally used. It is employed,
in a powdered condition, at the rate of 4 to 8 Ibs. per cubic yard.
C. TREATMENT OF WASTE SEWAGE WATER. This reagent
is employed in several works for treating waste sewage water,
the addition of ferric sulphate deodorising the liquid and giving
an abundant precipitate, which, when treated in a filter-press,
furnishes cakes rich in nitrogen.
D. DISINFECTING URINALS, BARRACKS, HOSPITALS, AND

INSALUBRIOUS PREMISES. Sprinkled about in powder, ferric
sulphate is a very useful disinfectant for places where human or
other egesta are deposited, such as urinals, cesspools in public

conveniences, railway stations, schools, barracks, hospitals, prisons,
etc. The usual dressing is at the rate of 3 to 6 ozs. per square
yard of surface covered.

In time of epidemic this salt should be used in the state of a
dilute solution for watering the streets and gutters of insalubrious
districts.
For hospital use itshould be employed not only in the cess-
pools, but also in the washing water, ventilation pipes, bed-pans,

spittoons, etc.
In works where insalubrious trades are practised, and wherever
unstable organic matters are treated such as tallow melting, for
example ferric sulphate may be used to disinfect the raw materials
employed. It is also very useful in cleansing establishments like

breweries, distilleries, etc., where great care has to be devoted to
the destruction of putrefactive germs. For stables, etc., a i

per
cent, solution is suitable for swilling the place down. For medical
operating theatres and dissecting rooms, ferric sulphate is free
from the dangers attending mercury dichloride.

For household use it may be advantageously placed in the
drains removing waste waters, etc. liable to putrefaction, the
briquette form being very useful for this purpose.

E. PRESERVING ANATOMICAL SPECIMENS. As Messrs.
Buisine have shown, ferric sulphate may be used for preserving
anatomical specimens, and for enabling putrescent specimens to

be handled without danger. Similarly, the dead bodies of animals
killed by infectious diseases should be covered with this salt at
the time of burial.

F. DISINFECTING MUD, SWEEPINGS, ETC. Ferric sulphate
is good for this purpose as ferrous sulphate, which has
just as
already been mentioned in this connection.

G. COAGULATING BLOOD. Normal ferric sulphate can be
used for coagulating blood, but it is preferable to employ a
concentrated solution strongly acidified with sulphuric acid. A
very suitable solution is met with in commerce under the name
of coagulant, which has already been mentioned in dealing with
the preparation of rouil mordant.
The method of application is very simple, the coagulant being
poured on to the blood and the whole intimately mixed
in a vat
by stirring. A pasty mass forms directly, and may be filtered in

a press or spread out on the ground to drain. The resulting
cakes contain about 12 per cent, of nitrogen and 1*5 per cent, of
phosphoric acid, and are therefore of considerable commercial

value. The quantity of coagulant used is I volume to 20 of
blood.
H. MIXTURES OF FERRIC SULPHATE AND OTHER ANTI-
SEPTICS. We have seen that ferric sulphate prepared by the
Buisine process sets like plaster when mixed with a small quantity
of water, a property which may be utilised for making briquettes
containing any other known antiseptics, such as salts of copper,

zinc, mercury, or potassium permanganate, phenol, etc.
With phenol, for example, the manufacture is very simple, the
phenol being emulsified water required for treating the

in the
ferricsulphate. The
resulting paste is then cast into moulds,
where it sets rapidly and forms hard briquettes, the constituents of
which dissolve slowly when brought in contact with water. The
association of ferric sulphate with phenol forms a powerful disin-
fectant capable of rendering great service, especially in hospitals.
In fact, this is the best and most convenient method of utilising
phenol for this

purpose.
These examples could be multiplied, but are sufficient to
illustrate the interest attaching to ferric sulphate as a disinfectant

and antiseptic.
156. Purifying Waste Liquors, Drainage Waters, etc.

For this purpose ferric sulphate forms an excellent reagent,
conclusive results having been obtained from the experiments on
the water of the river Espierre which receives the drainage
of the towns of Roubaix
and Tourcoing carried out by the
French Government Department of Roads and Bridges at the
Grimontpont works. The degree of impurity of the liquid there
treated will be evident from the subjoined analyses :
*
This sample was taken on a Sunday when the factories were not working.
N.B. These analyses are taken from the report of the committee on purifying the
water of the Espierre (1881).
The following table, cited by Buisine, shows the excellent

results of treating the above water with ferric sulphate :
Espierre Water, 2\st April 1892.

The average composition of the air-dry purification sediment
furnished by the ferric sulphate from Espierre water at the
Grimontpont works was

Water 20*90
Mineral matter (sand, clay, ferric oxide) . .
3O'63
Fat 30-00
Nitrogenous organic matter i8'47
Total . . . loo'oo
The fat is derived from the numerous wool-combing works

inRoubaix and Tourcoing, or from the household waste thrown
down the drains, and is therefore different from wool fat (suinf}.
It maybe extracted from the sediment by means of carbon di-
sulphide,and purified by distillation with superheated steam,
followed by fractionation into a series of products utilisable
partly in stearine manufacture, partly for soap-making, and partly

as lubricants.
The residue left after extraction contains-
Ferric oxide
Clay, sand, etc. .......

Nitrogenous organic matter (containing N 2 '92
25 '35
37 '05
per cent.) 37 '60
and thus forms a fairly nitrogenous poudrette highly useful as an

agricultural fertiliser.
Ferric sulphate has been applied, with equal success, to a
large number of waste waters from manufacturing processes, and
may be particularly recommended for purifying those of starcli
factories, distilleries, sugar works, breweries, yeast factories, glue
works, gelatine works, paper works, dye works, tanneries, wool-

washing factories, slaughter-houses, etc., etc.
The modus operandi is very simple, and consists in stirring
into the water to be treated sufficient ferric sulphate solution to
ensure the complete and rapid deposition of the resulting pre-
cipitate. After settling, the clear liquors are run off, and the
residue is removed for use as manure on account of its nitrogen.
The ferric sulphate is dissolved in 5 or 6 times its own
weight of water in a wooden vat, and heated by steam blown in
through a leaden pipe. When as much as possible has been

dissolved, more water is added to bring the solution down to
10 per cent, strength.

For the preliminary tests the solution may be prepared from
loo grms. of the salt in a I -litre flask.
The next point is to determine how much of the solution

should be added to the water under treatment.
For this purpose three I -litre samples are taken, one being
treated with 5 c.c. of the ferric sulphate solution, the second
with 10 c.c., and the third with I
5 c.c. All are then stirred, and
note taken which precipitates the best, the result showing
is
whether |, I, or i| kilos, of ferric sulphate is required per cubic

metre of the water.
Usually, the fact of the nitrate draining easily and free from
smell indicates that sufficient ferric sulphate has been employed.
The quantity and method of application depend on the position
of the works, and on the nature and volume of water to be
purified, but the following figures will serve as a general
guide :
Waste water from starch works . . 2-10 Ibs. per cub. yard,
Red water from starch works . . 2-6 , , , ,
Water from distilleries . . .

4-8 ,, ,,
,,
, ,
wool-washing
breweries .... . . .
4-6
4-6
,,
, ,
,,
, ,
In the case of waters with an acid reaction, such as those

from distilleries, dye works, etc., they must be neutralised with
lime before the ferric sulphate isadded. On the other hand,
alkaline or neutral water (from starch works, wool-washing, sugar
works, breweries, paper works, glue works, etc.) can be treated

with the ferric sulphate at once.
If the works be situated in a town and have no open space
available in the vicinity, the waste waters may be run into a
masonry reservoir, where they are agitated by suitable means and,

after the addition of the necessary amount of ferric sulphate, are
immediately passed through a filter-press.
Wool-washing liquor may furnish, per 22,000 gallons (100

cubic metres), about 450 to 650 Ibs. of dry residues, which, on
issuing from the filter-press, contain 60 to 65 per cent, of moisture,

and occupy a volume of 2 5 to 35 cubic feet.
Some of the precipitates are very difficult to filter in the press,

and such case only very thin cakes can be made. Before going
in
to the expense of setting up a filter-press, experiments should be
made to see whether this artificial aid is of any use. When the
works has vacant land near by, settling basins may be made by
digging out shallow pits of about 1000 square feet area and
16 to 20 inches deep, the excavated earth being banked up about
40 inches high all round so as to form basins 60 inches in depth.
In addition to this there should be a masonry tank, large enough
to collect one day's waste, at the works, from which tank ,the
liquid can be raised in 2 to 3 hours and delivered through a cast-

iron main, or, better still, suspended wooden troughs, to the
settling basins. The latter can then be at some distance from
the works.
A small pipe from the ferric sulphate tank can be led into
the suction pipe of the pump and the outflow regulated by a tap
so that the solution tank and the collecting tank will be discharged
together. In this way the pump acts as a mixer, and the water
is discharged into the settling basins, where the precipitate will
come down in a single night, so that the clarified water is run off
every morning and the basin filled with a fresh supply.

After about 20 operations the sediment will have attained
a depth of I 6 to 20 inches, the liquid is run into another basin,
and the sediment drained by means of gutters. When the mud
has thickened to a certain extent it is gradually shovelled out
and spread on and round the banks, where it dries and can then
be removed for use as manure.
In summer-time a couple of these basins, large enough to hold
a day's output in addition to the sediment, will be enough but ;
in winter, when drying is more difficult, a larger number will be
required.
In view of the necessity of shovelling the sediment on to the
it will save labour if the basins are made long
banks to dry, and
narrow.
The may also be pumped into a series of basins in
liquid
communication with one another, in which event, if the traverse
will run out clear from the end

is sufficiently long, the liquid
basin. In this case only a small centrifugal or other continuous
pump will be required.

The cost of purifying with ferric sulphate is very low, this
product being obtainable at 2s. to 33. per cwt.
3. APPLICATIONS OF MIXTURES OF IRON AND ALUMINIUM

SULPHATES
157. Manufacture of Fuming or Nordhausen Sulphuric

Acid. A. INTRODUCTION. Sulphuric acid was first prepared
by calcining ferrous sulphate or green vitriol, hence its name oil
FIG. 193. Gallery furnaces for the manufacture of Nordhausen

sulphuric acid.
of vitriol; and this process is still carried on for certain special
purposes. The acid so obtained is in a highly concentrated state,

and represents a solution of sulphur trioxide in 66 Be. sulphuric
acid it is used in the manufacture of certain varnishes, for dis-
;
solving indigo, and in the alizarine colour industry.

Formerly the manufacture of this acid was concentrated at
Nordhausen in the Harz District, whence its name but after- ;
wards large works were established in Bohemia by J. D. Starck.

The production of this substance is intimately connected with
that of the green vitriol extracted from pyritic shale.
B. MANUFACTURE. (i) Preparation of Vitriol Stone. The
crude material is furnished by Prziban shales belonging to the
Silurian formation, which are scattered about in small aggrega-

tions in the pits of clay shale. Only such as are bituminous and
contain from I to 20 per cent, of pyrites are used.
The mineral is first concentrated by levigation. Formerly

it was preferred to calcine the pyritic shale in contact with air in
earthenware retorts. In this manner from 12 to 14 per cent, of
sulphur, suitable for purposes, was obtained, and the

different
residue was already partly decomposed. Later, however, it was

desired to utilise the whole of the sulphur for the special object in
view, and for this purpose the mineral was spread on an im-
pervious flooring and exposed to the action of air and moisture for
several years, thus oxidising the pyrites and producing sulphates
of iron and aluminium (see Chapter IV., 2).
When sufficiently oxidised the heaps are sprinkled with water,
and the liquor is drained into large .tanks where it clarifies. It
has a density of I 8 to 23 Be., and consists principally of ferrous

sulphate, ferric sulphate, and aluminium sulphate.
The next stage is to concentrate the liquor to 40 Be. in order
to extract the ferrous sulphate by crystallisation. The mother
liquor is re-evaporated in iron pans to a syrupy consistence, and
is then poured out on to a made floor.
The concentration is carried so far that the mass sets hard on
cooling, and furnishes a hard greenish-yellow product (vitriol stone),

which consists mainly of ferric sulphate, ferrous sulphate, and
aluminium sulphate.
From 15 to 20 parts of pyritic shale are needed to furnish
I This residue is placed in roasting furnaces,
part of vitriol stone.
where heated at a low temperature, and is stirred up in order
it is
to complete the oxidation of the ferrous sulphate, after which it is
distilled.
The constituent sulphates present are by no means. of equal

value for the manufacture of fuming acid. The ferric sulphate is
the best in this respect, and, in fact, is the only one which will
part with the whole of its sulphuric acid without the latter under-
going decomposition
Fe 2 (S0 4 ) 3 =3S0 3 +Fe 2 3
.
The ferrous sulphate, on the other hand, is first converted into

ferric sulphate, half of its sulphur being given off as sulphur di-
oxide, which in this case is wasted.
Finally, aluminium sulphate will not part with its sulphuric

acid except at a temperature whereat this latter is decomposed
into oxygen and sulphur dioxide. Consequently the best vitriol
stone for distilling is one containing the largest possible amount
of iron in the state of ferric sulphate.
(2) Distillation. The decomposition of ferric sulphate neces-
sitating a high temperature, the stills have to be made of crucible

clay, and small enough in size for the heat to penetrate all
through. They are slightly conical in shape (A, Fig. 193), about
8 inches in diameter and 30 inches long, and are arranged in

three or four rows around the gallery furnace, each of them
corresponding to a condenser B of practically equal size. Each
still is embedded in the wall of the furnace, and the condensers
are supported by iron plates. The neck of each condenser
engages in that of the corresponding still, and the joint is luted.
Usually the furnace contains 272 small stills, in addition

to which a row of large stills, C, extending right across the
furnace, and each containing 32 small stills, is sometimes
arranged in the upper part of the furnace, in which event there
are altogether 304 stills. The furnace is heated by i or 3 fires.
Each charged with 3 kilos. (6'6 Ibs.) of broken vitriol
still is
stone. When
they are all charged, gentle heat is applied by burn-
ing dried pinewood. At the end of about 4 hours distillation
commences, water vapour, with traces of sulphur trioxide and sul-
phur dioxide, coming over first. As soon as the white vapours of
sulphur dioxide appear, the condensers, which contain a little water,
or 66 Be. acid, are connected up, and the temperature is gradually
raised to white heat. The operation takes 24 to 36 hours.
When the distillation is finished the reservoirs are taken away
without being emptied, and the stills are emptied in order to
be refilled and the operation repeated, which furnishes a fresh
quantity of trioxide to enrich the acid already collected. When
this acid is sufficiently charged with trioxide to measure 79 or
80 Be., it is placed in stoneware vessels and left for about a week
to clarify.
The condensers are then re-charged with 500 grms. of water,

or 1
90 c.c. of 60 Be. acid. In the former case four or five dis-
tillations are required to produce 79 Be. acid ;

in the latter event,
three or four distillations will give 80 Be. acid. The acid is
stored in stoneware vessels, closed by a stoneware stopper luted

with wax.
For every 100 parts by weight of acid there remain about
1 2 5 parts of nearly pure iron oxide, known as Caput mortuum,
Colcothar, etc., which is employed for polishing glass, as a pig-
ment, etc. For the latter purposes it is calcined in closed vessels

with or without an admixture of common salt, and is supplied
in 5 7 different shades, ranging from blood - red to Havana
"
brown (Sorel, article on " Chemical Products in Fremy's
Encyclopedic).
(3) Cost Price. To obtain I cwt. of fuming acid, about 2i

cwts. of vitriol stone and I ton of fuel (lignite) are required.
According to Payen, the cost of manufacture is as follows :
s. d.
Dried iron sulphate, z\ cwts 56
Fuel (lignite), I ton 13
32
Labour
Repair to plant
Interest
....
........09 o 10
Total II 6
Less value of residue . . . o 10
(Sorel.) Nett cost of I cwt. fuming acid . 10 8
158. Purifying Waste Water from Manufactories with

Mixtures of Aluminium Sulphate and Iron Sulphates. These
mixtures, generally waste products, have been successfully
applied to water purification. The residual liquors from the

manufacture of alum and ferrous sulphate from lignites have
been, and still are, used in sugar works, distilleries, starch works,
tanneries, etc. Their composition has already been described
(Part II., Treatment of Lignites).
M. Vivien, of St. Ouentin, has taken great interest in the
utilisation of these residual liquors, and the following
notes are
extracted from his work on the purification of waste waters from
factories and sewage waters.
The waste waters from starch works, distilleries, sugar

works, etc. are contaminated with mineral matters (earth and
inorganic salts) and various organic substances, soluble and
insoluble.
The changes produced in the watercourses into which these

waste waters are discharged are principally due to the organic
substances in question. Such as are soluble act immediately,
whilst the insoluble substances undergo decomposition, which in
turn converts them into the soluble and more injurious condition.
Vuc en plan d'une.seric i!e bassins isoles el md^pendants.
Fir,. 194. Purification of waste waters. Plan of a series of isolated and
independent decantation basins.

Vanne = sluice ; Canal d' arrives, etc. =feed conduit ; Canal de fnite
= outflow channel.
The germs of inferior organisms, such as bacteria, monads,

mucors, mucedinae, allabundantly disseminated in nature, act in
contact with air ; others, such as vibrios, spirilla, bacilli, etc., act in
the absence of air, the result in both cases being the decomposi-
tion of the organic matters, even cellulose, with the formation
of micro-organisms and more or less foetid gaseous products.
If the decomposed matter is non-nitrogenous a liberation of
carbon dioxide and hydrocarbons occurs, and water is produced
along with acetic acid, oleaginous and humous products of various

kinds. In the case of organic matter containing nitrogen and
sulphur, a liberation of sulphuretted and phosphuretted hydrogen

and production of ammonia and nitric acid will be noticeable.
Concurrently, the watercourse will become infested with
special kinds of algae, hypheothrix being the first to appear,

and followed by beggiatoa, leptomitus, spirogyra, and finally by
cladopkora, the forerunner of purification. Aquatic plants dis-
appear at the outset, but again come upon the scene when the
water is once more in a pure state.
To obviate the foregoing inconveniences, the water must be
purified and afterwards aerated, either by allowing it to flow
thinly over the surface of a meadow or by filtration through a

porous soil. To obtain the destruction of organic matter, how-
ever, this filtration must be gradual, and a soil that is too
permeable is therefore unsuitable.

Waste water from manufactories ought to be purified im-
mediately it leaves the works, and before any internal change

begins. This is very important.
In order to obtain thorough purification of the water from
beet-sugar refineries, the following conditions which are subject

to modification to meet the requirements of each particular case
should be fulfilled :
(1) The water from the pulp presses should be purified
separately before use in washing the beet; and in default of

a thoroughly efficient method of purification for that purpose,
or to fit the water for discharge into a watercourse, it should
be treated by known means, and turned on to the land or oxidised
by running it for a sufficient distance over the meadows. The

press water represents about 6 to 9 gallons per cwt. of beet, or
1
400 gallons per i oo tons ;
and enough ground is generally
available to oxidise this quantity after the necessary clarifica-
tion.
(2) The other waste waters should be united and treated

with lime, either alone or with a salt of iron or alumina, followed
by lime to render them alkaline. The residual liquors from the

manufacture of alum and ferrous sulphate from lignites may be
successfully employed for this purpose, in the proportion of i

part of 32 Be. liquor per 1000 parts of beet; after the water
has travelled a distance of about I o yards the metallic salts will
have had time to act, whereupon sufficient 10 to 15 Be. milk
of lime is added to completely decompose the iron and alumina
salts, and to impart a slightly alkaline character to the liquor,
which then deposits a flocculent sediment and clarifies. The
degree of alkalinity (expressed in terms of CaO) should vary
between 100 and 200 m. grms. per litre.
FIG. 195. Vertical section of decantation basin.
Arrivee s\\ i
>'p\y ; Pente = gradient ; Canal de fuite = outflow.
Treated in this manner, the waste waters from sugar works

are rendered easy of decantation. The operation is performed
in a series of basins, each of which can be isolated from the
system when full, the waters being delivered through a channel
with a fall of about 20 per 1000. The arrangement of these
basins is shown in Figs. 194, 195. Here A, B, C, D are the
basins, varying in number and

according to the quantity size
of matter to be precipitated, the dimensions being chosen so that

each basin can be filled in the shortest possible time 10 to
1
5 days according to the susceptibility of the sediment to
decomposition. The waters settle in the first basin, and then

pass in turn through the second, third, and others in the series,
being only discharged into the outflow when perfectly limpid
for instance, after leaving the basin C. At this stage they should
be slightly alkaline to test paper. If they can then be made to
overflow the surface of a plot of ground in a thin layer, e.g., used

for irrigating meadow land or filtered through permeable soil,
they will be inoffensive, well aerated, and purified to the fullest
extent.
When the first basin of the series is full the supply is stopped
and the impure waters are delivered into the second basin (15),
and so on to the end of the series, the end basins being placed
in communication, by means of a conduit, to establish a con-
tinuous circulation and recommence a fresh series when the last
basin has been reached.
Where the available ground space is large enough for a
sufficient number of basins to hold the whole of the deposits
there is nothing further to do but if space is limited, each basin
;
will have to be emptied when shut off from the rest, and cleaned
out for use over again.
If the basins are above ground which is preferable to
sinking them below the surface they are easy to drain and
empty, it being sufficient to lay a few (8-inch) earthenware pipes,
H, on the lower side of each basin, and cover the inner ends with
faggots to serve as a filter and prevent obstruction. While the
basin is in use these pipes are closed with plugs, which are re-
moved when the work of discharging the deposited mud is
commenced. The sloping bottom allows the water to drain

away, and a breach can be made in one of the banks in order
to clear out the mud.
In sugar works the acidified waters from the triple-washing
process should be completely neutralised before they are run into

the collecting tank, lime or even chalk being suitable for this
purpose.
In factories where caustic soda is used for washing the
utensils, the waste liquids should be stored separately, and not
run off until they have been neutralised by some acid.
The cost of purifying the waste waters of sugar works, for
example, by means of alum waste liquor, may be put down as

follows per ton of beet treated in the works :
Reagent, 2 '2 Ibs. at 325. per ton . . = O'4d.

Lime, 22 Ibs = 0-14
Labour . . . . O'i8
Total
or,taking 500 gallons as the volume of waste water from treating

iton of beet, the cost will be O'i4d. per 100 gallons treated.
The pasty mixture or magma obtained by evaporating the
extract from oxidised lignites, and consisting of a very impure
35O USES OF THE SULPHATES OE ALUMINIUM AND IRON
aluminium sulphate with a large proportion of ferric and ferrous

sulphate (see Part II., Chap. III.), may also be used for this puri-
fication.
Trials have been made with this sulphate in the vicinity of
the large collecting basin at Clichy, about 2 Ibs. being used

per 1000 gallons of sewage water. That the results are fairly
satisfactory will be evident from the following table, the figures
being averages for a working period of nine months :
The oxidised lignites themselves have also been used for the
same purpose, by the Houzeau and Devedeix method, which
consists in thinning down the lignite with water and pouring it
into the waste water under treatment, a certain quantity of milk

of lime being then stirred in. A coagulum forms, and the sub-
stances are rapidly precipitated. The quantity of lignite required
varies from I to 3 grms. per litre (1000 grms.) of waste water
treated.
159. Utilising Pyritic Lignites for Fertilising and Im-

proving Soils. The oxidised pyritic lignites, and even the
lixiviation residues from the same, are still largely employed in
agriculture, though nothing like to the same extent as they were
thirty years ago.

The virgin cinder or unextracted oxidised lignite is applied at
the rate of about I 2 bushels per acre, chiefly for meadow land or
artificial grasses. It acts by virtue of its ferrous sulphate, and
produces the same result as this latter. On artificial grasses it
has the same effect as gypsum, and is very useful. Moreover,
containing o 3 to Q'5 of nitrogen, though
-
in a slowly assimil-
USES OF THE SULPHATES DF ALUMINIUM AND IRON 351
able form, it also possesses a certain value as a nitrogenous

manure.
The lixiviated cinder is applied to the same uses, but the
dressings are much larger, namely 60 bushels per acre.
Both kinds of cinder are largely used in the vine districts of

Champagne, where they are made into compost with stall manure,
sweepings, mud, etc. When mixed with fossil phosphates they
render a portion of the phosphate soluble and assimilable, and
fairly good results have been obtained by treating stall manure

with this mixture.
Pyritic lignite or cinder should be used on calcareous sandy

soils, the dressing being applied in autumn or spring.
PART IV
CHEMICAL CHARACTERISTICS OF IRON AND ALUM-
INIUM. ANALYSIS OF VARIOUS ALUMINOUS OR
FERRUGINOUS PRODUCTS.
CHAPTER VII
ALUMINIUM
I. CHEMICAL CHARACTERISTICS OF THE ALUMINIUM

COMPOUNDS
1 60. General Reactions of the Aluminium Salts. Solutions

of aluminium salts are generally acid to test paper.
Caustic Alkalis give with aluminium salts a white gelatinous
precipitate soluble in excess of the reagent.

Ammonia completely precipitates alumina in the state of
hydroxide, when the precipitation is effected in presence of

ammonium chloride and boiled until all the excess of ammonia
has been driven off.
The Alkali Carbonates give a white precipitate of alumina,

with liberation of carbon dioxide, and the precipitate is insoluble
in an excess of the reagent.
Oxalic Acid and Alkali Oxalates do not precipitate aluminium

salts.
Sodium PhospJiate throws down a white precipitate of hyd rated

aluminium phosphate, which is difficult to identify owing to its
great resemblance to alumina, being gelatinous and soluble in
both caustic alkalis and acids.

ANALYSIS OF ALUMINOUS OR FERRUGINOUS PRODUCTS 353
Barium Carbonate and Calcium Carbonate in considerable

excess precipitate alumina, even in the cold ;
the reaction is
slow at the ordinary temperature, but rapid at boiling heat.
SulpJiuretted Hydrogen gives no precipitate with aluminium

salts, but ammonium sulphide completely precipitates aluminium
in the condition of hydroxide, with liberation of H 2 S.
Sodium Hyposulphite (thiosulphate) completely precipitates

alumina in the warm, and when the reagent is in excess.
A somewhat characteristic reaction is obtained by evaporating
aluminium sulphate in presence of an excess of potassium sul-
phate alum is formed, crystallising in cubes or octahedra.

;
Aluminium can be readily detected by microchemical means.

One exceedingly delicate reaction is aluminium
to precipitate the
salt as a cesium alum (Cs 2 SO 4 A1 2 (SO 4 ) 3

, , 24H 2 O), the limit of
sensitiveness being 0*3 micromilligram of aluminium.
Aluminium is easily distinguished before the blowpipe, by
furnishing a fine blue coloration when heated along with cobalt
nitrate. This reaction is characteristic, provided the mass does
not fuse, a blue fusible bead not being distinctive of this
metal.
161. Estimation of Aluminium. The metal is estimated in
the condition of alumina. When combined with nitric or hydro-
chloric acid thrown down, as hydroxide, by adding ammonium
it is
chloride, boiling, and, after removal from the flame, treating with
ammonia, which gives a gelatinous precipitate impregnated with

ammoniacal salts. After re-boiling to expel the excess of am-
monia, the liquid is leftfor the precipitate to subside, and is then
filtered. The precipitate is washed by decantation, until the
washings cease to leave a residue when a portion is evaporated

on a strip of platinum. After drying at 100 the filter and
the cover
precipitate are calcined in a covered platinum crucible,
being removed when it is certain that all moisture has been
expelled.
Ammonium Sulphide is a good precipitant for this metal, but
not in presence of other metals precipitable by the same reagent.
Moreover, there is always the risk of a portion of the sulphide

oxidising during filtration, and forming an insoluble
aluminium
23
354 CHEMICAL CHARACTERISTICS OF IRON AND ALUMINIUM
sub-sulphate which is difficult to decompose by calcination, in

which event the weight of alumina is somewhat in excess of the
truth.
If the precipitation by ammonia be effected in presence of

sulphuric acid, the formation of insoluble sub-sulphates will occur,
and the final traces of sulphuric acid will be difficult to eliminate
in calcination. When this accident is feared, the precipitate must
be re-dissolved in hydrochloric acid and thrown down anew with
ammonia.
Sodiimi Hyposulphite (thiosulphate) is a good precipitant for
alumina in presence of sulphuric acid.
The volumetric estimation of alumina has also been proposed.

Aluminium phosphate is insoluble in acetic acid in presence
of alkali phosphates ;
and a weak solution of alumina, too dilute
for detection by ammonia, will still give a decided turbidity on

the addition of a phosphate. Aluminium phosphate only exhibits
the constant composition A1 2 (PO 4) 2 when the aluminic solution
is treated with sodium acetate and poured into a solution of a
tribasic phosphate acidified with acetic acid, otherwise the pre-
cipitate will be of variable composition.

On this reaction Fleischer founded the following volumetric
method of estimating alumina :
The aluminic solution is treated with sodium acetate and

poured into a burette having previously, if alkaline, been satur-
ated with HC1 and is then run, drop by drop, into a standardised
phosphate solution. To ascertain whether the end point of the
reaction has been attained, it is necessary to filter a few drops of
the phosphatic liquid at intervals and see whether it still gives a
turbidity with the aluminium solution. An alcoholic solution of
brasiline, which gives a violet-blue coloration with a slight

excess of aluminium acetate in the warm, may also be used as
indicator.
The phosphate solution is prepared by dissolving equal parts

of ordinary (uneffloresced) sodium phosphate and sodium acetate
to form a decinormal solution (Fleischer).
162. Separating" Aluminium from other Metals. Alu-
minium may be separated from the alkali metals, calcium, and
magnesium by precipitation, as alumina, with ammonia in pres-

ence of ammoniacal salts. The alkali salts, the calcium, and the
magnesium remain in solution ;
but if a large proportion of
calcium be present a portion may be carried down along with
the alumina, or precipitated by the carbon dioxide in the air.
When barium and strontium are present they must be removed
by sulphuric acid before proceeding to the precipitation of the
alumina.
If the aluminium and calcium are in the form of nitrates they
maybe separated by evaporation and heating to i7o-i8oC.,
whereupon the aluminium nitrate decomposes, with liberation of
nitrous fumes, whilst calcium- and magnesium nitrate remain
almost unchanged. Ontaking up the mass with concentrated
ammonium nitrate, the whole of the calcium and magnesium will
aluminium hydroxide entirely insoluble.
re-dissolve, leaving the
For separating aluminium from phosphoric and arsenic acids,
the first-named must be in the state of nitrate or chloride. The
liquid is evaporated, along with an excess of H 2 SO 4 until the ,
appearance of white fumes. After cooling, a concentrated solution

of aluminium is added, and the liquid shaken up, whereupon alum
is formed, and is thrown down by alcohol. On filtering after
several hours' rest, the arsenic and phosphoric acids pass away in
the filtrate. Sometimes a small quantity of alumina escapes
with the acid solution ;
this can be tested by neutralising the
phosphoric acid with ammonia and precipitating with ammonium

coming down as oxide.
sulphide, the remainder of the alumina
Aluminium can be separated from zinc, nickel, or cobalt by
adding sodium carbonate, followed by potassium cyanide and
digestion in the cold. The carbonates dissolve and the alumina
is collected on a filter, but must be re-dissolved in acid and re-
precipitated before weighing, in order to free it from alkali.
Sodium hyposulphite is employed to separate aluminium from

iron and manganese, an excess of this reagent, in the warm,
in solu-
throwing down alumina completely, but retaining iron
tion as a double hyposulphite.
The aluminium and iron being dissolved in hydrochloric acid
or sulphuric acid, the excess of free acid is nearly neutralised, and

\vater is added to reduce the content of the two oxides to below

OT grm. per 50 c.c. To this solution (cold] a slight excess of
hyposulphite is added, and after decoloration has taken place heat

is applied, and the liquid kept on the boil so long as an odour of
SO 2
continues noticeable. The granulated precipitate is washed
quickly, dried, calcined, and weighed. The alumina is always
white (Gerhardt and Chancel).
Among other methods proposed, the following may be

mentioned :
(1) Separation by using NaHO or KHO.

(2) Fusion of the two oxides with NaHO or KHO.
(3) Reducing the oxides by hydrogen, and dissolving the iron
in dilute hydrochloric acid.
(4) Treatment of the solution with H 2 S or (NH ) S
4 2
after an
addition of ammonium tartrate or citrate.
An original method for separating aluminium and iron is that
proposed by F. A. Gooch and F. S. Havens, and based on the

fact that hydrated aluminium chloride (A1 2 C1 6 ,
I2H 2 O) is but
very slightly soluble in hydrochloric acid, whereas Fe 2 Cl c is
extremely soluble therein.

The mixed chlorides are dissolved in a minimum of water,
and poured into a mixture of equal parts of ether and con-
centrated HC1, aluminium chloride being less soluble in this than
in HC1 alone. The liquid being kept at 15 C., is saturated with
gaseous HC1, this being repeated after an addition of several c.c.
of ether. The A1 2 C1 6 comes down and is filtered over asbestos in
a Gooch crucible, then washed with the ether-HCl mixture,
re-dissolved in water, and thrown down by ammonia for estimation
as A1 2 O 3 . One part of A1 2 O 3 corresponding to 5 parts of A1 2 C1 6
, ,
dissolves in 125,000 parts of the ether-acid mixture.
Vignon proposed to separate iron from aluminium by treat-

ing the mixed oxides with trimetliylamine. This forms soluble
trimethylamine aluminate, which is separated from the insoluble
ferric oxide by filtration.
Ilinski and Knorre proposed another organic reagent, nitroso-
$-naphthol, for this purpose, ferrous and ferric salts being thrown
down from an acetic acid solution, whilst alumina remains dis-
solved. The method, however, is inapplicable when phosphates

are present.
Electrolysis can also be successfully employed for separating
aluminium from iron. The operation is performed in presence of
a large excess of ammonium oxalate, with a current of about
amperes, care being taken to prevent a rise in temperature.

-
i
In this manner aluminium may be separated from iron, nickel,

cobalt, and zinc.
When the electrolysis is prolonged the aluminium is thrown
down as hydroxide never in the metallic state, and in such

event must be re-dissolved by an addition of oxalic acid (Classen
and Ludwig, Berickte, I
8, 1795).
The metals of the third group are separated en bloc by treating
the mixture with potash in presence of tartaric acid. Sodium
sulphide is then added, the liquid poured off after settling, and the
precipitate filtered, sodium sulphide water being used for washing.

The solution will contain only aluminium and chromium, which
may then be separated by heating with potassium nitrate and
fusing the residue with 4 parts of K CO

2 3 and 2 parts of KNO 3
.
The fused mass is treated with HC1 and KC1O 3 evaporated, and
,
taken up again with water. On adding ammonia, alumina is

precipitated, the chromium being left in solution.
Aluminium can be easily separated from the metals precipitable
by sulphuretted hydrogen from acid solutions.
2. ANALYSING ALUMINIUM PRODUCTS
163. Analysis of a Clay or Kaolin. A. TOTAL ANALYSIS.

The substances to be estimated are (i) hygroscopic moisture;
(2) water of combination; (3) organic matter; (4) alumina; (5)

ferric oxide; (6) silica and insoluble matter; (7) lime; (8)
magnesia; (9) potash ; (10) soda.

I. Hygroscopic moisture is determined by drying a sample at
i 20 C. until constant.
Water of Combination and Organic Matter. The dried

II.
from I. is calcined at bright red heat, which removes the

sample
water of combination, organic matter, and carbon dioxide. The
latter is estimated by the usual methods, and the difference gives

water of combination and organic matter together.
III. Silica and Insoluble Matter. The calcination residue is
pulverised with care, and grm. is mixed with 4 or 5 grms.

i
of pure dry sodium carbonate in a platinum crucible, which is

then gradually heated to bright redness. Alkali silicates and
aluminates are formed, w hilst the lime, magnesia, and
r
ferric oxide
are separated. When the mass is fused the crucible is cooled
suddenly by standing it on a cast-iron plate or by immersion

in cold water, which generally enables the contents to separate
from the walls of the vessel. The whole is then placed in a
porcelain capsule and treated with 15 to 20 parts of dilute
hydrochloric acid. As soon as solution is complete the crucible

is withdrawn and washed, the washings being united to the
solution, and the whole evaporated to dryness. It is then taken
up with water acidified with HC1, filtered, washed, calcined, and

weighed, the result being the silica.
IV. Alumina and Iron. -The washings from the preceding test
are made up to a known volume, and an aliquot portion is taken
and treated with a little bromine water to peroxidise the iron.
After expelling the excess of bromine by boiling, ammonia is
added in slight excess, this being next removed by boiling up

again, after which the liquid washed by
is filtered, the precipitate
decantation and on the filter, and and
weighed.dried, calcined,
This gives the alumina and ferric oxide together, and the iron can
then be estimated in the ordinary way. It is, however, preferable
towork with another aliquot part of the solution and to acidify
same with H 2 SO 4 evaporate until white fumes appear, take up
,
with water, reduce by means of zinc, and estimate the iron (as
ferric oxide) with potassium permanganate. Alumina is taken by
difference in either case.
V. Lime, Magnesia. The filtrate from the precipitation of

iron and alumina is treated with ammonium oxalate to throw
down the lime ; and, after removing the calcium oxalate by
filtration, sodium phosphate is added, with the usual precautions,
to precipitate the magnesia.
VI. Potash, Soda. From 2 to 4 grms. of the substance under

examination are weighed out and calcined, the residue being
dissociated by means of sulphuric and hydrofluoric acids. Hydro-
chloric acid is then added, and the liquid made up to a known
volume, an aliquot part of which is next treated with barium

hydroxide and filtered. After washing, the excess of barium in
the filtrate is thrown down by ammonium carbonate, re-filtered,
and evapor'ated to dryness. The residue is calcined, taken up
with water, again treated with ammonium carbonate, and filtered
a third time, whereafter it is evaporated to dryness, calcined, and
weighed, thus giving the sum of the two chlorides. The potash is
separated by platinum tetrachloride, and the soda is then readily

calculated.
Or the following method may be pursued :
i to 2 grms. of the product are mixed with a sixfold volume

of ammonium fluoride, and heated to redness in- a platinum
crucible. The silica is volatilised as silicon fluoride, leaving the
fluorides of calcium, magnesium, and the alkali metals, as residue.
On treating these with H SO

they are converted into sulphates,
2 4
which should completely dissolve in water acidified with HC1, and

are then transformed into chlorides by precipitating the sulphuric
acid with barium chloride. The iron and alumina are separated
with ammonia, and the lime with ammonium oxalate ;
the liquid
is then evaporated, and the residue calcined to expel the ammonia
salts, leaving magnesia and alkali metals as chlorides. These can

finally be separated in the usual manner.
B. PARTIAL ANALYSIS.
Clay intended for producing
aluminium sulphate or alum can be analysed in a far simpler
manner, which, however, is quite sufficient to determine its value

for manufacturing purposes. Moreover, the method has the
advantage of being a reproduction of the manufacturing process
on a small scale.
A small sample (about 50 grms.) of the clay is placed in a
tared porcelain platinum capsule and moderately calcined.
or
When the clay has attained dull red heat the capsule is withdrawn
and weighed after cooling, the difference giving the loss of weight
o)i calcination,
The powdered residue is then treated with 100 grms. of

60 Be. sulphuric acid, the whole being well mixed and heated
gently until it solidifies, thus converting the alumina into sulphate ;
whereupon it is extracted with boiling water, filtered, and the

united liquids concentrated to about 35 Be. This solution is
next boiled with a slight excess of potassium- or ammonium
sulphate and left to crystallise. When the capsule is cold the

liquor is poured off, the alum being washed with a cold saturated
solution of alum, and afterwards dried and weighed. The weight
of alumina is ascertained by calculation (Pouchet).
1
64. Analysing Bauxite. The constituents to be estimated
are (i) water and organic matter; (2) insoluble matter;
(3) titanic acid; oxide; and (5) alumina.
(4) ferric
I. Water and Organic Matter are determined by calcining

0*3 grm. of the mineral, beginning at gentle heat and finally
before the blowpipe until constant.
II. Insoluble Matter. 1*5 grms. of mineral, ground and dried
at iooC., c.c. of 42 Be. sulphuric acid, and
are treated with 50
evaporated fumes
until white
are evolved. The mass is taken up
with i oo c.c. of water, boiled for I o minutes, then filtered and washed
with hot water. The united filtrates should measure i 7 5 c.c.
The insoluble residue is calcined and weighed. It consists
mainly of silica, with a little titanic acid, ferric oxide, and

alumina. To estimate the SiO 2 the
,
insoluble matter is taken
up with HF and H SO 2 4, evaporated, calcined, and weighed, the

loss in weight being silica.
The new residue is fused with I

grm. of potassium bi-
sulphate, the cooled mass being returned to the beaker contain-
ing the sulphuric liquor from the original attack on the substance.
The slight residue left consists of silica, which must be added to
that already obtained.
III. Titanic Acid. The volume of the sulphuric solution is
made up to 250 c.c., and after agitation 50 c.c. of this solution
(
= o '3 g rm - of bauxite) are diluted to 300 c.c. and treated with
2 c.c. of HC1, followed by a slight excess of ammonia ;
then boiled
for 5 minutes, filtered, and washed with boiling water. The
precipitate, weighed after calcination, contains alumina, ferric
oxide, and titanic acid.

To estimate the last-named, 100 c.c. of the sulphuric solution
(
=o6
grm. of bauxite) are treated with ammonia until a per-
-
manent precipitate is formed, this being then re-dissolved in a

few drops of H SO
2 4,
and the solution diluted to 400 c.c. If the
solution contain much iron it will be of a yellow colour, and in
such event is reduced by a current of SO and boiled for

2
an
hour, a little of a saturated solution of SO being added
2
at
intervals. The titanic acid precipitate is filtered, and washed

with boiling water. If yellow, iron is indicated, and the mass
must be fused with 4
taken up with water, and
I
grm. of KHSO ,
the iron titrated with permanganate after reduction with zinc.

IV. Ferric Oxide. 50 c.c. of the sulphuric solution are
treated with 10 c.c. of dilute H 2 SO 4 and I grm. of granulated
zinc. After the reduction is complete the solution is titrated
with permanganate. When the mineral contains but very little
iron, 0*5 grm. must be taken. This is evaporated in a platinum

crucible with 3 c.c. of 25 per cent. H SO
2 4 and 5 c.c. of HF until
white fumes are given off, the excess of sulphuric acid being then
expelled by heat. When cool the residue is taken up with water

and i o c.c. of dilute H 2 SO 4 the liquid being then reduced by zinc
,
and titrated with

permanganate.
V. Alumina. This is determined by deducting the weights
of ferric oxide and titanic acid from the first precipitate obtained
in Test III. (J. Otis Handy, Industries and Iron, vol. xxi.
Nos. 1239-1241).
165. Analysis of Alunite. Constituents estimated (i) water

and loss on calcination ; (2) silica and insoluble matter ; (3) potash ;
(4) alumina; (5) ferric oxide.
I. Water and Loss on Calcination are found by calcining

I
grm. of substance at moderate heat, preferably over a Bunsen
flame, so as not to decompose the sulphates.
II. Silica and Insoluble Matter. Two grms. of pulverised
substance are treated with dilute HC1 in a porcelain capsule;
then evaporated to dryness, taken up with HC1 and boiling water,
filtered, washed, and calcined. The solutions are united and
made up to a known volume.
III. Stdphuric Acid\<-> determined by precipitating an aliquot
362 CHEMICAL CHARACTERISTICS OE IRON AND ALUMINIUM
portion of the clear liquid with barium chloride, the usual pre-
cautions being taken.
IV. Alumina and Ferric Oxide. Another portion of the
liquid is treated with bromine water to peroxidise the iron,
which is thrown down, along with the alumina, by ammonia after
boiling. The precipitate is washed, calcined, and weighed.

The iron is determined by treating a known volume of the liquid
with H SO
2 4, followed by evaporation, reduction by zinc, and titration
with permanganate. The alumina is then easily calculated.
V. Potash. One grm. of substance is acted upon with HC1,
the residue is removed and the liquid precipitated by barium
hydroxide, the excess of which is afterwards removed by
ammonium carbonate. filtration, washing, and evapora-
After
tion to dryness, the residue taken up with water acidified with
is
HC1, filtered again, evaporated, and the potash estimated by

means of platinum chloride.
1
Analysis of Alumina.
66. A. ALUMINIUM HYDROXIDE.
The following are determined (i) water; (2) silica; (3) alumina ;
(4) soda.
I. Water. One grm. of substance is calcined in a well closed
crucible, the heat being applied gently at first, but afterwards by

the gas blowpipe for 20 minutes. The loss in weight represents
water and CO 2
. This latter is afterwards calculated from the
weight of soda found at a later stage, and is then deducted, the

difference being water.
II. Aluminium hydroxide is soluble in 42 Be.

Silica.
sulphuric acid prepared from 900 c.c. of concentrated H 2 SO 4

and 1290 c.c. of water which leaves silica unchanged.
Five grms. of substance are dissolved by heating with 25 c.c.
of 42 Be. acid, the liquid being then made up to 100 c.c. and
boiled. washed, dried, and fused
After filtration the residue is
with i grm. of potassium bisulphate, after which it is cooled, taken
up with water, filtered, washed, calcined, and weighed in a

platinum crucible. This calcined residue is treated with HF and
H SO
2 evaporated to dryness, calcined anew, and weighed the
4) ;
difference between the two weights represents silica (J. O. Handy).
III. Soda. One grm. of substance is treated with a mixture

of nitric and hydrochloric acids. After boiling to drive off HC1

the solution evaporated to dryness, in a large platinum capsule,
is
over a Bunsen burner until nitric vapours cease to come off. The
residue is crushed and mixed with I
grm. of pure 4 C1
and NH
8 grms. of CaCO 3 . It is then heated in a covered platinum
crucible, the Bunsen flame merely touching the bottom during
the first I hour, after which it is raised to a bright red heat for
45 minutes. After cooling, the mass is treated with just enough

water to make it friable, then powdered in a mortar and ex-
tracted with hot water, filtered,and washed, the filtrate being
shaken up with a slight excess of ammonium carbonate. The
calcium carbonate precipitate is filtered, the filtrate evaporated
in a platinum capsule over the water bath, then heated to drive
off the ammonia salts, re-dissolved in a little water, again treated
with ammonium carbonate, shaken up, filtered, washed, evaporated,
dried, gently calcined, and weighed. The result is sodium chloride,
from which the weight of carbonate is ascertained by calculation
(J. Otis Handy).

IV. Alumina is estimated by difference.
B. CALCINED ALUMINA. Water and soda are determined as
in hydrated alumina, the soda being calculated as Na.2 O.
The silica is estimated by fusing I grm. of substance with
10 grms. of KHSO 4,
the mass being taken up with water and
filtered. The insoluble residue is calcined and then fused with
i
grm. of Na 2 CO 3)
the melt being taken up with I
5 c.c. of water
and 25 c.c. of 25 per cent. H SO
2 4
in a covered porcelain capsule,
solution being followed by evaporation until white fumes appear.
After cooling, the mass is treated with water, filtered, washed,
dried, calcined, and weighed. The residue taken up by HF and

H SO 2 4 is re-weighed after calcination, the difference giving the
weight of silica.
167. Analysis of Sodium Aluminate. In this case alumina

and soda have tobe determined. Gravimetric methods may be
employed, but G. Lunge (Monit. Sclent., 1891, p. 285) recom-
mends the following titrimetric method :
A given weight of the aluminate is dissolved and diluted to a

known volume, the insoluble residue being determined. One
portion of the clear liquid is treated with phenolphthalein and

titrated in the warm with normal HC1 solution until decoloration
occurs. This gives the amount of soda combined with alumina
and silica. A drop of methyl orange is then added to the same
portion of liquid, and titration is continued at 30 to 37 C. until
the red tinge becomes permanently yellow, this change marking
the end point of the alumina determination. The method gives
highly satisfactory results, 26*08 per cent, of A1 2 O 3 being found
in one case instead of 25*92
per cent, furnished by the gravimetric
method. With a pure product the latter method gave 2
-
8iS grms.
of A1 2 O 3 per
litre, and the volumetric method 2'82O3 grms. A
somewhat similar method was proposed by Bayer (Zeits. Anal.
Chem., 24, p. 542).
1 68. Analysis of Aluminium Sulphate. The substances to
be estimated are (i) water; (2) insoluble residue; (3) alumina;
(4) total sulphuric acid ; (5) potash and soda ; (6) iron ; (7) free
sulphuric acid.
I. Water. This is easily determined by calcining the sub-
stance with great care.
II. Insoluble Residue. 2 to 5 grms. of substance are dis-
solved in distilled water, the insoluble portion being dried and
weighed.
ill. Alumina. This is easily estimated from an aliquot part
of the foregoing solution by means of sodium hyposulphite, the
precautions already given being observed. p.<3*T
IV. Total Sulphuric Acid. This estimation is performed on
another aliquot part of the solution from II.

V. Potash and Soda are also determined from an aliquot part
of the solution after eliminating the other constituents by the
usual means.
VI. Iron. When the substance is impure and contains much
iron, that metal can be estimated by the permanganate method
This is, however, rarely the case, the amount of iron being usually
not more than traces, to which the titrimetric method is inap-
plicable. In such event colorimetry must be resorted to, and

for this purpose it was at first proposed to employ potassium
sulphocyanide and compare the colorations obtained.
According, however, to G. Kriiss and H. Moraht, the resulting

red coloration is not necessarily proportionate to the percentage
of iron, but is greatest when the iron and the sulphocyanide are
in equivalent proportions. The coloration is, in fact, due to a
ferri-potassium sulphocyanide which is decomposed by water ; and,

its intensity being a function of the dilution, cannot serve as a
guide to the percentage of iron present.
The equation
Fe,Cl 6 + 6KCNS = Fe 2 (CNS) G + 6KC1
does not exactly express the reaction corresponding to the
maximum of coloration. In fact, 24 molecules of KCNS
are required to i of Fe 2 Cl c ,
which indicates a double salt
as the cause of the coloration, namely Fe 2 (CNS) 6 , iSKCNS,

a salt crystallising, with 8H 2 O, to form hygroscopic prisms.
On dilution it is decomposed into I2KCNS and another
double salt, Fe 2 (CNS) G , 6KCNS, which crystallises in hex-
agonal prisms furnishing a lighter coloured solution of a more
orange tinge.
Magnanini arrived at results slightly differing from these,
but likewise indicating the unreliability of the process.
On the other hand, it has been experimentally proved by
J. Riban that solutions of ferric sulphocyanide and coloured
solutions of acetates and double tartrates of the alkalis are
subject to progressive dissociation of the pigmentary salt, and,

being therefore impossible of comparison with standards, are
inapplicable to the colorimetric estimation (even approximately)
of iron. .
R. Tatlock's method of colorimetric determination with
sulphocyanide performed as follows

is The" red solution is :
agitated in a tube with ether, and the resulting coloration is
compared with those furnished by standard ferric solutions under
the same conditions.
G. Lunge (Monit, Scient., 1897, P- 160) gives the following

method for estimating small quantities (only) of iron in aluminium
sulphate by colorimetry :
Use is made of tubes of very clear glass, with emery stoppers,

and graduated, in TV c.c., to 25 c.c., their size (internal diameter,
1
3 mm.) being such as to leave plenty of room for shaking
up the contents. Three at least are required for each test,
but it is better to have five or six.
The reagents consist of

-
y (i) A -jV solution of potassium sulphocyanide.

'
(2) Pure ether.
(3) A solution of ammonium ferrosulphate prepared by dis-
solving 7 grms. in I litre of water containing a little H.,SO 4 .
For use, I c.c. is diluted to 100 c.c., the new solution therefore
containing croi grm. per litre.
(4) Nitric acid, as free from iron as possible.

When the substance under examination is pure, I to 2 grms.
are dissolved in a little water and treated with I c.c. of HNO 3,
the liquid being made up to 50 c.c. after heating and re-cooling.

At the same time, I c.c. of the nitric acid is also diluted to
50 c.c.
Five c.c. of the solution of substance are then placed in a test-
tube, and an equal quantity of the dilute nitric acid in three or
four other tubes, a variable quantity of the ammonium ferro-
sulphate being added to each, so as to form a scale of percentages

which shall include that of the substance under examination.
Each tube receives a uniform addition of water and 5 c.c.
of potassium sulphocyanide, whereupon coloration ensues but ;
as this is generally a dirty reddish yellow, and not in relation
to the percentage of iron, each sample is treated with 10 c.c.

of ether, and well shaken up. The compound sulphocyanide
of potassium, iron, and aluminium is decomposed by the ether,
which dissolves out the iron sulphocyanide alone, and is tinged

in proportion to the amount of iron present. The aqueous
solution should be completely decolorised and as the colour ;
of the ethereal layer progressively deepens, it is advisable to

leave a"t rest for some hours before comparison, though not
too long, as otherwise decoloration may set in.
The degree of precision may attain to-j-O'i c.c. of the

ferrous solution, i.e. to + crooooo I
grm. of iron per 5 c.c. of
solution tested, provided these 5 c.c. do not contain more than
0*00002 grm. of iron.
ANALYSIS OF ALUMINOUS OR FERRUGINOUS PRODUCTS. 367
VII. Free Sulphuric Acid. The presence of this acid may

be tested by campeachy wood tincture (i part of wood, 3 of
water, and i of alcohol), the violet tinge of which is changed to
brown. The estimation is a delipate operation.
(1) Determination in an Alcoholic Extract. According to O.

Miller (Zeits. Anal. Chem., vol. 24, p. 258), the extract prepared
by treating the substance with alcohol is evaporated to expel

the latter, and titrated with jV-normal soda in presence of
methyl orange. According to Williams, the idea of expelling

the alcohol must be abandoned, in order to avoid loss of H 2 SO 4 ,
the acidity being then titrated with NaHO in presence of
phenolphthalein as indicator.
In the former case, according to Lunge, the results are too
low, and in the latter too high, besides being irregular.

(2) Estimation by Boiling- with an Excess of Ammonium-
magnesuni Phosphate. According to Erlenmeyer and Levinstein,
the whole of the A1 2 O 3 is
precipitated as a neutral salt, and the
free H SO2 4
can be determined in the filtered liquid. Beilstein and
Grosset, however, do not recommend this method, preferring
the following, based on the fact that when neutral ammonium
sulphate is added to aluminium sulphate the latter is precipitated
as alum, leaving the free sulphuric acid in solution. The re-
mainder of the alum and the excess of ammonium sulphate are

precipitated by alcohol.
i
grms. of aluminium sulphate are dissolved in 5 c.c.
or 2
of water, the solution being treated with 5 c.c. of a saturated
solution of (NH 4).2 SO 4 then shaken up frequently during
,
hour, and afterwards treated with 50 c.c. of 95 per cent, alcohol.

After filtration and washing with 50 c.c. of alcohol the filtrate
and washings are evaporated on the water bath, taken up with
water, and titrated with J^-normal soda in presence of phenol-
phthalein.
Lunge regards this method as the most exact.
The method consisting in the direct titration of the substance
with tropeolin oo, methyl orange, etc., is inaccurate (H. de
Keler and G. Lunge, Monit. Scient., i
896, p. 40).
CHAPTER VIII
IRON
I. ANALYTICAL CHARACTERISTICS OF IRON SALTS
169. General Reactions of the Iron Salts. A. FERROUS

SALTS. These salts are generally pale green when hydrated,
white when anhydrous. They are thrown down from solution,
by potash a white precipitate, turning green, and
or soda, as
finally brown, and insoluble in an excess of the reagent. Owing

to the influence of the air it is difficult to obtain the precipitate
quite white, unless the experiment is madein a glass through
which a current of carbon dioxide is passed for several minutes.

A similar precipitate, insoluble in excess, is also furnished by
ammonia.
An alkali carbonate, poured into a solution of a ferrous salt,
gives a white precipitate of carbonate, of low stability, which rapidly

parts with CO 2
and undergoes the same transformations as the
hydroxide.
Sulphuretted hydrogen gives no precipitate with ferrous salts
so long as they are acid, but ammonium sulphide gives a black
precipitate, insoluble in excess.
Oxalic acid and the soluble oxalates furnish a yellow pre-
cipitate of ferrous oxalate, unalterable in air, and soluble in acids.
Yellow prussiate of potash (potassium ferrocyanide) gives a

white precipitate, turning blue in air.
Red prussiate (potassium ferricyanide) gives a very deep blue

and highly characteristic precipitate.
Ammonium succinate and benzoate give no precipitate ;
neither does tannin, though in this case the liquid turns black
directly on exposure to the air.

Potassium phosphate gives a white precipitate, turning to
blue ;
and the arsenate a white precipitate, which turns green.
B. FERRIC SALTS. These are obtained by the oxidation
of ferrous salts, or by dissolving ferric hydroxide in acids. They
are deep yellow or red-brown in colour.
The alkalis, potash, soda, and ammonia give a brown
precipitate of ferric hydroxide, insoluble in an excess of the
reagent.
The alkali carbonates give the same brown precipitate of
hydroxide, CO, being liberated.
Sulphuretted hydrogen gives a finely divided white precipitate

of sulphur, the ferric salt being at the same time reduced to the
ferrous state
Fe 2 CI 6 + H S - 2 HC1 + S + 2 FeCl
2 2,
Fe 2 (SO 4 ) 3 + H S = H SO + S + 2FeSO
2 2 4 4.
Barium carbonate is able to throw down ferric oxide even in
the cold, CO 2 being disengaged, and the barium displacing iron

in the solution.
Potassium ferrocyanide gives a deep blue precipitate, whilst

the ferricyanide does not produce any. These reagents enable
the ferrous salts to be distinguished from the ferric salts.
In neutral or ammoniacal solutions a brown precipitate is
produced by ammonium succinate or benzoate.

Tannin gives a bluish-black precipitate of ordinary ink ;
and potassium thiocyanate turns ferric salts a blood-red colour.

The presence of organic matter in the solution prevents
precipitation by ammonia or potash, but ammonium sulphide
will always throw down the whole of the iron as an insoluble
sulphide.
When, as often happens, ferrous and ferric salts are present
together, the mixture may be tested with sulphuretted hydrogen,

which, in presence of a ferric salt, will give a white deposit of
sulphur. Another portion of the solution may then be tested

with potassium ferricyanide, a deep blue precipitate indicating
that a ferrous salt is also present.
170. Estimation of Iron. This may be effected by gravi-

metric, volumetric, or colorimetric methods. The last-named
24
37O CHEMICAL CHARACTERISTICS OF IRON AND ALUMINIUM
having been already described in the analysis of aluminium

sulphate, need not be further discussed now.
For gravimetric determinations the whole of the iron is
peroxidised by means of HNO 3, chlorine, aqua regia, bromine,

etc. On boiling the liquid and adding NH 3,
the iron comes
down as hydroxide, which is collected, decanted, and washed
until free from all soluble salts ;
after which it is dried and
removed from the filter, the latter being then calcined separately.
To counteract any reduction of the iron adhering to the filter by

the carbon formed during calcination, the residue is treated with
a little HNO 3,
then evaporated, calcined afresh, and united to
the main precipitate, which is afterwards calcined, cooled, and
weighed.
If the iron is in the condition of nitrate, this method is very
accurate ;
the state of chloride, the precipitate will have
but if in
to be washed until the washings cease to react in presence of
silver nitrate. In the absence of this precaution volatile ferric

chloride will be formed during calcination, and will falsify the
results.
When the iron cannot be isolated by NH 3 as, for instance,
in presence of citric acid, tartaric acid, or other organic bodies

ammonium sulphide is employed as precipitant, the iron sulphide
being collected, washed, calcined, and weighed. The results will
be accurate, provided the amount of sulphide is small other- ;
wise the calcination residue must be taken up with HC1 and
re-precipitated with ammonia.

The method most generally used, however, is the Marguerite
titrimetic method, based on the action of potassium permanganate.
This salt oxidises ferrous salts in dilute acid solutions, and con-
verts them into ferric salts, being itself decolorised and broken
up manganese and potassium.
into salts of
When the reaction is complete, the end point is shown by the

persistent rose-red coloration produced by a single drop of the
reagent in excess
i oFeSO 4 + 8 H SO 4 + K 2 Mn 2 O 8
2
= 5[Fe 2 (S0 4 ) 3 ]+ K S0 + 2 MnSO + 8H

2 4 4 2
O.
The reagent employed is a solution containing 4 to 5 grms.
of pure crystallised permanganate per litre. This is run into a

burette graduated in cubic mm., and is standardised to ascertain
the volume required to peroxidise a given weight of iron.
For this purpose about 3 to 4 dgrms. of very pure iron wire,
in small fragments, are dissolved by heat in a 100 c.c. flask con-

taining water and 5 to 6 grms. of H SO 2 4. Ferrous sulphate is
formed and hydrogen liberated, the latter escaping through a

tube traversing the cork. When all the metal is dissolved the
solution is placed in a porcelain capsule, the flask washed with
cold distilled water, and the whole made up to 300400 c.c.
The permanganate is then run in from the burette, with constant
stirring ;
the red drops disappear rapidly at first, and the hitherto
colourless liquid turns yellow owing to the conversion of the
ferrous sulphate into the ferric state. Soon the reaction becomes
slower,and the permanganate must be added with care so as to
enable the operator to judge at which drop the red coloration
becomes permanent despite the stirring. The volume consumed
isthen read off and calculated to unity, i.e. to I grm. of iron.
This being done, \ to I grm. of the substance under ex-
amination (according to the presumed richness in iron) is
dissolved in boiling HC1 and evaporated with 5 to 6 grms. of
H SO 2 4untilwhite fumes begin to appear, whereupon the mass
is cooled and taken up with water. The resulting solution
generally contains the iron as ferric sulphate, and has to be
reduced to the ferrous state before the permanganate can react.
This conversion is best effected by adding granulated zinc, the
nascent hydrogen thereupon liberated reducing the iron salt.
As soon as the liquid becomes decolorised it is transferred to a
white capsule, and acidified if necessary, after which it is diluted,
and titrated as already described.
Provided the above conditions be strictly maintained, this

method is very accurate ;
but it is only suitable for cases where
the iron alone has to be estimated.
In place of metallic iron, which always contains 0-3 to 0-4
per cent, of carbon and other impurities, the double sulphate of

iron and ammonium
FeS0 4 + (NH 4) 2 SO 4 + 6H 2 O
is employed for standardising the permanganate reagent. This
sulphate is obtainable pure, keeps without changing, and, as it

contains just f of its own weight of iron, all that is necessary
for the rapid standardising of the permanganate is to dissolve
2 to 2*5 grms. of the sulphate in 300 to 400 c.c. of pure cold
water and 5 to 6 grms. of free sulphuric acid.
171. Separation of Iron from other Metals. To separate

iron from the alkali metals, it
peroxidised and thrown down by
is
ammonia. The filtrate and washings are united, and calcined to

drive off ammonium salts, the alkali metals being left in the
residue.
When barium and strontium are present the same treatment

is applied, except that the iron oxide precipitate should be
re-dissolved and re-precipitated if there is any risk that it has
carried down traces of these alkaline earths. If, on the other
hand, the latter are first thrown down by sulphuric acid, a good
deal of the iron is carried away and cannot be entirely recovered,
even by washing in boiling concentrated HC1. The same applies
when calcium and magnesium are present, provided there be an
excess of ammonium salts in the solution. In such event the
method based on the decomposition of the nitrates already
indicated in the case of aluminium and calcium may be
utilised to advantage. The iron remains in the state of per-
oxide, insoluble in ammonium nitrate, whilst the lime and
magnesia are entirely dissolved.
To determine iron in presence of aluminium, they are pre-
cipitated together by ammonium sulphide, then calcined, oxidised
by nitric heated again and weighed, after which they are

acid,
re-dissolved in HC1, evaporated with H 2 SO 4 and the iron titrated ,
with permanganate.
Another method consists in reducing the mixture of the two
oxides by hydrogen at red heat and taking up the residue with
very dilute nitric acid, which dissolves out the iron alone. This
treatment is also
applicable in presence of chromium oxide.
Iron can also be separated from manganese, cobalt, nickel,
etc., by precipitation as peroxide by barium carbonate out of
contact with air.

Finally, when iron peroxide, alumina, manganese oxide, cobalt

oxide, etc., are present in the same solution, the usual mode of
analysis is to throw down the iron and aluminium as acetates.

The hydrochloric acid solution is greatly diluted, and saturated
with sodium carbonate until the liquid turns red and loses its
transparence, whereupon it is treated with an excess of sodium

acetate and boiled. The iron and alumina separate as insoluble
basic acetates, leaving a clear, colourless solution. The precipi-
tate is with the usual precautions and calcined, the
collected
resulting oxides being weighed. The manganese will be found

in the filtrate, and can be thrown down by bromine or ammonium
sulphide.
All the metals precipitable by sulphuretted hydrogen in acid
solutions are readily separated from iron by this reagent.
2. ANALYSIS OF CERTAIN FERRUGINOUS PRODUCTS
172. Analysis of Pyritic Lignite. The substances to be

estimated are :
moisture, insoluble matter, ferrous sulphate, ferric
sulphate, aluminium sulphate, total H SO2 4, iron disulphide.
I. Moisture. A portion of the sample is finely powdered, and

2 grms. are then dried at 1 00 C. until of constant weight.
II. Insoluble Matter. Another 2 grms. are treated for this

purpose, and washed with hot water as quickly as possible in
order to prevent oxidation of the sulphide. The clear liquids

are united and made up to a definite volume, the residue being
dried and weighed.
III. Ferrous Sulphate. This is titrated with permanganate
on an aliquot portion of the solution. Owing to the presence of
organic matter, which decolorises the permanganate after all the
iron has been oxidised, the end point is not well defined. For
its better detection a few drops of the solution are taken at
intervals and tested with ferricyanide, the absence of the char-
acteristic blue precipitate indicating complete oxidation of the
iron. The result is calculated in terms of ferrous sulphate.

IV. Ferric Sulphate. A portion of the liquid is reduced by
means of zinc, and then titrated with permanganate. The differ-
3/4 CHEMICAL CHARACTERISTICS OF IRON AND ALUMINIUM
ence between this result and that of the preceding test gives the
amount of iron in the ferric state, and from this the quantity of
ferric sulphate is calculated.
V. Aluminium Sulphate is determined by precipitation with

sodium thiosulphate.
VI. Total Sulphuric Acid. A portion of the clear solution
is acidified by HC1 and precipitated with barium chloride, the
barium sulphate being collected with the usual precautions.
VII. Iron Disulphide. One grm. of the very finely powdered
substance is treated with aqua regia on the sand bath at moderate
heat, the acid being renewed as evaporation progresses. Finally,

greater heat employed, a few crystals of potassium chlorate
is
being added from time to time. Under these conditions the

sulphur is oxidised to sulphuric acid. After the excess of nitric
acid has been expelled by heat the mass
is taken
up with water,
filtered, and washed, a portion of the solution being tested to
determine the sulphuric acid present. On deducting the figures
from the preceding test, the remainder gives the sulphuric acid
corresponding to the unoxidised sulphur in the substance. This
is then calculated to iron disulphide.
173. Analysis of Ferrous Sulphate. As a rule the iron

alone is estimated, in the form of ferrous sulphate, by simply
dissolving the salt, acidifying with H,SO 4 and
, titrating with
permanganate. If the insoluble matter ferric sulphate, total

H SO 2 4 ,
etc. are also to be determined, this is done by the
methods already described.
174. Analysis of Ferric Sulphate. Substances to be de-
termined :
moisture, insoluble residue, soluble ferric sulphate,
soluble H SO 2 4, free H SO
2 4 .
I. Moisture. Five grms. are dried in the oven till constant.

II. Insoluble Residue. Five grms. are extracted with hot
distilled water, the residue being washed until the liquid ceases
to give a precipitate with barium chloride. This residue is dried
and weighed.
III. Soluble Ferric Sulphate is estimated by titration with
permanganate after the reduction of a portion of the above

solution by means of zinc.
IV. Soluble H.2 SO. An aliquot part of the solution is
acidified with HC1. The iron is then thrown down by am-

monia, and is washed, dried, and weighed. The weight should
correspond to that of the ferric sulphate. In case of difference,
search must be made for alumina, lime, etc.
The clear liquid, acidified by HC1, is used to estimate the
H SO2 4 by means of barium chloride.
V. Free H SO 2
is ascertained in an approximate manner by
deducting the combined H 2 SO 4 from the total.
175. Analysis of Rouil Mordant. The estimation usually
includes sulphuric acid, ferrous sulphate, total iron, and soda.
I. Sulphuric Acid. This is estimated by means of barium
chloride after the iron has been thrown down by ammonia, or
even before such precipitation. In the latter event the results
are accurate enough for practical purposes, even though a little
iron be carried down by the precipitate. In either event the

solution must be acidified with HC1 before the barium chloride
is added.
II. Ferrous Sulphate is readily estimated by the permanganate
method, 10 c.c. being made up to 100 c.c., then strongly acidified
with H SO 2 4,
and titrated until a permanent rose-red tint appears.
III. Total Iron. Some

necessary owing to the precaution is
almost invariable presence of small quantities of nitrous products,

free HNO
3 etc., which bodies are also reduced by zinc and
,
falsify the by their influence on the permanganate. To

results
remove or destroy them, 10 c.c. of the substance are boiled with

2 to 3 c.c. of H 2 SO 4 and evaporated to near dryness.
,
The mass
isthen taken up with water, reduced with zinc, and titrated in
the usual manner, the result giving the total iron.

IV. Soda. This may be estimated as chloride after the
metals and H SO
2 4
have been removed. This method is, how-
ever, cumbrous, and may be replaced by the following, which gives
results near enough to show the quality of the substance.
Ten c.c. of the Rouil liquor are treated with an excess of
normal soda, a note being taken of the quantity used. The
liquid and precipitate are then made up to 500 c.c., shaken, and
filtered. 100 to 200 c.c. of the filtrate (= i or 2 c.c. of original
liquor) are collected, and the excess of soda titrated with normal
sulphuric acid, the difference giving the amount of H SO
2 4 relat-
ing to the bases precipitable by soda. On deducting this
from the total H SO

2 4,
the remainder is calculated to sodium
bisulphate.
FINIS
INDEX
ACHMITE
...... PAGE
I3 1
Albite .
Alizarin lakes
.
.........
Agriculture, use of ferrous sulphate in
.......... . . . . . . .
-57
329
294
Allophane
Almandine garnet
Alum, ammonia
,, ,,
........
.........
basic
.
.
.
.
. .
.
.
.
. .
.
.
.
-37
.130
35, 171
54
,,
,,
.,
.,
cake.
ferri-ammoniuni
ferri-potassium
general remarks
........ .
.
.
.
.
.
.
.
.
.
.
and alum manufacture)

.
.
.
.28
137
101
101
Tiianufacture (see also Ferrous sulphate 163, 226
....
,, .
,, ,, from alunite . . . . . .
.173
,, ,, ,, clay, kaolin, bauxite, etc. 165
,, .. ,, pyritic shales and lignites . . . .182
,, ,, ,, shale, Spence method . . . .
.171
',, ,, La Tolfa process . . . . .
173
,, ,, Pommier process . . . . J 73
,, ,, present method . . . . . .
.175
,, ,, ,, attacking mineral . . .
.176
,, ,, ,, ,, and purifying the alum
crystallising .
.179
,, ,, ,, ,, preparation of mineral . . .
.176
,, ,, ,, ,, treatment of mother liquor for aluminium
.181
.......
. .
sulphate . .
31
....
. .
,, potassium . . . . .
,, ,, anhydrous 33
., ,,
......
....
basic .34
........ calcined 32
. .
,, ,,
Alum, Roman
Alum, sodium
Alumiane
Alumina
........
..._...
...
. .
.
.48
.
33, 35
37, 167
16
....
crystalline
.18
.........
!
hydrated . 7
occurrence . . . . . .18
...... ...
soluble 17
Alun inates . . . . . . . . 18, 47
Aluminium I
Aluminium and
Applications
Use
....
iron sulphates
in manufacturing Xordhausen sulphuric acid

mixed-
. .
342
34 2
Use in purifying waste waters . . 345

378 INDEX
PAGE
........
Aluminium compounds (see also Alums and Aluminates) . . 10
.11
,,
,,
arsenate
arsenite ........
Aluminium and sodium fluoride (cryolite)
.....
. .
41
41
bromide
.......
1
, ,
. . . . .
5
........
,, chlorides . . 12
,,
,,
dithionate
fluorides
double
........
...
........ .16
15
38
10
.....
iodide
,,
,,
,,
nitrate
nitride
oxide (see
.
......
...
Alumina)
38
38
16
39. 5 1
....
,, phosphates.
..... ...
,.
silicates . . . . . . . .
41, 52
21, 48
....
.
,, sulphates
,, sulphides
. . 20
........
,, sulphites
21
Aluminium, estimation of
...... 354
. . . .
Aluminium manufacture 2
,, ,,
chemical methods
...
... Castner process
2
2
....
,, ,, ,, ,,
Grabau process
.....
,, ,, ,, ,. 5
,, ,, ,, Netto process 3
...
,,
,, ,, electrolytic methods 6
,, ,, ,, ,, Cowles process . 6
6
......
,, ,, ,, ,, Heroult process . .
.......
,, ,, ,, ,,
Minet process . .
7
........
in laboratory I
Aluminium, preparation
I
, , preparation, historical
.........
,, properties
8
separation for analysis from other metals
...... 354
. . . .
,,
......
uses 9
uses for purifying metals 10
.... ....
,,
Aluminium minerals 42
Aluminates
Containing fluorine
Hydroxides
...
.... . .
47
42
45
-43
Oxides.
.........
. . . . . .
Phosphatic . . . . . > .
51
Silicates 5*
Sulphatic
Aluminium salts, general
Aluminium sulphate
.
... ... ..... ...

.
reactions
. .
'
. . .
353
21,48, 134, 181
.48
do. manufacture from alumina . . 140
do. manufacture from argillaceous and pyritic lignites .
139
do. manufacture from bauxite . . . .
140, 146, 159
do. do. chemical treatment . . . .
.150
do. do. concentrating the liquor . . . . J
55
do. do. preparation of mineral . . . .
.147
do. do. treatment of finished product 157
....
. .
do. manufacture from clay, shale, and sulphurous acid 135

. .
do. manufacture from cryolite 140

do. manufacture from kaolin and sulphuric acid .
135
do. manufacture, Pommier process . . .181
INDEX 379
380 INDEX
Barium ferrite . . . . . . . . . .82

Basic ferric sulphate.
Bauxite
,,
.
grinding mills for

Bleaching, use of alum in
........
See Rouil mordant.
.18, 45, 140
147
.....
. k . . . . . .
307
Bog ore
Boles and ochres
Botryogene
.
.
...
.'
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.119
.124
54
Buisine method. See Ferrous sulphate manufacture.

,,
CACOXINE
Calcium
.........
process.
........
........
ferrite
See Ferric sulphate manufacture.
Capuchin red
........
.........
Carlx>nising wool, use of aluminium sulphates in
Castner process
......
.
Ceylanite
Cbadwyk and Kynaston
Chalcopyrite
Chlorite
........
......... process
...
Chlorophoeite
Chlorospinel
Chrome ochre
........
.
......
. .
Chlorosis in vines, treatment with ferrous sulphate
........
.
Chrysoberyl
Clays ... ....
, ,
,,
Cochineal lake ........

analysis of
.........
smectic
.........
. . . . .
...
........
Colcothar
Copiapite
Copper ferrite
Coquimbite . . . . .
........
Corundum . . . . . . . . .
,,
Cowles process
Cronstedtite ........
preparation
.........
.....
. . .
Cryolite
........
Cutting rake for aluminium sulphate
Cymophane
.........
DlASI'ORE
.....
,,
Dufrenite
,,
.........
Disinfection, use of ferric sulphate in
ferrous sulphate (Rabot's method)
EMERALD
Emery
.........
Dyeing, use of iron sulphates in
....
......... . .
Epidote
Estimations of iron.
FAHLBERG
Fayalite
.......
........
.........
process
See Iron, estimation.
Felspars
Albite .
INDEX 381
Felspars Andesine ........

.........
.........
PAGE
56
.........
Anorthite
56
.........
Labradorite
56
......
Oligoclasc 57
Orthose
57
Ferri-ammonium alum
,,
Ferri-potassiurn fluorides
Ferri-sodium fluoride
Ferric acid
........
........
fluoride . . . . . . .
101
.65
65
65
. . . . . . . . . . 82
Ferric compounds. See Iron compounds.
Ferric salts, general reactions
.......
. . . . . .
368
Ferric sulphate, basic. See Rouil mordant.
Ferric sulphate manufacture
.....
...... Buisine process
266
268
.....
,, ,,
,) introduction 266
266
.....
, > , ,
Marguerite process
,, ,, ordinary peroxidation process . . .
267
Rohart process
....
,, ,,
267
Ferric sulphate, applications in dyeing
......
. . . . .
331
use as antiseptic and disinfectant
....
,, 334, 337
in coagulating blood
,. ,,
337
,, ,, preserving anatomical specimens 336
Ferrites
,,
Ferro-ammonium sulphate
,,
........
purifying waste liquors, drainage waters, etc.
........
.
........
. . . . .
.
.
.
.81
338
96
Ferro-ferric chloride
,,
,,
hydrate
oxides .........
........
........
67
75
74
,. sulphates
Ferro-potassium chloride
,,
,,
........
........
........
fluorides
sulphates
97
66
64
96
.......
Ferro-sodium sulphate 96
See Iron compounds.
......
Ferrous compounds.
......
Ferrous salts, general reactions 368
Ferrous sulphate and alum manufacture 183
do. from pyritic lignites 193, 205
do. construction and upkeep of plant
.....
do. . . .
247
do. do. do. autogenous soldering 249
....
. . .
do. do. cost price of alum 235

do. do. general manufacturing account 246
do. do. improvements possible in the process . . .
254
do. do. the ore or raw material . . .
.197
do.
do.
do.
do.
do.
do.
do.
do.
do.
composition
enrichment
.
.
.
method of working deposits

... .
.
.
.199
.
255
201
do. do. do. preparation . . . 202
do. do. lixiviation of the ore . . . .
205
do. do. concentration of liquor .
214
do. do. and purifying the ferrous sulphate .219
....
crystallising .
do. do. re-crystallising the ferrous sulphate . .

225
do. do. PSR crystals (ferrous sulphate) 225
do.
do.
do.
do.
the residual liquor, mould on
do. treatment for alum .... . . . 226
227
382 INDEX
Ferrous sulphate and alum manufacture From pyritic lignites, treatment of crude
.... alum . . .
.236
do.
do.
do.
do.
do.
do.
do.
from shale
do.
do.
........
yield of
.....
alum
theory of systematic lixiviation
....
lixiviation of roasted ore
treatment of liquor
.
. . .
233
258
190
192
193
do. weathering and roasting of ore
do. . . .
192
Ferrous sulphate manufacture (see also Ferrous sulphate and alum manufacture) .
183
,, ,, from iron and sulphuric acid . . .186
,, ,, native ores
...
. . . . .186
184
....
,, ,, pyrites. .
.185
....... Spence method .
,, ,, ,,
.310
......
Ferrous sulphate, uses
.
,, ,, as fertiliser 328
......
,, ,,
insecticide 325
,, ,, mordant on cotton, silk, and wool . .
.310
,, ,, in agriculture 320
destroying dodder .321
.....
. . . .
,, ,,
,, ,, ,, moss . . . . .
.321
......
,, ,, ,, weeds 326
,, ,, disinfection . . . . .
317
,, ,, indigo dyeing 311
,, ,, manufacture of other iron mordants . .
.311
,, ,, ,, Mars or martial pigments . .
314
,, ,, ,, Nordhausen sulphuric acid . .
317
,, ,, ,, pigments. . .
313
,, ,, ,, Prussian blue . . .
313
,, ,, ,, writing inks . . .
315
,, ,, metallurgy of gold . . . .
317
,,
,,
, ,
,,
,,
, ,
microbiology
photography
preservation of
...
.
manure.....
. . , .
315
316
328
,, ,, purifying lighting gas . .
318
........
treating vine and other plant diseases .321
. .
,, ,,
Fibro-ferrite . . . . . . . .
.123
Fixing or dunging dyes 289
Fluellite
Fluo-aluminic acids
...
Flesh colours on porcelain
.
.
.
.
. . . . .
.
.
. .
.10
315
42
Franklinitc .119
....
. . . . . . . .
GAHNITE
Gibbsite
...
.......... .
19, 47
18
Glauconite . . . . . . . . .
133
Gcethite .
.........
Grabau aluminium process
Green lakes
.
. . .
297
119
5
HAEMATITE
Halloysite
Hedenbergite
....... .
.
.
. . . . . .
.
.
116, 118
.54
.130
..........
Hennebutte and Ue Vaureal sewage process
Heroult aluminium process
Hercytine
.
. .
.
308
6
19
INDEX 383
...... VAGE
........
Hides and leather industry, use of alum 299
Hisingerite . . . . . . . . . .128
Homburg's pyrophore 33
Ilypersthene . . . . . . . .
.130
ILMENITE
Ilvaite
Indian yellow
Ink.
.
..........
......... . . . . . . . . .118
131
299
315
........
Iron 59
, , atomicity of . . . . . . . . .62
,, chemically pure 59
Iron compounds (see also under Ferri- and Ferro-) . . . .
.63
Arsenates . . . . . . . . . in
Arsenides . . . . . . . . in
Arsenites . . . . . . . . . in
Borates
Boride
Bromates
Bromides
Carbides
.
.........
.
.
.........
. .
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.115
.115
.112
72
72
Carbonates
Chlorates
Chlorides
,,
.........
.
double........
.....
intermediate
.
.
.
.
.
.
.
.
.
.
.
.
.
.
.113
.71
65-71
70
66
,,
Double
Fluorides
Fluosilicates
salts.
.........
.
See Ferri- and Ferro-.
....
....
. . . . . . . .
63, 64
64, 65
Hypophosphites
Hyposulphite
lodates .........
.........
.
.....
.
.
107
91
73
Iodides
Nitrates
Nitride .........
.........
.
72
104
103
Nitrosulphides
Nitrosulphocarbonate
...... . . . . . . .
.114
-73
87
Oxides
,,
Oxychlorides
Perchlorates
Periodates
hydrated
.........
.........
.........
. . . . . .
74, 75, 78
70
72
73
.107
.......
.
Phosphates . . . . . . .
.......
Phosphides . . . . . . . 106
.107
Phosphites
Seleniates
......
...... .103
.102
......
Selenide
Selenite .103
.....
Silicates . .
114
.112
Sulpharsenates
Sulpharsenites
Sulphates .......
.....
....
.112
-99
91
Sulphides
,, basic
.........
double 96, ioi
84
384 INDEX
Iron compounds Sulphites

Sulphocarbonates
Tellurites
Tetrathionate .
Thiosulphates .
Iron, estimation in aluminium sulphate

., ,, alunite .
,, ,, bauxite,
clay .
,, ,, ferruginous products
,, ,, iron salts
Iron ores .
Arsenical
Carbonate
Oxides
Phosphatic
....
Silicates
Sulphatic
Sulphidic
preparation in laboratory
properties, chemical
.....
.
,, physical .-
salts, general reactions
separation from other metals in analysis

See Ferric and Ferrous sulphate manufactures, etc.
KAOLIN
,,
sulphates.
......
....
analysis of
Kessler process. See Sodium alum.
Knebelite ,,
LABRADORITE
Lac lakes
.....
......
Lake pigments, manufacture
La Tolfa alum process
Lemery's volcano .....

Leather industry, use of aluminium sulphates in the
.....
......
Lencauchez sewage process
Lepidocrocite
Lievrite
Lime washes, use ...
...... alum
.....
of in
......
Limonite
Lithomarg'e
Loewigite
....
Luteoline in lake pigments
MADDER lakes .....

....
Magnesium aluminate
,, .....
ferrite
Magnetic oxide of iron

,,
Magnetite
Manganese
.....
pyrites
ferrite . . .
Manufacture of alum. Sec Alum manufacture.

INDEX 385
Manufacture of aluminium
r , , ,
.
sulphate.
.
See
. . .
Aluminium sulphate manufacture.

. .2 PAGE
,, ,, general remarks . . .
.134
,, basic ferric sulphate. See Rouil mordant.
,, ferrous sulphate. See Ferrous sulphate.
,, ,, and alum . . . . .
.190
,, lake pigments . . . . . .
291
Marcassite . . . . . . . . . 122
Mars orange
........ .
315
. . . . . . .
'
,, violet . . . . . . . . . .
315
,, yellow 298, 315
Martite . . . . . . . . . .118
Medicine, use of alum and aluminium sulphate in . . . .
307
.123
......
Melanterite . . . . . . . .
Mineral blue
Minet aluminium process
.........
Microbiology, use of ferrous sulphate in
........
Mildew, use of ferrous sulphate for .
. . . . .
.316
321
298
7
Mispickel .. . . . . . . .
.125
........
Moss, destruction by ferrous sulphate .321
. . . . .
NETTO aluminium process 3

.161
........
Newiand's process . . . . . . . .
Non-inflammable fabrics . . . . . . .
306
wood
Nontronite
,,
......
.
Nordhausen sulphuric acid manufacture

. . . . . . .
306
55, 128
342
OCHRES
,,
Oligoclase felspar
.
chrome.........
.........
.
.
.
.
.
.
.
.
.
.
.
. .
.
.
-54
54
-57
.......
Orthose felspar 57
PAPER-MAKING,
Peridote ..........
.......
use of alum in
.126
301
128
......
Pharmacosiderite . . . . . . . .
Photography, use of alum in 307

,,
Physalite
Picotite ..........
.
,,
........
.
ferrous sulphate in
. . . . . . .
.43
.118
316
47
........
Pisolitic ore . . . . . . . . .
alum
Plaster, use of
......
in 303
Pleonaste .47
Pommier alum .173
Potassium alum
......
.........
process
. . . . . . . .
.31
.19
,,
,.,
Prussian blue
.........
aluminate
.........
ferrate
ferrite
83
81
.....
298
.156
Pycnite
Pyrites
........
Pulveriser for aluminium sulphate
Purification of sewage and waste waters
..... . .
.
...
. . . . .
37> 33^ 345

.43
86, 121
.86
,,
Pyrophysalite
magnetic
25
... .43
386 INDEX
I'AGE
Pyrrhosiderite . . . . . . . .
.119
.120
Pyrrhotine
.......
. . . . . . . . .
RABOT'S method of disinfection
Red and rose lakes

Redwood
.........
Rassiguier's treatment of disease in vines
...
...
. . . . .
.321
317
294
......
lake . . . . . . .
297
Roman alum
...... 33. 35
.
Rouil acetate
...... 271
.
,, aceto-nitrate . .
271
,, mordant . .
270
.281
.......
,, ,, characteristics . . . .
Rouil mordant manufacture .271

.....
. . . . .
do. Geschwind process 278

do.
do.
do.
do.
do.
do.
.... dissolving the sediment
sodium nitrate
do.
use of sodium nitrate ..... 279
280
278
do. nitric acid method . . . . . .
.271
do. do. insoluble basic sediment 277
....
. . . . .
do. do. plant . . . . . .

.271
do. do. recuperation of nitrous products 274
Rouil nitrate . . . . . . . .
,271
,, sulphate . . . . . . . . .
270
SAPPHIRE ......
...... 44
. .
Sewage treatment, Hennebutte and De Vaureal process
..... 308
. . .
,, Lencauchez process 308

use of alum in .
307
...
, ,
,, ,, ferricsulphate in . . . .
336
......
,, ,, ferrous sulphate in . . . .
317
Siderose .
Silk dyeing, use of iron sulphates in

Smectic clays
Sodium alum manufacture
.........
. .
.
.
.
.
.
.
.
.
.
.
.
.
.
113, 126
.167
332
53
,, aluminate . . . . . . .
.19, 292
...
,,
,,
,,
ferrate
ferrite
stannate
Spathose iron ore

Spence process, alum manufacture
'
.
.
.
.
.
.
.
.
....
.
...
.
.
.
.
.
..
.
.84
.8:
113, 126
.171
292
,,
ferrous sulphate manufacture . .
.185
Spinels
.....
... 19, 47
. .
,,
Stil
iron
de grain lake
Stilpnomelane
.
...
.
.
.119
.132
294
TAWING
Thenard blue .........
hides and leather . . . . . ... .
300
298
Topaz
Trip-hammer
Triphylline
Triplite
..........
.
..........
mill .
...
.
.157
44
124
125
Troilite
Turgite
Turquoise ..........
.
.
.
.
.
.
.
.
.
. . . . .
78,
121
119
52
INDEX 38;
VINES, treatment
Violet lakes
Vivianite
.......
........
for disease .
.
.
PAGE
321
297
WASTE ....
liquors, purification by alum
124
308
........
iron sulphates
,, ,, ,, 338
........
Waste waters, purification by mixed aluminium and iron sulphates 332
Wavellite
....
51
........
Websterite .
48
........
Weeds, destruction by ferrous sulphate 321, 324
Weld
.......
lake 293
Wichtine 132
Wolkouskoite 55
Wool
YELLOW
Yenite
lakes .......
dyeing, use of iron sulphates in
........
332
293
ZINC ferrite 82
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VEGETABLE PATS AND OILS: Their Practical Prepara-

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"This knowledge is conveyed with characteristic German thoroughness in this useful svork
of Herr Andes, which loses nothing of clearness in Mr. Sailer's excellent translation. The
causes of rust formation are examined, the proper methods of cleansing the ironwork detailed,
and the constitution and application of suitable preventative coverings explained. . . The
.
book is a welcome contribution to technological literature, and will be found worthy of the
careful study of all who are professionally engaged in the arrangement or superintendence of
the class of work dealt with." II 'estit -n Daily Mercury.
"The author explains the nature of rust and its formation, and the text is illustrated from
about fifty photographs. An immense amount of carefully arranged information follows as to
the best methods of applying anti-corrosive substances and the various pigments most effi-
cacious for use under all circumstances. The author has evidently thoroughly investigated and
mastered the subject of iron corrosion, its cause and its prevention and we regard his book as
;
of the greatest importance to bridge-builders and makers and users of structural iron and
steel. The book is illustrated throughout and is admirably indexed and arranged." Iron and
Steel Trades Journal.
" It is of the utmost
importance to have reliable information on the various so-called infal-
lible anti-corrosive paints which flood the market, and the large experience which evidently had
been gained by the author in relation to the subject enables him to present in the work under
notice an important contribution towards the solution of the problem involved, which is bound
to prove extremely serviceable not only to paint manufacturers, but to engineers, contractors,
ironfounders, shipbuilders and others. The subject is thoroughly dealt with in all its various
phases, and the vast fund of information afforded not only regarding rust formation and its
prevention, but in reference to paints, varnishes, oils and pigments generally, should prove very
valuable to the large class interested, while additional importance is given to the book by the
numerous illustrations which were prepared by the author in the course of a series of personal
experiments on the formation of rust." Builders' Reporter.
THE MANUFACTURE OF ALUM AND THE SUL-

PHATES AND OTHER SALTS OF ALUMINA AND
IRON. Their Uses and Applications as Mordants in Dyeing
and Calico Printing, and their other Applications in the Arts, Manufac-
tures, Sanitary Engineering, Agriculture and Horticulture.
Contents.
Part I., Theoretical Study of Aluminium, Iron, and Compounds of these Metals.
Chapters I., Aluminium and its Compounds. II., Iron and Iron Compounds.
Part II., Manufacture of Aluminium Sulphates and Sulphatesof Iron. Chapters III.,
Manufacture of Aluminium Sulphate and the Alums. IV., Manufacture of Sulphates of Iron.
Part III., Uses of the Sulphates of Aluminium and Iron. Chapters V., Uses of
Aluminium Sulphate and Alums Application to Wool and Silk Preparing and using Aluminium
Acetates Employment of Aluminium Sulphate in Carbonising Wool The Manufacture of
Lake Pigments Manufacture of Prussian Blue Hide and Leather Industry Paper Making
Hardening Plaster Lime Washes-Preparation of Non-inflammable Wood, etc. Purifica-
tion of Waste Waters. VI., Uses and Applications of Ferrous Sulphate and Ferric
Sulphates. Dyeing Manufacture of Pigments Writing Inks Purification-'of Lighting Gas
Agriculture Cotton Dyeing Disinfectant Purifying Waste Liquors Manufacture of
Nordhausen Sulphuric Acid Fertilising.
Part IV.. Chemical Characteristics of Iron and Aluminium. Analysis of Various
Aluminous or Ferruginous Products. Chapter VII., Aluminium.
LUBRICATING OILS, FATS AND GREASES: Their

Origin, Preparation, Properties, Uses and Analyses. A Handbook for
Oil Manufacturers, Refiners and Merchants, and the Oil and Fat
Industry in General. By GEORGE H. HURST, F.C.S. Sixty-five
Illustrations. 313 pp. 1896. Price 10s. 6d. ;
India and Colonies, 11s. ; ,
Other Countries, 12s. ; strictly net, post free.
Contents.
Chapters I., Oils and Fats, Fatty Oils and Fats, Hydrocarbon Oils, Uses
Introductory.
of Oils. II., Hydrocarbon Oils. Distillation, Simple Distillation, Destructive Distillation,
Products of Distillation, Hydrocarbons, Paraffins, Olefins, Napthenes. III., Scotch Shale
Oils. Scotch Shales, Distillation of Scotch Oils, Shale Retorts, Products of Distilling Shales,
Separating Products, Treating Crude Shale Oil, Refining Shale Oil, Shale Oil Stills, Shale
Naphtha Burning Oils, Lubricating Oils, Wax. IV., Petroleum. Occurrence, Geology, Origin,
Composition, Extraction, Refining, Petroleum Stills, Petroleum Products, Cylinder Oils,
Russian Petroleum, Deblooming Mineral Oils. V., Vegetable and Animal Oils. Intro-
duction, Chemical Composition of Oils and Fats, Fatty Acids, Glycerine, Extraction of Animal
and Vegetable Fats and Oils, Animal Oils, Vegetable Oils, Rendering, Pressing, Refining,
Bleaching, Tallow, Tallow Oil, Lard Oil, Neatsfoot Oil, Palm Oil, Palm Nut Oil, Cocoanut
Oil, Castor Oil, Olive Oil, Rape and Colza Oils, Arachis Oil, Niger Seed Oil, Sperm Oils,
Whale Oil, Seal Oil, Brown Oils, Lardine, Thickened Rape Oil. VI., Testing and Adultera-
tion of Oils. Specific Gravity, Alkali Tests, Sulphuric Acid Tests, Free Acids in Oils, Vis-
cosity Tests, Flash and Fire Tests, Evaporation Tests, Iodine and Bromide Tests, Elaidin
Test, Melting Point of Fat, Testing Machines. VII., Lubricating Greases. Rosin Oil,
Anthracene Oil, Making Greases, Testing and Analysis of Greases. VIII., Lubrication.
Friction and Lubrication, Lubricant, Lubrication of Ordinary Machinery, Spontaneous Com-
bustion of Oils, Stainless Oils, Lubrication of Engine Cylinders, Cylinder Oils. Appendices.
A. Table of Baume's Hydrometer B. Table of Thermometric Degrees C. Table of Specific
Gravities of Oils Index.
Press Opinions.
"The book is well printed, and is a credit alike to author, printer-and publisher." Textile
Mercury.
" be a valuable addition to the technical library of every steam user's establishment."
It will
Machinery Market.
"
Mr. Hurst has in this work supplied a practical treatise which should prove of especial
value to oil dealers, and also, though in a less degree, to oil users." Textile Manufacturer.
"This is a clear and concise treatment of the method of manufacturing and refining lubri-
cating oils. The book is one which is well worthy the attention of readers who are users
. . .
of oil." Textile Recorder.

"
We in saying that in our opinion this book ought to be very useful to
have no hesitation
all those who are interested in oils, whether as manufacturers or users of lubricants, or to
those chemists or engineers whose duty it may be to report upon the suitability of the same
for any particular class of work." Engineer.
"The author is widely known and highly respected as an authority on the chemistry of oils
and the technics of lubrication, and it is safe to say that no work of similar interest or equal
value to the general oil-selling and consuming public has heretofore appeared in the English
language." Dnigs, Oils and Paints, U.S.A.
"
This valuable and useful work, which is both scientific and practical, has been written
with a view of supplying those who deal in and use oils, etc., for the purpose of lubrication,
with some information respecting the special properties of the various products which cause
these various oils to be of value as lubricants." Industries and Iron.
" A mere
glance at the table of contents is sufficient to show how various are the conditions
to which these materials have to be applied, how much knowledge is required for the selection
of the right kind for each particular purpose, and how by processes of mixture or manufacture
the requisite qualities are obtained in each case." Manchester Guardian.
6
THE MANUFACTURE OF VARNISHES, OIL RE-

FINING AND BOILING, AND KINDRED INDUS-
TRIES. Describing the Manufacture of Spirit Varnishes
and Oil Varnishes Raw Materials Resins, Solvents and Colouring
; :
Principles Drying Oils their Properties, Applications and Prepara-

;
:
tion by both Hot and Cold Processes; Manufacture, Employment and

Testing of Different Varnishes. Translated from the French of ACH.
LIVACHE, Ingenieur Civil des Mines. Greatly Extended and Adapted
to English Practice, with numerous Original Recipes. By JOHN
GEDDES MC!NTOSH, Lecturer on Oils, Colours and Varnishes, Regent
Street Polytechnic. Twenty-seven Illustrations. 400 pp. 1899.
Price 12s. 6d. India and Colonies, 13s. 6d.
; Other Countries, 15s.;
;
strictly net, post free.
Contents.
i. rCesins: Gum Resins, Oleo Resins and Balsams, Commercial Varieties, Source, Collec-
tion, Characteristics, Chemical Properties, Physical Properties, Hardness, Adulterations.
Appropriate Solvents, Special Treatment, Special Use. II. Solvents: Natural, Artificial,
Manufacture, Storage, Special Use. III. Colouring Principles, (1) Vegetable, (2) Coal Tar,
:
(3) Coloured Resmates, (4) Coloured Oleates and Linoleates. Gum Running Furnnce
:
Bridges, Flues, Chimney Shafts, Melting Pots, Condensers, Boiling or Mixing Pans. Copper
Vessels, Iron Vessels (Cast), Iron Vessels (Wrought), Iron Vessels (Silvered), Iron Vessels
.Enamelled), Steam Superheated Plant, Hot-air Plant. Spirit Varnish .Manufacture: Cold
Solution Plant, Mechanical Agitators, Hot Solution Plant, Jacketted Pans, Mechanical
\gitators, Clarification and Filtration, Bleaching Plant, Storage Plant. Manufacture, Char-
acteristics and Uses of the Spirit Varnishes yielded by Amber, Copal, Dammar, Shellac,
:
Mastic, Sandarac, Rosin, Asphalt, India Rubber, Gutta Percha, Collodion, Celluloid, Resin-
fltes, Oleates. Manufacture of Varnish Stains. Manufacture of Lacquers. Manufacture of
Spirit Enamels. Analysis of Spirit Varnishes. Physical and Chemical Constants of Resins.
Table of Solubility of Resins in different Menstrua. Systematic qualitative Analysis of
Resins, Hirschop's tables. Drying Oils: Oil Crushing Plant, Oil Extraction Plant, Individual
Oils, Special Treatment of Linseed Oil, Poppyseed Oil, Walnut Oil, Hempseed Oil, Llamantia
Oil, Japanese Wood Oil, Gurjun Balsam, Climatic Influence on Seed and Oil. Oil Refining
Processes, Thenard's, Liebig's, Filtration, Storage, Old Tanked Oil. Oil Boiling Fire Boil- :
ng Plant, Steam Boiling Plant, Hot-Air Plant, Air Pumps, Mechanical Agitators, Vincent's
Process, Hadfield's Patent, Storer's Patent, Walton's Processes, Continental Processes, Pale
Boiled Oil, Double Boiled Oil, Hartley and Blenkinsop's Process. Driers :
Manufacture,
Special Individual Use of (1) Litharge, (2) Sugar of Lead, (3) Red Lead, (4) Lead Berate,
(5) Lead Linoleate, (6) Lead Resinate, (7) Black Oxide of Manganese, (8) Manganese Acetate,
(9) Manganese Borate, (10) Manganese Resinate, (11) Manganese Linoleate, Mixed Resinates
and Linoleates, Manganese and Lead, Zinc Sulphate, Terebine, Liquid Driers. Solidified
Boiled Oil. Manufacture of Linoleum. Manufacture of India Rubber Substitutes. Printing
Ink Manufacture. Lithographic Ink Manufacture. Manufacture of Oil Varnishes. Running
and Special Treatment of Amber, Copal, Kauri, Manilla. Addition of Oil to Resin. Addition
of Resin to Oil. Mixed Processes. Solution in Cold of previously Fused Resin. Dissolving
Resins in Oil, etc., under pressure. Filtration. Clarification. Storage. Ageing. Coach-
makers' Varnishes and Japans. Oak Varnishes. Japanners' Stoving Varnishes. Japanners'
Gold Size. Brunswick Black. Various Oil Varnishes. Oil-Varnish Stains. Varnishes for
" Enamels ". India Rubber Varnishes. Varnishes
Analysis Processes, Matching. Faults in
:
Varnishes: Cause, Prevention. Experiments and Exercises.
Press Opinions.
"There is no question that this is a useful book." Chemist and Druggist.
" '
The different formula; which are quoted appear to be far more practical than such as
'
are usually to be found in text-books and assuming that the original was published two or
:
three years ago, and was only slightly behindhand in its information, the present volume gives
a fair insight into the position of the varnish industry." The Ironmonger.
Letter from the Teacher of a Technical Class.

" As a teacher have often been consulted as to the best work on Varnish Manufacture
I
and kindred and have been at a loss in recommending a really practical one. It is
industries,
therefore with pleasure that I can now testify as to the merits of the book on these subjects
by A. Livache and J. G. Mclntosh recently published by Messrs. Scott/Greenwood & Co. In
my opinion no varnish maker ought to be without it moreover, it is the best text-book that
:
could be put into the hands of trade students or beginners. It has also the merits of being
thoroughly up-to-date and of possessing a remarkably comprehensive index. I can conscien-
tiously recommend it to my students and trade friends." CHARLES HARRISON, Lecturer on
the Manufacture of Painters' Oils, Colours and Varnishes, Borough Polytechnic, Borough
Road, S.E.
"23rd May, 1896"
THE MANUFACTURE OF LAKE PIGMENTS FROM
ARTIFICIAL COLOURS. By FRANCIS H. JENNISON,
F.I.C., F.C.S. Sixteen Coloured Plates, showing Specimens of Eighty-
nine Colours, specially prepared from the Recipes given in the Book.
136 pp. 1900. Price 7s. 6d. India and Colonies, 8s. Other Countries,
; ;
8s. 6d. strictly net, post free.

;
Contents.
Chapters I., Introduction. II., The Groups of the Artificial Colouring Matters. III., The
Nature and Manipulation of Artificial Colours. IV., Lake-forming Bodies for Acid Colours.
V., Lake-forming Bodies' Basic Colours. VI., Lake Bases. VII., The Principles of Lake
Formation. VIII., Red Lakes. IX., Orange, Yellow, Green, Blue, Violet and Black Lakes.
X., The Production of Insoluble Azo Colours in the Form of Pigments. XL, The General
Properties of Lakes Produced from Artificial Colours. XII., Washing, Filtering and Fin-
ishing. XIII., Matching and Testing Lake Pigments. Index.
Press Opinions.
"It
evidently the result of prolonged research, and cannot but prove a valuable con-
is
sulting work
to those engaged in the industry." Derby Mercury.
"The book is well written and full of just such information as will enable a young man to
'
into his work. The various classes of colouring matters are carefully described
'
put brains
and the process by which the lakes are produced fully discussed." Northern Daily Telegraph.
"This work just issued is a very valuable treatise on the manufacture of lake pigments of
the coal-tar series principally. The plan adopted by the author in writing up the subject
enables the manufacture to be very readily understood. The general properties of lakes
. . .
produced from artificial colours, washing, filtering and finishing, and matching and testing
lake pigments are well and exhaustively described, so that no manufacturer or user of lake
pigments can well afford to be without this work." Chemical Trade Journal.
"This is undoubtedly a book which will occupy a very high place amongst technical works,
and will prove of exceptional value to all whom it immediately concerns. have no We
hesitation in recommending it as one of the best works of its class we have ever read. Air.
Jennison has set about his task with a lucid style, and with a complete mastery of his subject.
. . . We
do not think students of the technical side of the paint and colour industry can
possibly spend 7s. 6d. in a more profitable way than by buying this publication." Eastern
THE TESTING AND VALUATION OF RAW MATE-

RIALS USED IN PAINT AND COLOUR MANU
FACTURE. By M. W. JONES, F.C.S. A Book lor the
Laboratories cf Colour Works. 88 pp. 1900. Price 5s. ; India and
Colonies, 5s. 6d. Other Countries, 6s.
; ; strictly net, post free.
Contents.
Aluminium Compounds. China Clay. Iron Compounds. Potassium Compounds. Sodium
Compounds. Ammonium Hydrate. Acids. Chromium Compounds. Tin Compounds. Cop-
per Compounds. Lead Compounds. Zinc Compounds. Manganese Compounds. Arsenic
Compounds. Antimony Compounds. Calcium Compounds. Barium Compounds. Cadmium
Compounds. Mercury Compounds. Ultramarine. Cobalt and Carbon Compounds. Oils
Index.
Press Opinions.
"Though this excellent little work can appeal only to a limited class, the chemists in colour
works, yet it will appeal to them very strongly indeed, for it will put them on the track of
and yet approximately, accurate methods of testing the comparative value of
short, rapid,
competing samples of rasv material used in paint and colour manufacture." North British
Daily Mail.
"This little text-book is intended to supplement the larger and more comprehensive works
on the subject, and it embodies the result of Mr. Jones' experiments and experiences, extend-
ng over a long period. It gives, under separate headings, the principal ingredients and im-
purities found in the raw materials, and is a handy work of reference for ascertaining what is
valuable or detrimental in the sample under examination." Blackburn Times.
"There is no attempt at literary adornment nor straining after literary effect, but the
lessons are imparted in simple and concise language. This is just what a text-book should
be. ... The treatise is certainly most useful, and bears internal evidence of being the results
of actual work in a busy manufactory and not of ephemeral cramming in a technical school.
The chapter arrangement is good, the index satisfactory, and the book is altogether one which
the practical chemist should keep as accessible to his crucibles and filter paper." Manchester
Courier.
8
THE CHEMISTRY OF ESSENTIAL OILS AND ARTI-

FICIAL PERFUMES. By ERNEST J. PARRY, B.Sc.
(Lond.), F.I.C., F.C.S. Illustrated with Twenty Engravings. 400 pp.
1899. Price 12s. 6d. ;
India and Colonies, 13s. 6d. ;
Other Countries,
15s.; strictly net, post free.
Contents.
Chapters I., The General Properties of Essential Oils. II., Compounds occurring
in Essential Oils. III., The Preparation of Essential Oils. IV., The Analysis of
Essential Oils. V., Systematic Study of the Essential Oils. VI., Terpeneless Oils.
VII., The Chemistry of Artificial Perfumes. Appendix Table of Constants. :
Press Opinions.
"There can be no doubt that the publication will take a high place in the list of scientific
text-books." London Argus.
"We can heartily recommend this volume to all interested in the subject of essential oils
from the scientific or the commercial standpoint." British and Colonial Druggist.
" Mr.
Parry has done good service in carefully collecting and marshalling the results of the
numerous researches published in various parts of the world. "Pharmaceutical Journal.
"A most useful appendix is inserted, giving a table of constants for the more important
essential oils.. This, in itself, is of sufficient importance and use to warrant the publication
. .
of the book, and, added to the very complete classification and consideration of the essential oils
which precedes it, the volume becomes of great value to all interested." Glasgow Herald.
" At various times
monographs have been printed by individual workers, but it may safely
be said that Mr. Parry is the first in these latter days to deal with the subject in an adequate
manner. His book is well conceived and well written. ... He is known to have sound practi-
cal experience in analytical methods, and he has apparently taken pains to make himself aufait
with the commercial aspects of the subject." Chemist and Druggist.
" Mr.
Parry's reputation as a scientist is fully established, and we can therefore accept any
work emanating from his pen as being of the greatest practical value. have perused theWe
work before us with much care, and are convinced that the contents will be found most service-
able and its publication most opportune. He avoids unnecessary details, but includes
. . .
everything that is essential to systematic treatment, while he attempts no more than to give
'
an outline of the principles involved'. . . . We

congratulate Mr. Parry on the scientific value
of his work, and hope that if the progress of the colonies in the manufacture of essential oils
and perfumes equals what we are justified in expecting, it will become an Australian hand-book,
everywhere appreciated." The Australian Brewers' Journal.
DRYING OILS, BOILED OIL AND SOLID AND

LIQUID DRIERS. By L. E. ANDES. A Practical Work
for Manufacturers of Oils, Varnishes, Printing Inks, Oilcloth and Lino-
leum, Oilcakes, Paints, etc. Expressly Written for this Series of Special
Technical Books, and the Publishers hold the Copyright for English and
Foreign Editions. Forty-two Illustrations. 360pp. 1901. 8vo. Demy
Price 12s. 6d. ; India and Colonies, 13s. 6d. ; Other Countries, 15s.
Contents.
Chapters I., General Chemical and Physical Properties of the Drying Oils Cause of the ;
Drying Property; Absorption of Oxygen; Behaviour towards Metallic Oxides, etc. II., The
Properties of and Methods for obtaining the Drying Oils. III., Production of the Drying Oils
by Expression and Extraction; Refining and Bleaching; Oil Cakes and Meal; The Refining
and Bleaching of the Drying Oils The Bleaching of Linseed Oil. IV., The Manufacture of
;
Boiled Oil; The Preparation of Drying Oils for Use in the Grinding of Paints and Artists'
Colours and in the Manufacture of Varnishes by Heating over a Fire or by Steam, by the Cold
Process, by the Action of Air, and by Means of the Electric Current; The Driers used in
Boiling Linseed Oil; The Manufacture of Boiled Oil and the Apparatus therefor Livache's :
Process for Preparing a Good Drying Oil and its Practical Application. V., The Preparation
of Varnishes for Letterpress, Lithographic and Copperplate Printing, for Oilcloth and Water-
proof Fabrics The Manufacture of Thickened Linseed Oil, Burnt Oil, Stand Oil by Fire Heat,
;
Superheated Steam, and by a Current of Air. VI., Behaviour of the Drying Oils and Boiled
Oils towards Atmospheric Influences, Water, Acids and Alkalies. VII., Boiled Oil Substitutes.
VIII., The Manufacture of Solid and Liquid Driers from Linseed Oil and Rosin: Linolic
Acid Compounds of the Driers. IX., The Adulteration and Examination of the Drying Oils
and Boiled Oil.
GLUE AND GLUE TESTING. By SAMUEL RIDEAL, D.Sc.

Lond., F.I.C. Fourteen Engravings. 144 pp. 1900. Price 10s. 6d. ;
India and Colonies, lls. Other Countries, 12s.; strictly net, post free.
;
Contents.
Chapters I., Constitution and Properties: Definitions and Sources, Gelatine, Chondrin
and Allied Bodies, Physical and Chemical Properties, Classification, Grades and Commercial
Varieties. II., Raw Materials and Manufacture : Glue Stock, Lining, Extraction, Washing
and Clarifying, Filter Presses, Water Supply, Use of Alkalies, Action of Bacteria and of
Antiseptics, Various Processes, Cleansing, Forming, Drying, Crushing, etc., Secondary Pro-
ducts. III., Uses of Glue : Selection and Preparation for Use, Carpentry,
Veneering,
Paper-Making, Bookbinding, Printing Rollers, Hectographs, Match Manufacture, Sandpaper,
etc., Substitutes for other Materials, Artificial Leather and Caoutchouc. IV., Gelatine :
General Characters, Liquid Gelatine, Photographic Uses, Size, Tanno-, Chrome and Formo-
Gelatine, Artificial Silk, Cements, Pneumatic Tyres, Culinary, Meat Extracts, Isinglass, Medi-
cinal and other Uses, Bacteriology. V., Glue Testing-: Review of Processes, Chemical
Examination, Adulteration, Physical Tests, Valuation of RawJVIaterials. VI., Commercial
Aspects.
Press Opinions.
"This work is of the highest technical character, and gives not only a full and practical ac-
count of the raw materials and manufacture of glues, gelatines and similar substances, but
gives many hints and information on the use of such substances in veneering, carpentry and
many other purposes. Many tests are given for glue in different stages of the progress of its
manufacture, and the commercial value of a commodity so much in general use is exemplified
by statistics and figures, it is certainly a valuable treatise upon an article for which very
little literature in any form has previously been obtainable."
" Books on the art of Carpenter and Builder.
glue making are more than usually scarce, and users of that article,
as well as thjse who may be tempted to embark in the industry, should therefore welcome
this book by Dr. Samuel Rideal, a Fellow of the Institute of Chemistry, and a
leading authority.
In this book he has collected the more important facts connected with the manufacture of glue
and allied products, and stated the experience he has gained in examining various commercial
samples during the past ten years. . Dr. Rideal's book must be regarded as a valuable con-
. .
tribution to other technical literature, which manufacturers, merchants and users may study
with profit." British Trade Journal.
"This volume is the latest addition to the excellent series of special technical works for
manufacturers and professional and commercial men issued by the well-known publishers of
The Oil and Colourman's Journal. The volume in every way fully maintains the high standard
of excellence of the whole series, and deals with the subject of glue making and glue testing in
a thoroughly exhaustive manner. Chapters are given on the constitution and properties, and
raw material and manufacture, and of the uses of glue, and in this latter respect it will doubtless
be information to many readers to learn to what extent glue enters into the manufacture of
many commercial products not apparently associated with glue. Exhaustive chapters on the
processes and methods of glue testing, and on its commercial aspects, complete this useful and
most carefully prepared volume." Carriage Builders' Journal.
TECHNOLOGY OF PETROLEUM : Oil Fields of the

World Their History, Geography and Geology Annual Production
and Development Oil-well Drilling Transport. By HENRY NEU-
BERGER and HENRY NOALHAT. Translated from the French by J. G.
MclNTOSH. 540 pp. Illustrations, Maps and Plates. [In the Press.
Contents.
Part I., Study of :the Petroliferous Strata Chapters I., Petroleum Definition. II.,
The Genesis or Origin of Petroleum. III., The Oil Fields of Galicia, their History. IV.,
Physical Geography and Geology of the Galician Oil Fields. V., Practical Notes on Galician
Land Law Economic Hints on Working, etc. VI., Roumania History, Geography, Geology.
VII., Petroleum in Russia History. VIII., Russian Petroleum (continued) Geography and
Geology ot the Caucasian Oil Fields. IX., Russian Petroleum (continued). X., The Secondary
Oil Fields of Europe, Northern Germany, Alsace, Italy, etc.-XL, Petroleum in France. XII.,
Petroleum in Asia Transcaspian and Turkestan Territory Turkestan Persia British
India and Burmah British Burmah or Lower Burmah China Chinese Thibet Japan,
Formosa and Saghalien. XIII., Petroleum in Oceania Sumatra, Java, Borneo Isle of
Timor Philippine Isles New Zealand. XIV., The United States of America History.
XV., Physical Geology and Geography of the United States Oil Fields. XVI., Canadian and
other North American Oil Fields. XVII., Economic Data of Work in North America.
XVIIL. Petroleum in the West Indies and South America.-XIX., Petroleum in the French
Colonies.
Part II., Excavations. Chapter XX., Hand Excavation or Hand Digging of Oil Wells.
Part HI., Methods of Boring.-Chapters XXI., Methods of Oil-well Drilling or Boring.
XXII., Boring Oil Wells with the Rope.-XXIII., Drilling with Rigid Rods and a Free-fall-
Fabian System. XXIV., Free-fall Drilling by Steam Power. XXV., Oil-well Drilling by the
Canadian System. XXVI., Drilling Oil Wells on the Combined System. XXVII., Com-
parison between the Combined Fauck System and the Canadian. XXVIII., The American
System of Drilling with the Rope. XXIX., Hydraulic Boring with the Drill by Hand and
Steam Power. XXX., Rotary Drilling of Oil Weils, Bits, Steel-crowned Tools, Diamond
Tools Hand Power and Steam Power Hydraulic Sand-pumping. XXXI., Improvements
in and different Systems of Drilling Oil Wells.
10
Part IV., Accidents. Chapters XXXII., Boring Accidents Methods of preventing them
.Methods of remedying them. XXXIII., Explosives and the use of the "Torpedo" Leviga-
tion. XXXIV., Storing and Transport of Petroleum. XXXV., General Advice Prospecting,
Management and carrying on of Petroleum Boring Operations.
Part V., General Data. Customary Formulas. Memento. Practical Part. General
Data bearing on Petroleum. Glossary of Technical Terms used in the Petroleum Industry.
Index.
A DICTIONARY OF CHEMICALS AND RAW PRO-

DUCTS USED IN THE MANUFACTURE OF
PAINTS, COLOURS, VARNISHES AND ALLIED
PREPARATIONS. By GEORGE H. HURST, F.C.S. Demy
8vo. 380 pp. 1901. Price 7s. 6d. India and Colonies, 8s.; Other
;
Countries, 8s. 6d. strictly net, post free.

;
Contents.
The names of the Chemicals and Raw Products are arranged in alphabetical order, and
the description of each varies in length from half to eight pages. The following are some of
the articles described and explained Acetates Acetic Acid Acidimetry Alcohol Alum
:
Ammonia Amber Animi Arsenic Beeswax Benzol Bichromates of Potash and Soda
Bleaching Powder Bone Black Boric Acid Brunswick Green Cadmium Yellow Car-
bonates Carmine Carnauba Wax Caustic Potash and Soda Chrome Colours Clay Coal
Tar Colours Copal Dammar Drying Oils Emerald Green Gamboge Glue Glycerine
Gums Gypsum Indian Red Japanese Lacquer Lac Lakes Lamp Black Lead Com-
pounds Linseed Oil Magnesia Manganese Compounds Mica Nitric Acid Ochres
Orange Lead Orr's White Paraffin Prussian Blue Rosin Oil Sepia Sienna Smalts-
Sodium Carbonate Sublimed White Lead Sulphuric Acid Terra Verte Testing Pigments
Turpentine Ultramarine Umbers Vermilionettes White Lead Whiting Zinc Com-
pounds. Appendix: Comparison of Baume Hydrometer and Specific Gravity for Liquids
Lighter than Water Hydrometer Table for Liquids Heavier than Water Comparison of
Temperature Degrees Tables for Converting French Metric Weights and Measures into
English Table of the Elements etc., etc. Copious Index.
PURE AIR, OZONE AND WATER. A Practical Treatise

of their Utilisation and Value in Oil, Grease, Soap, Paint, Glue and
other Industries. By W. B. COVVELL. Twelve Illustrations. 1900.
Price 5s. India and Colonies, 5s. 6d.
; Other Countries, 6s. strictly
; ;
net, post free.

Contents.
Chapters I., Atmospheric Air; Lifting of Liquids: Suction Process; Preparing Blown Oils ;
Preparing Siccative Drying Oils. II., Compressed Air; Whitewash. III., Liquid Air; Retro-
cession. IV., Purification of Water; VVater Hardness. V., Fleshings and Bones. VI., Ozon-
ised Air in the Bleaching and Deodorising of Fats, Glues, etc. ;>Bleaching Textile Fibres.
Appendix: Air and Gases; Pressure of Air at Various Temperatures Fuel; Table of Com- :
bustibles; Saving of Fuel by Heating Feed Water; Table of Solubilities of Scale Making
Minerals; British Thermal Units Tables; Volume of the Flow of Steam into the Atmosphere;
Temperature of Steam. Index.
Press Opinions.
"This is a valuable work in little space. ... In arrangement it is a commendable work,
and its value is increased by the index which brings the little volume to a close." \fwcastle
Daily Journal.
"The book is written solely for manufacturers, who, without doubt, will find it exceedingly
practical and useful. The volume contains an appendix wherein is given a great many tables,
etc., which manufacturers in the trades referred to will find of inestimable value." Blackburn
Times.
THE MANUFACTURE OF MINERAL AND LAKE

PIGMENTS. Containing Directions for the Manufacture
and Painters' Colours, Enamel, Soot and Me-
of all Artificial, Artists
tallic Pigments. A
Text-book for Manufacturers, Merchants, Artists
and Painters. By Dr. JOSEF BERSCH.
Translated from the Second
Revised Edition by ARTHUR C. WRIGHT, M.A. (Oxon.), B.Sc. (Lond.),
formerly Assistant Lecturer and Demonstrator in Chemistry at the
Yorkshire College, Leeds. Forty-three Illustrations. 476 pp., demy
8vo. 1901. Price 12s. 6d. India and ; Colonies, 13s. 6d. ;
Other
Countries, 15s. strictly net, post free.
;
11
Contents.
Chapters I., Introduction. II.. Physico-chemical Behaviour of Pigments. III., Raw
Materials Employed in the Manufacture of Pigments. IV., Assistant Materials. V., Metallic
Compounds. VI., The Manufacture ot Mineral Pigments. VII., The Manufacture of White
Lead. VIII., Enamel White. IX., Washing Apparatus. X., Zinc White. XI., Yellow
Mineral Pigments. XII., Chrome Yellow. XIII., Lead Oxide Pigments. XIV., Other
Yellow Pigments. XV., Mosai? Gold. XVI., Red Mineral Pigments. XVII., The Manu-
facture of Vermilion. XVIII., Antimony Vermilion. XIX., Ferric Oxide Pigments XX
Other Red Mineral Pigments.-XXI Purple of Cassius. XXII., Blue Mineral Pigments.
,
XXIII., Ultramarine. XXIV., Manufacture of Ultramarine. XXV., Blue Copper Pigments

XXVI., Blue Cobalt Pigments. XXVII., Smalts. XXVIII., Green Mineral Pigments
XXIX., Emerald Green.-XXX., Verdigris.-XXXI., Chromium Oxide.-XXXII., Other
Green Chromium Pigments. XXXIII., Green Cobalt Pigments. XXXIV., Green Man-
ganese Pigments.^-XXXV., Compounded Green Pigments. XXXVI., Violet Mineral Pig-
ments.-XXXVII., Brown Mineral Pigments. XXXVIII., Brown Decomposition Products.
XXXIX., Black Pigments. XL., Manufacture of Soot Pigments. XLI., Manufacture of
Lamp Black. XLII., The Manufacture of Soot Black without Chambers. XLIII. Indian
Ink. XLI V., Enamel Colours. XLV., Metallic Pigments. XLVI., Bronze Pigments
XLVII., Vegetable Bronze Pigments.
PIGMENTS OF ORGANIC ORIGIN. Chapters XLVIII., Lakes. XLIX., Yellow Lakes. L.,
Red Lakes. LI., Manufacture of Carmine. LII., The Colouring Matter of Lac. LIII., Saf-
flower or Carthamine Red. LIV., Madder and its Colouring Matters. LV., Madder Lakes.
LVI., Manjit (Indian Madder). LVI I.. Lichen Colouring Matters. LVIII., Red Wood Lakes
-LIX., The Colouring Matters of Sandal Wood and Other Dye Woods. LX., Blue Lakes.
LXI., Indigo Carmine. LXI I., The Colouring Matter of Log Wood. LXIII., Green Lakes.
LXIV., Brown Organic Pigments. LXV., Sap Colours. LXVI., Water Colours. LXVI I.
Crayons. LX VI 1 1., Confectionery Colours.-LXIX., The Preparation of Pigments for
Painting. LXX., The Examination of Pigments. LXXI., Examination of Lakes. LXXIL,
The Testing of Dye- Woods. LXX II I., The Design of a Colour Works. LXXI V. Commercial
Names of Pigments. Appendix: Conversion of Metric to English Weights and Measures.
Centigrade and Fahrenheit Thermometer Scales. Index.
BONE PRODUCTS AND MANURES An Account of the

:
most recent Improvements in the Manufacture of Fat, Glue, Animal

Charcoal, Size. Gelatine and Manures. By THOMAS LAMBERT, Techni-
cal and Consulting Chemist. Illustrated by Twenty Plans and Diagrams.
Demy 8vo. 1901. Price 7s. 6d. India and Colonies, 8s.; Other
;
Countries, 8s. 6d.

Contents.
Chapters I., Chemical Composition of Bones Arrangement of Factory Crushing of Bones
Treatment with Benzene Benzene in Crude Fat Analyses of Clarified Fats Mechanical
Cleansing of Bones Animal Charcoal Tar and Ammoniacal Liquor, Char and Gases, "
from
"
good quality Bones Method of Retorting the Bones Analyses of Chars Spent Chars
Cooling of Tar and Ammoniacal Vapours Value of Nitrogen for Cyanide of Potash Bone
Oil Marrow Bones Composition of Marrow Fat Premier Juice Buttons. II., Properties
of Glue Glutin and Chondrin Skin Glue Liming of Skins Washing Boiling of Skins-
Clarification of Glue Liquors Acid Steeping of Bones Water System of Boiling Bones-
Steam Method of Treating Bones Nitrogen in the Treated Bones Glue-Boiling and Clarify-
ing-House Plan showing Arrangement of Clarifying Vats Plan showing Position of Evapora-
tors Description of Evaporators Sulphurous Acid Generator Clarification of Liquors
Section of Drying-House Specification of a Glue Size Uses and Preparation and Composi-
tion of Size Concentrated Size. III., Properties of Gelatine Preparation of Skin Gelatine
Washing Bleaching Boiling Clarification Evaporation Drying Bone Gelatine Se-
lecting Bones Crushing Dissolving Bleaching Boiling Properties of Glutin and Chondrin
Testing of Glues and Gelatines. IV., The Uses of Glue, Gelatine and Size in Various
Trades Soluble and Liquid Glues Steam and Waterproof Glues. V., Manures Importation
of Foodstuffs Soils Germination Plant Life. VI., Natural Manures Water and Nitrogen
in Farmyard Manure Full Analysis of Farmyard Manure Action on Crops Water-Closet
System Sewage Manure Green Manures. VII., Artificial Manures Bones Boiled and
Steamed Bones Mineral Phosphates English Coprolites French and Spanish Phosphorites
German and Belgian Phosphates Basic Slag Guanos Proper Guano Phosphates. VIII.,
Mineral ManuresCommon Salt Potash Salts Calcareous Manures Prepared Nitrogenous
Manures Ammoniacal Compounds Sodium Nitrate Potassium Nitrate Organic Nitro-
genous Matters Shoddy Hoofs and Horns Leather Waste Dried Meat Dried Blood-
Superphosphates Composition Manufacture Section of Manure-ShedFirst and Ground
Floor Plans of Manure-ShedQuality of Acid Used Mixings Special Manures Potato
Manure Dissolved Bones Dissolved Bone Compound Enriched Peruvian Guano Special
Manure for Garden Stuffs, etc. Special Manure for Grass Lands Special Tobacco Manures
Sugar-Cane Manure Compounding of Manures Valuation of Manures. IX., Analyses of
Raw and Finished Products Common Raw Bones Degreased Bones Crude Fat Refined
Fat Degelatinised Bones Animal Charcoal Bone Superphosphates Guanos Dried Animal
Products Potash Compounds Sulphate of Ammonia. Index.
12
MANUFACTURE OF PAINT. By J. CRUICKSHANK SMITH,

B.Sc. With numerous Illustrations. [In the Press.
Contents.
Part I. Chapters I., Preparation of Raw .Material. II.. Storing of Raw Material. III.,
Testing and Valuation of Raw Material Paint Plant and Machinery.
Part II. Chapters V., The Grinding of White Lead. VI., Grinding of White Zinc. VII.,
Grinding of other White Pigments. VIII., Grinding of Oxide Paints. IX., Grinding of Stain-
ing Colours. X., Grinding of Black Paints. XI., Grinding of Chemical Colours Yellows.
XII., Grinding of Chemical Colours-Blues.-Xl 1 1., Grinding Greens. XIV., Grinding Reds.
XV., Grinding Lakes.-XVI., Grinding Colours in Water. XVII., Grinding Colours in
Turpentine.
Part III. Chapters XVIII., The Uses of Paint. XIX., Testing and'Matching Paints.
XX., Economic Considerations. Index.
THE RISKS AND DANGERS OF VARIOUS OCCUPA-

TIONS AND THEIR PREVENTION. By LEONARD
A. PARRY, M.D., B.S. (Lond.). 196 pp., demy 8vo. 1900. Price 7s. 6d. ;
India and Colonies, 8s. Other Countries, 8s. 6d. strictly net, post free.
; ;
Contents.
Chapters I., Occupations which are Accompanied by the Generation and Scattering of
Abnormal Quantities of Dust. II., Trades in which there is Danger of Metallic Poisoning.
Certain Chemical Trades. IV., Some .Miscellaneous Occupations. V., Trades in which
III.,
Various Poisonous Vapours are Inhaled. VI., General Hygienic Considerations. Index.
This book contains valuable information for the following trades Aerated Water Manu-
facture, Alkali Manufacture, Aniline Manufacture, Barometer Making, Brass Founders, Bromine
Manufacture, Bronze Moulders, Brush Making, Builders, Cabinet Makers, Calico Printing,
Chloride of Lime Manufacture, Coal Miners, Cocoa-nut Fibre Making, Colour Grinders,
Copper Miners, Cotton Goods Manufacture, Cotton Yarn Dyeing, Cutlery Trades, Dry Clean-
ing, Electricity Generating, Electroplaters, Explosives Manufacture, File Making, Flint
Milling, FloorCIoth Makers, Furriers, Fustian Clothing Making, Galvanised Iron .Manufacture,
Gassing Process, Gilders, Glass Making, Glass Paper Making, Glass Polishing and Cutting,
Grinding Processes, Gunpowder Manufacturing, Gutta-percha Manufacture, Hat Makers,
Hemp Manufacture, Horn Goods Making, Horse-hair .Making, Hydrochloric Acid Manufacture,
India-rubber Manufacture, Iodine Manufacture, Ivory Goods Making, Jewellers, Jute Manu-
facture, Knife Grinders, Knife Handle Makers, Lace Makers, Lacquering. Lead Melters, Lead
Miners, Leather Making, Linen Manufacture Linoleum .Making, Lithographic Printing and
Bronzing, Lithographing, Masons, Match Manufacture, Melanite Making, Mirror Making,
Needle Grinders, Needle Making, Nitro-benzole Making, Nitro-glycerine Making, Paint
Makers, Paper Making, Philosophical Instrument Makers, Photographers, Picric Acid Making,
Portland Cement Making, Pottery Manufacture, Printers, Quicksilver Mining, Rag Pickers,
Razor Grinders, Red Lead Making, Rope Making, Sand Paper Making, Saw Grinders, Scissors
Grinders, Shoddy Manufacture, Shot Making, Silk .Making, Silver .Mining, Skinners, Slag, Wood
Manufacture, Steel Makers, Steel Pen Making, Stereotypers, Stone Masons, Straw Hat Makers,
Sulphuric Acid Manufacture, Sweeps, Table-knife Grinders, Tanners, Telegraphists, Textile
Industries, Tin Miners, Turners, Type Founders, Umbrella .Makers, Wall Paper Making,
White Lead Making, Wood Working, Woollen Manufacture, Wool Sorters, Zir.c Qvide
Manufacture, Zinc Working, etc., etc.
Press Opinions.
"The language used is quite simple, and can be understood by any intelligent person en-
gaged in the trades dealt with." The Clarion.
"This is an appalling book. It shows that there is scarcely a trade or occupation that has
not a risk or a danger attached to it." Local Government Journal.
" Dr. '
Parry has not only pointed out the risks and dangers of various occupations he has
'
;
suggested means for their prevention. The work is primarily a practical one." Colliery
Manager.
"This a most useful book which should be in the hands of all employers of labour,
is
foremen, and intelligent workmen, and is one of great utility to sanitary inspectors, and even
on occasion to medical men." Health.
"The writer has succeeded in collecting a large amount of information, and though one
could wish he had presented it in a rather more attractive style, he has certainly condensed it
into a very small space." Physician and Surgeon.
"The little book before us is one which will be found exceedingly useful to manufacturers
and even factory inspectors. . . No attempt is made to show how diseases when originated
.
are to be cured, but, acting on the sound principle that prevention is better than cure, means
are stated how to avoid the harm." Bristol Mercury.
"The author has endeavoured to treat the question in simple rather than in technical lan-
guage, and he has lucidly catalogued the most dangerous trades and their symptoms, and in
each case specified the best methods of dealing with them. ... To those for whom the volume
is specially designed, Dr. Parry's treatise should be a useful handbook." Sheffield Independent.
13
"Avery useful manual for employers of labour, foremen, intelligent workmen, and, in spite
of the author's modesty, for medical men. We have the peculiar risks and dangers of all the
dangerous trades carefully described the mode of action of various chemicals, etc., used in
;
different industries given, with full directions how to minimise unavoidable risks." Leeds
Mercury.
"Most of the trades in the country are alluded to, and upon those that are dangerous the
necessary attention is bestowed, and means are recommended whereby danger may be pre-
vented or lessened. The author has evidently studied his subject with care, and has made full
use of the experience of others who have had a larger insight into the industries of the country."
^British Medical Journal.
"The work is well written and printed, and its verbiage such as to be comprehensible to the
workman no less than to the master. The careful and general perusal of a work of this nature
cannot but be attended by beneficial results of a far-reaching nature, and we therefore heartily
recommend the book to our readers. Medical Officers of Health and Sanitary Inspectors
especially should find the work of great interest." Sanitary Record.
" It is written in
simple language, and its instructions can be easily followed. . . There
.
are some employers, at any rate, who are more ignorant of, than indifferent to, the slow murder
of their workpeople, and if the facts so succinctly set forth in this book were brought to their
notice, and if the Trade Unions made it their business to insist on the observance of the better
conditions Dr. Parry described, much might be done to lessen the workman's peril." Weekly
Times and Echo.
PRACTICAL X RAY WORK. By FRANK T. ADDYMAN,

B.Sc. (Lond.), F.I.C.,Member of the Roentgen Society of London ;
'
Radiographer to St. George's Hospital Demonstrator of Physics an

;
Chemistry, and Teacher of Radiography in St. George's Hospital

Medical School. Demy 8vo. Illustrated. [In the Press.
Contents.
Part I., Historical Chapters I., Introduction. II., Work leading up to the Discovery of
the X Rays. III., The Discovery.
Part II., Apparatus and its Management Chapters I., Electrical Terms. II., Source?
of Electricity. III., Induction Coils. IV., Electrostatic Machines. V., Tubes. VI., Air
Pumps. VII., Tube Holders and Stereoscopic Apparatus. VIII., Fluorescent Screens.
Part III., Practical X Ray Work Chapters I., Installations.-II., Radioscopy. III.,
Radiography. IV., X Rays in Dentistry. V., X Rays in Chemistry. VI., X Rays in War.
Index.
DRYING BY MEANS OF AIR AND STEAM. Explana-

tions, Formulae, and Tables for Use in Practice. Translated from the
German of E. HAUSBRAND. Two Diagrams and Thirteen Tables.
Contents. [In the Press.
Preface. Chapters I., Introduction. Estimation of the .Maximum Weight of Saturated
II.,
Aqueous Vapour which can be contained 1 kilo, of Air at Different Pressure and Tem-
in
peratures. III., Calculation of the Necessary Weight and Volume of Air, and of the Least
Expenditure of Heat, per Drying Apparatus with Heated Air, at the Atmospheric Pressure:
A, With the Assumption that the Air is Completely Saturated with Vapour both before Entry
and after Exit from the Apparatus. B, When the Atmospheric Air is Completely Saturated
before entry, but at its exit is only |, A or J Saturated. C, When the Atmospheric Air is not
Saturated with Moisture before Entering the Drying Apparatus. IV., Drying Apparatus, in
which, in the Drying Chamber, a Pressure is Artificially Created, Higher or Lower than that
of the Atmosphere. V., Drying by Means of Superheated Steam, without Air. VI., Heating
Surface, Velocity of the Air Current, Dimensions of the Drying Room, Surface of the Drying
Material, Losses of Heat.
Leather Trades.
THE LEATHER WORKER'S MANUAL. Being a Com-
pendium of Practical Recipes and Working Formulae for Curriers,
Bootmakers, Leather Dressers, Blacking Manufacturers, Saddlers,
Fancy Leather Workers, and all Persons engaged in the Manipulation
of Leather. By H. C. STANDAGE. 165 pp. 1900. Price 7s. 6d. ;
India and Colonies, 8s. Other Countries, 8s. 6d. strictly net, post free.
; ;
Contents.
Chapters I., Blackings, Polishes, Glosses, Dressings, Renovators, etc., for Boot and Shoe
Leather. II., Harness Blackings, Dressings, Greases, Compositions, Soaps,
and Boot-top
Powders and Liquids, etc., etc. III., Leather Grinders' Sundries. IV., Currier's Seasonings,
Blacking Compounds, Dressings, Finishes, Glosses, etc. V., Dyes and Stains for Leather.
VI., Miscellaneous Information. VII., Chrome Tannage. Index.
14
Press Opinions.
"The book being absolutely unique, is likely to be of exceptional value to all whom it con-
cerns, as it long-felt want." Birmingham Gazette.
meets a
" This a valuable collection of practical receipts and working formulae for the use of those
is
engaged in the manipulation of leather. We

have no hesitation in recommending it as one of
the best books of its kind, an opinion which will be endorsed by those to whom it appeals."
Liverpool Mercury.
"We think we may venture to state, so far as the opinion of the leather trade under the
Southern Cross is concerned, that it will be one of approval. As practical men, having a long
and wide experience of the leather trade in Australia, we are certain that there are many
tanners and curriers carrying on business in remote townships of the colonies to whom such a
manual of practical recipes will be invaluable. This manual is not a mere collection of re-
. . .
cipes for the various purposes to which they may be applied, but it is also replete with instruc-
tions concerning the nature of the materials recommended to be used in making up the recipes.
.. . We
think every intelligent leather man should avail himself of the manual. It is un-
doubtedly a valuable contribution to the technology of the leather trade." Australian Leather
Journal and Boot and Shoe Recorder.
PRACTICAL TREATISE ON THE LEATHER IN-

DUSTRY. By A. M. VILLON.
Translation of Villon'sA
" Traite
Pratique de la Fabrication des cuirs et du Travail des Peaux ".
By FRANK T. ADDYMAN, B.Sc. (Lond.), F.I.C., F.C.S. and Corrected ;
by an Eminent Member of the Trade. 500pp., royal 8vo. 1901. 123

Illustrations. Price 21s. India and Colonies, 22s. Other Countries,
; ;
23s. 6d. ; strictly net, post free.

Contents.
Preface Translator's Preface List of Illustrations.
Part I., Materials used in Tanning: Chapter '-. Skins: I., Skin and its Structure; II.,
Skins used in Tanning; III., Various Skins and their Uses Chapter II., Tannin and Tanning
Substances: I., Tannin; II., Barks (Oak); III., Barks other than Oak; IV., Tanning
Woods; V., Tannin-bearing Leaves; VI., Excrescences; VII., Tan-bearing Fruits; VIII.,
Tan-bearing Roots and Bulbs IX., Tanning Juices X., Tanning Substances used in Various
; ;
Countries; XI., Tannin Extracts; XII., Estimation of Tannin and Tannin Principles.
Part II., Tanning Chapter I., The Installation of a Tannary: I., Tan Furnaces; II..
Chimneys, Boilers, etc.; III., Steam Engines Chapter II., Grinding and Trituration of
Tanning Substances: I., Cutting up Bark; II., Grinding Bark; III., The Grinding of Tan
Woods; IV., Powdering Fruit, Galls and Grains; V., Notes on the Grinding of Bark Chap-
ter III., Manufacture of Sole Leather: I., Soaking; II., Sweating and Unhairing; III.,
Plumping and Colouring; IV., Handling; V., Tanning; VI., Tanning Elephants' Hides;
VII., Drying; VIII., Striking or Pinning Chapter IV., Manufacture of Dressing Leather:
I., Soaking; II., Depilation "ill., New Processes for the Depilation of Skins; IV., Tanning;
;
V., Cow Hides; VI., Horse Hides; VII., Goat Skins; Manufacture of Split Hides Chap-
ter V., On Various Methods of Tanning: I., Mechanical Methods; II., Physical Methods;
III.. Chemical Methods; IV., Tanning with Extracts Chapter VI., Quantity and Quality:
I., Quantity; II., Net Cost; III., Quality of Leather Chapter VII., Various Manipulations
of Tanned Leather: I., Second Tanning; II., Grease Stains; III., Bleaching Leather; IV.,
Waterproofing Leather; V., Weighting Tanned Leather; VI., Preservation of Leather-
Chapter VIII., Tanning Various Skins.
Part III., Currying Chapter I., Waxed Calf: I., Preparation; II., Shaving; III.,
Stretching or Slicking; IV., Oiling the Grain V., Oiling the Flesh Side VI., Whitening and
; ;
Graining; VII., Waxing; VIII., Finishing; IX., Dry Finishing; X., Finishing in Colour;
XL, Cost Chapter II., White Calf: I., Finishing in White Chapter III., Cow Hide for
Upper Leathers: I., Black Cow Hide; II., White Cow Hide; III., Coloured Cow Hide.
Chapter IV., Smooth Cow Hide Chapter V., Black Leather Chapter VI., Miscellaneous
Hides: I., Horse; II., Goat; III., Waxed Goat Skin; IV., Matt Goat Skin Chapter VII.,
Russia Leather: I., Russia Leather; II. Artificial Russia Leather.
Part IV., Enamelled, Hungary and Chanioy Leather, Morocco, Parchment, Furs
and Artificial Leather Chapter I., Enamelled Leather: I., Varnish Manufacture; II,
Application of the Enamel; III., Enamelling in Colour Chapter II., Hungary Leather: I.,
Preliminary; II., Wet Work or Preparation; III., Aluming; IV., Dressing or Loft Work;
V., Tallowing; VI., Hungary Leather from Various Hides Chapter III., Tawing: I., Pre-
paratory Operations; II., Dressing; HI., Dyeing Tawed Skins; IV., Rugs Chapter IV.,
Chamoy Leather Chapter V., Morocco: I., Preliminary Operations; II., Morocco Tanning;
III., Mordants used in Morocco Manufacture; IV., Natural Colours used in Morocco
Dyeing; V., Artificial Colours; VI. Different Methods of Dyeing; VII., Dyeing with Natural
Colours; VIII., Dyeing with Aniline Colours; IX., Dyeing with Metallic Salts; X., Leather
Printing; XL, Finishing Morocco; XII., Shagreen; XIII., Bronzed Leather Chapter VI.,
Gilding and Silvering: I., Gilding; II., Silvering; III., Nickel and Cobalt Chapter VII.,
Parchment Chapter VIII.. Furs and Furriery: I., Preliminary Remarks; II., Indigenous
Furs; III., Foreign Furs from Hot Countries; IV. Foreign Furs from Cold Countries; V.,
Furs from Birds' Skins; VI., Preparation of Furs; VII., Dressing; VIII., Colouring; IX.,
Preparation of Birds' Skins; X., Preservation of Furs Chapter IX., Artificial Leather: I.,
, 15
Leather made from Scraps; II., Compressed Leather; III., American Cloth; IV., Papier
Mache; V., Linoleum; VI., Artificial Leather.
Part V., Leather Testing and the Theory of Tanning Chapter I., Testing and Analysis
of Leather: I., Physical Testing of Tanned Leather; II., Chemical Analysis Chapter II.,
The Theory of Tanning and the other Operations of the Leather and Skin Industry: I.,
Theory of Soaking; II., Theory of Unhairing; III., Theory of Swelling; IV., Theory of
Handling; V. Theory of Tanning; VI., Theory of the Action of Tannin on the Skin; VII.,
Theory of Hungary Leather Making; VIII., Theory of Tawing; IX., Theory of Chamoy
Leather Making; X., Theory of Mineral Tanning.
Part VI., Uses Of Leather Chapter I., Machine Belts: I., Manufacture of Belting; II.,
Leather Chain Belts; III., Various Belts, IV., Use of Belts Chapter II., Boot and Shoe-
making: I., Boots and Shoes; II., Laces Chapter III., Saddlery: I., Composition of a
Saddle; II., Construction of a Saddle Chapter IV., Harness: 1., The Pack Saddle; II.,
Harness Chapter V., Military Equipment Chapter VI., Glove Making Chapter VII.,
Carriage Building Chapter VI1L, Mechanical Uses.
Appeendix, The World's Commerce in Leather I., Europe; II., America; III., Asia;
., rica; Australasia
Afri Index.
Press Opinions.
"The book well and lucidly written. The writer is evidently.a practical man, who also
is
has taken the trouble to make himself acquainted with the scientific and technical side of his
trade. . French methods differ largely from our own sometimes we think our ways the
. . ;
best, but not always. The practical man may pick up many useful hints which may help him
to improve his methods." Shoe Manufacturers' Monthly Journal.
"This book cannot fail to be of great value to all engaged in the leather trades. The
. . .
British may believe that the French can teach them nothing in the work of leather tanning
generally, but a comparison of the methods of the two countries will certainly yield a few
wrinkles which may lead to advantageous results. Only a man understanding the science and
technique of the trade could have written the book, and it is well done." Midland Free Press.
"Gives much useful and interesting information concerning the various processes by which
the skins of animals are converted into leather. Written by a French Chemist after five
years of constant study and application it shows all that detail of analysis which we are
;
accustomed to find in scientists, and which the practical tanner is too much in the habit of
ignoring, sometimes to his own loss." Leeds Mercury.
"Nor can there be much doubt that this expectation will be fully justified by the result.
Thanks to the conspicuous painstaking with which Mr. Addyman has discharged his duty, and
the 123 illustrations by which the text is elucidated, the volume can hardly fail to prove a very
valuable standard work of its class. It can thus be confidently recommended to all who are
more or less practically interested in the technology of a very important subject." Leicester
Post.
" M. Villon writes as one having a very full knowledge of all branches of the subject, and in
days when foreign competition has enforced on English manufacturers the importance of no
longer being content with rule-of-thumb methods which have come down to them from their
forefathers it certainly should be worth the while of English tanners to see what lessons they
can learn from French practice, and French practice, we should imagine, could hardly have a
better exponent than the author of this large volume." Western Daily Press and Bristol Times.
"At a time when all or nearly all our British industries are to a greater or less extent
hampered by the pressure of continental and American competition, any hints that can be
obtained as to the methods pursued by competitors must necessarily be of value. . .That it
.
will be of interest and value, not merely to English tanners, but to those associated with many
kindred industrial branches, goes without saying. ... As a work of reference the volume will
be extremely useful in the trade, and where leisure affords sufficient opportunity a careful
perusal and study of it would afford ample reward." Ktttermg Guardian.
"This is a very handsomely got up and elaborate work just issued by this well-known
technical book-publishing firm. .When we say that the work consists of over 500 large
. .
pages with about 120 illustrations, and almost innumerable tables, it will be seen at once that
we cannot attempt anything like an exhaustive resume of its contents, and even if we did the
details would be of little interest to our general readers, while those who are engaged in the
leather industry will probably obtain the book for themselves at least they would do well to
do so. ... Altogether the Treatise has evidently been very carefully prepared, and by a man
' '
who thoroughly knows the subject, and hence it will be a very valuable technical book for
English firms and workers.' Walsall Observer.
Books on Pottery, Glass, etc.

THE MANUAL OF PRACTICAL POTTING. Second
Edition, Revised and Enlarged. 200pp. 1897. Price 17s. 6d.; India
and Colonies, 18s. 6d. Other Countries, 20s. strictly net, post free.
; ;
Contents.
Introduction. The Rise and Progress of the Potter's Art. Chapters I., Bodies. China
and Porcelain Bodies, Parian Bodies, Semi-porcelain and Vitreous Bodies, Mortar Bodies,
Earthenwares Granite and C.C. Bodies, Miscellaneous Bodies, Sagger and Crucible Clays,
16
Coloured Bodies, Jasper Bodies, Coloured Bodies for Mosaic Painting, Encaustic Tile Bodies,
Body Stains, Coloured Dips. II., Glazes. China Glazes, Ironstone Glazes, Earthenware
Glazes, Glazes without Lead, Miscellaneous Glazes, Coloured Glazes, Majolica Colours. III.,
Gold and Cold Colours. Gold, Purple of Cassius, Marone and Ruby, Enamel Coloured
Bases, Enamel Colour Fluxes, Enamel Colours, Mixed Enamel Colours, Antique and Vellum
Enamel Colours, Underglaze Colours, Underglaze Colour Fluxes, Mixed Underglaze Colours,
Flow Powders, Oils and Varnishes. IV., Means and Methods. Reclamation of Waste
Gold, The Use of Cobalt, Notes on Enamel Colours, Liquid or Bright Gold. V., Classification
and Analysis. Classification of Clay Ware, Lord Playfair's Analysis of Clays, The Markets
of the World, Time and Scale of Firing, Weights of Potter's Material, Decorated Goods
Count. VI., Comparative Loss of Weight of Clays. VII., Ground Felspar Calculations.
VIII., The Conversion of Slop Body Recipes into Dry Weight. IX., The Cost of Prepared
Earthenware Clay. X., Forms and Tables. Articles of Apprenticeship, Manufacturer's
Guide to Stocktaking, Table of Relative Values of Potter's Materials, Hourly Wages Table,
Workman's Settling Table, Comparative Guide for Earthenware and China Manufacturers in
the use of Slop Flint and Slop Stone, Foreign Terms applied to Earthenware and China
Goods, Table for the Conversion of Metrical Weights and Measures on the Continent of South
America. Index.
CERAMIC TECHNOLOGY :
Being some Aspects of Tech-
nical Science as Applied to Pottery Manufacture. Edited by CHARLES
F. BINNS. 100 pp. 1897. Price 12s. 6d. India and Colonies, 13s. 6d.
; ;
Other Countries, 15s. ; strictly net, post free.

Contents.
Preface. Chapters I., The Chemistry of Pottery. II., Analysis and Syn-
Introduction.
thesis. Clays and their Components. IV., The Biscuit Oven. V., Pyrometry. VI.,
III.,
Glazes and their Composition. VII., Colours and Colour-making. Index.
RECIPES FOR FLINT GLASS MAKING. By a British

Glass Master and Mixer. Sixty Recipes. Being Leaves from the
Mixing Book of several experts in the Flint Glass Trade, containing
up-to-date recipes and valuable information as to Crystal, Demi-crystal
and Coloured Glass in its many varieties. It contains the recipes for
cheap metal suited to pressing, blowing, etc., as well as the most costly
crystal and ruby. British manufacturers have kept up the quality of
this glass from the arrivals of the Venetians to Hungry Hill, Stour-
bridge, up to the present time. The book also contains remarks as
to the result of the metal as it left the pots by the respective metal
mixers, taken from their own memoranda upon the originals. 1900.
Price for United Kingdom, 10s. 6d. Abroad, 15s. United States, $4
; ; ;

Contents.
Ruby Ruby from Copper Flint for using with the Ruby for Coating A German Metal
Cornelian, or Alabaster Crysophis Opal Turquoise Blue Gold Colour
Sapphire Blue
Dark Green Green (common) Green for Malachite Blue for Malachite Black for Mela-
chite Black Common Canary Batch Canary White Opaque Glass Sealing-wax Red
Flint Flint Glass (Crystal and Demi) Achromatic Glass Paste Glass White Enamel-
Firestone Dead White (for moons) White Agate Canary Canary Enamel Index.
COLOURING AND DECORATION OF CERAMIC

WARE. By ALEX. BRONGNIART. With Notes and Additions
by ALPHONSE SALVETAT. Translated from the French. 200 pp. 1898.
Price 7s. 6d. Abroad, 8s. strictly net, post free.
; ;
Contents.
The Pastes, Bodies or Ceramic Articles Capable of being Decorated by Verifiable Colours
The Chemfcal Preparation of Verifiable Colours Composition and Preparation of Verifiable
Colours The Oxides Preparation of Oxides Preparation of Chromates Preparation of
other Colours Composition and Preparation of Fluxes Muffle Colours Recipes for Colours
Use of Metals Lustres Preparation and Application of Colours Composition of Coloured
Pastes Underglaze Colours Colours in the Glaze Overglaze Colours Painting in Vitri-
fiable Colours Gilding Burnishing Printing Enlarging and Reducing Gelatine Prints
Muffle Kilns for Verifiable Colours Influence of the Material on the Colour Changes Re-
sulting from the Actions of the Fire Alterations Resulting from the Colours Alterations in
Firina.
17
HOW TO ANALYSE CLAY. Practical Methods for Prac-

tical Men. By HOLDEN M. ASHBY, Professor of Organic Chemistry,
Harvey Medical College, U.S.A. Twenty Illustrations. 1898. Price
2s. 6d. ; strictly net, post free, home or abroad.
Contents.
List of Apparatus List of Atomic Weights Use of Balance, and Burette, Sand Bath, and
ater Bath Dessicator Dry ing Oven Filtering Fusion Determination of Water, Organic
Matter, Iron, Calcium, Alkalies, Limestone, Silica, Alumina Magnesium, etc. Mechanical
Analysis Rational Analysis Standard Solutions Volumetric Analysis Standards for Clay
Analysis Sampling.
Architectural Pottery.
ARCHITECTURAL POTTERY. Bricks, Tiles, Pipes, Ena-
melled Terra-cottas, Ordinary and Incrusted Quarries, Stoneware
Mosaics, Faiences and Architectural Stoneware. By LEON LEFEVRE.
With Five Plates. 950 Illustrations in the Text, and numerous estimates.
500 pp., royal 8vo. 1900. Translated from the French by K. H. BIRD,
M.A., and W. MOORE BINNS. Price 15s. India and Colonies, 16s. ; ;
Other Countries, 17s. 6d. ; strictly net, post free.

Contents.
Part I. Plain Undecorated Pottery. Chapter I., Clays: g 1, Classification, General Geo-
logical Remarks. Classification, Origin, Locality; 2, General Properties and Composition:

Physical Properties, Contraction, Analysis, Influence of Various Substances on the Properties
of Clays 5 3, Working of Clay-Pits I. Open Pits Extraction, Transport, Cost II. Under-
: :
ground Pits Mining Laws. Chapter II., Preparation of the Clay Weathering, Mixing,
:
Cleaning, Crushing and Pulverising Crushing Cylinders and Mills, Pounding Machines-
Damping Damping Machines Soaking, Shortening, Pugging Horse and Steam Pug-Mills,
: :
Rolling Cylinders Particulars of the Above Machines. Chapter III., Bricks 1, Manufacture :
(1) Hand and Machine Moulding. I. Machines Working by Compression on Soft Clay, on
:
Semi-Firm Clay, on Firm Clay, on Dry Clay. II. Expression Machines with Cylindrical Pro- :
pellers, with Screw Propellers Dies Cutting-tables Particulars of the Above Machines
General Remarks on the Choice of Machines Types of Installations Estimates Plenishing,
Hand and Steam Presses, Particulars (2) Drying, by Exposure to Air, Without Shelter, and
Under Sheds Drying-rooms in Tiers, Closed Drying-rooms, in Tunnels, in Galleries De-
tailed Estimates of the Various Drying-rooms, Comparison of Prices Transport from
the Machines to the Drying-rooms, Barrows, Trucks, Plain or with Shelves, Lifts <3) Firing
I. In Clamps II. In Intermittent Kilns. A, Open :a, using Wood b Coal; b', in Clamps
; ;
b", Flame B, Closed: c, Direct Flame; c', Rectangular; c", Round; d, Reverberatory III.
Continuous Kilns C, with Solid Fuel Round Kiln, Rectangular Kiln, Chimneys (Plans and
: :
Estimates)!), With Gas Fuel, Fillard Kiln (Plans and Estimates), Schneider Kiln (Plans and
Estimates), Water-gas Kiln Heat Production of the Kilns 2, Dimensions, Shapes, Colours,
; ,5
Decoration, and Quality of Bricks Hollow Bricks, Dimensions and Prices of Bricks, Various
Shapes, Qualities Various Hollow Bricks, Dimensions, Resistance, Qualities 3, Applications ;
History Asia, Africa, America, Europe Greek, Roman, Byzantine, Turkish, Romanesque,
:
Gothic, Renaissance, Architecture Architecture of the Nineteenth Century in Germany, :
England, Belgium, Spain, Holland, France, America Use of Bricks Walls, Arches, Pavements,
Flues, Cornices Facing with Coloured Bricks Balustrades. Chapter IV., Tiles: 1, His-
tory': 2, Manufacture (1) Moulding, by Hand, by Machinery: Preparation of the Clay, Soft
Paste, Firm Paste, Hard Paste Preparation of the Slabs, Transformation into Flat Tiles, into
Jointed Tiles Screw, Cam and Revolver Presses Particulars of Tile-presses (2) Drying
Planchettes, Shelves, Drying-barrows and Trucks (3) Firing Divided Kilns Installation of
Mechanical Tileworks Estimates $ 3, Shapes, Dimensions and Uses of the Principal Types
;
of Tile Ancient Tiles: Flat, Round, Roman, Flemish Modern Tiles With Vertical Inter-
rupted Join: Gilardoni's, Martin's; Hooked, Boulet's Villa with Vertical Continuous Join:
;
Muller's, Alsace, Pantile Foreign Tiles Special Tiles Ridge Tiles, Coping Tiles, Border
Tiles, Frontons, Gutters, Antefixes, Membron, Angular Roofing Accessories Chimney-pots, :
Mitrons, Lanterns, Chimneys Qualities of Tiles Black Tiles Stoneware Tiles Particulars
of Tiles. Chapter V., Pipes: I. Conduit Pipes Manufacture Moulding Horizontal :
Machines, Vertical Machines, Worked by Hand and Steam Particulars of these Machines
" "
Dry-ing Firing II. Chimney Flues Ventiducts and Boisseaux," Waggons "Particular-
of these Products. Chapter VI., Quarries 1, Plain Quarries of Ordinary Clay 2, of Cleaned
: ;
Clay Machines, Cutting, Mixing, Polishing Drying and Firing Applications Particulars of
Quarries. Chapter VII., Terra-cotta History Manufacture Application
: Balustrades, :
Columns, Pilasters, Capitals, Friezes, Frontons, Medallions, Panels, Rose-windows, Ceilings

Appendix: Official Methods of Testing Terra-cottas.
Part II. Made-up or Decorated Pottery. Chapter L, General Remarks on the Deco-
ration of Pottery' Dips Glazes
:
Composition, Colouring, Preparation, Harmony with
:
18
Pastes Special Processes of Decoration Enamels, Opaque, Transparent, Colours. Under-

glaze, Over-glaze Other Processes Crackling, .Mottled, Flashing, Metallic Iridescence,
:
Lustres. Chapter II., Glazed and Enamelled Bricks History Glazing Enamelling Appli-
:
cations: Ordinary Enamelled Bricks, Glazed Stoneware, Enamelled Stoneware Enamelled

Tiles. Chapter III., Decorated Quarries: I. Paving Quarries 1, Decorated with Dips 2,
Stoneware: A, Fired to Stoneware; a, of Slag Base Applications: b, of Melting Clay
Applications B, Plain or Incrusted Stoneware a, of Special Clay (Stoke-on-Trent) Manu-
;
facture Application b, of Felspar Base Colouring, Manufacture, Moulding, Drying, Firing

Applications. II. Facing Quarries 1, in Faience A, of Limestone Paste B, of Silicious
Paste C, of Felspar Paste Manufacture, Firing 2, of Glazed Stoneware 3, of Porcelain
Applications of Facing Quarries. III. Stove Quarries Preparation of the Pastes, Moulding,
Firing, Enamelling, Decoration Applications Faiences for Fireplaces. Chapter IV., Archi-
tectural Decorated Pottery: 1, Faiences; 2, Stoneware; 3, Porcelain. Chapter V.,
Sanitary Pottery: Stoneware Pipes Manufacture, Firing Applications Sinks Applications
:
Urinals, Seats and Pans Applications Drinking-fountains, Washstands. Index.
Press Opinions.
" The work is
profusely illustrated, and contains a large amount of useful information, and
should be of great value to manufacturers." Burton Chronicle.
" Should have a
huge sale amongst those interested in enamelled terra cottas, ordinary and
incrusted quarries, stoneware mosaics, faiences, and architectural stoneware." Newark
A dvertiser.
"The fame of M. Lefevre's monumental work has already reached this country, and the
capable translation now produced will be cordially welcomed. Apart from its technical
value, the incitement which the work will give to architectural pottery is a factor that should
not be ignored. . The chief value of the work is that all modern processes advocated are
. .
not only clearly explained, but are shown to have justified themselves. In other words, they
nt the survival of the fittest." Manchester Courier.
THE ART OP RIVETING GLASS, CHINA AND

EARTHENWARE. By J. HOWARTH. Second Edition.
1900. Price Is. net ; by post, home or abroad, Is. 2d.
Contents.
Tools and Materials Required Wire Used for Rivets Soldering Solution Preparation
Commencement of Drilling Cementing
for Drilling Preliminaries to Riveting Rivets
Make To Fix the Rivets Through-and-through Rivets Soldering Tinning aaSolde
Soldering-iron
êrforated Plates, Handles, etc. Handles of Ewers, etc. Vases and Comports Marble
Alabaster Ware Decorating How to Loosen Fast Decanter Stoppers China Cements.
PAINTING ON GLASS AND PORCELAIN AND

ENAMEL PAINTING. A Complete Introduction to the
Preparation of the Colours and Fluxes used for Painting on Porce-
all
lain, Enamel, Faience and Stoneware, the Coloured Pastes and Col-
oured Glasses, together with a Minute Description of the Firing of
Colours and Enamels. On the Basis of Personal Practical Experience
of the Condition of the Art up to Date. By FELIX HERMANN, Technical
Chemist. With Eighteen Illustrations. 300 pp. Translated from the
German. Second and Enlarged Edition. 1897. Price 10s. 6d. India ;
and Colonies, 11s.; Other Countries, 12s.; strictly net, post free.
Contents.
History of Glass Painting. Chapters I., The Articles to be Painted Glass, Porcelain, :
Enamel, Stoneware, Faience. II., Pigments: 1, Metallic Pigments: Antimony Oxide, Naples
Yellow, Barium Chromate, Lead Chromate, Silver Chloride, Chromic Oxide. III., Fluxes:
Fluxes, Felspar, Quartz, Purifying Quartz, Sedimentation, Quenching, Borax, Boracic Acid,
Potassium and Sodium Carbonates, Rocaille Flux. IV., Preparation of the Colours for Glass
Painting. V., The Colour Pastes. VI., The Coloured Glasses. VII., Composition of the
Porcelain Colours. VIII., The Enamel Colours: Enamels for Artistic Work. IX., Metallic
Ornamentation: Porcelain Gilding, Glass Gilding. X., Firing the Colours: 1, Remarks on
Firing: Firing Colours on Glass, Firing Colours on Porcelain; 2, The Muffle. XI., Accidents
occasionally Supervening during the Process of Firing. XII., Remarks on the Different
Methods of Painting on Glass, Porcelain, etc. Appendix: Cleaning Old Glass Paintings.
Press Opinions.
Mr. Hermann, by a careful division of his subject, avoids much repetition, yet makes
4
tufficiently clear what is necessary to be known in each art. He gives very many formulae ;
and his hints on the various applications of metals and metallic lustres to glass and porcelains
llbe found of much interest to the amateur." Art Amateur, New York.
19
"For the unskilled and amateurs the name of the publishers will be sufficient guarantee tor
the utility and excellence of Mr. Hermann's work, even if they are already unacquainted with
the author. . The whole cannot fail to be both of service and interest to glass workers and
. .
to potters generally, especially those employed upon high-class work." Staffordshire Sentinel.
" In
Painting on Glass and Porcelain the author has dealt very exhaustively with the
technical as distinguished from the artistic side of his subject, the work being entirely devoted
to the preparation of the colours, their application and firing. For manufacturers and students
it will be a valuable work, and the recipes which appear on almost
every page form a very
valuable feature. The author has gained much of his experience in the celebrated Sevres
manufactory, a fact which adds a good deal of authority to the work." Builders Journal.
"
The compiler displays that painstaking research characteristic of his nation, and goes at
length into the question of the chemical constitution of the pigments and fluxes to be used in
glass-painting, proceeding afterwards to a description of the methods of producing coloured
glass of all tints and shades. .
Very careful instructions are given for the chemical and
. .
mechanical preparation of the colours used in glass-staining and porcelain-painting indeed,;
to the china painter such a book as this should be of permanent value, as the author claims to
have tested and verified every recipe he includes, and the volume also comprises a section de-
voted to enamels both opaque and translucent, and another treating of the firing of porcelain,
and the accidents that occasionally supervene in the furnace." Daily Chronicle.
"In Dr. Hermann's hand-book if such a term is fitting for so erudite and masterly a treatise
the student is first delighted by an interesting historical introduction, after which an ex-
haustive description follows of the metallic oxides and salts, the earths and earthy bodies and
the free metals used in the composition of the pigments. All who take an interest in the
colouring properties of matter will not fail to be instructed in this section of the work. . .
.
Exhaustive recipes are given in separate chapters for the composition of the colours and
fluxes for every shade and tint in the painting of glass, porcelain, enamel, faience, and stone-
ware, for the preparation of coloured pastes, for the application of metallic ornamentation, for
the colouring of the foundation in the 'frit 'or 'charge' stage, and for the encaustic opera-
tions in the kiln. ... In every district of England where art porcelain and glass is manu-
factured, this treatise should be widely circulated, and its contents made familiar to <ill engaged,
in whatever capacity, in the trade." Leeds Mercury.
A Reissue of
THE HISTORY OP THE STAFFORDSHIRE POTTER-
IES AND THE RISE AND PROGRESS OF THE
;
MANUFACTURE OF POTTERY AND PORCELAIN.

With References to Genuine Specimens, and Notices of Eminent Pot-
ters. By SIMEON SHAW. (Originally Published in 1829.) 265 pp.
1900. Price 7s. 6d. India and Colonies, 8s. Other Countries, 8s. 6d.
; ; ;

Contents.
Introductory Chapter showing the position of the Pottery Trade at the present time
(1899). Chapters I., Preliminary Remarks. II., The Potteries, comprising Tunstall,
Brownhills, Greenfield and New Field, Golden Hill, Latebrook, Green Lane, Burslem, Long-
port and Dale Hall, Hot Lane and Cobridge, Hanley and Shelton, Etruria, Stoke, Penkhull,
Fenton, Lane Delph, Foley, Lane End. III., On the Origin of the Art, and its Practice
among the early Nations. IV., Manufacture of Pottery, prior to 1700. V., The Introduc-
tion of Red Porcelain by Messrs. Elers, of Bradwell, 1690. VI., Progress of the Manu-
facture from 1700 to Mr. Wedgwood's commencement in 1760. VII. Introduction of Fluid
Glaze. Extension of the Manufacture of Cream Colour. Mr. Wedgwood's Queen's Ware.
Jasper, and Appointment of Potter to Her Majesty. Black Printing. VIII., Introduction
Of Porcelain. Mr. W. Littler's Porcelain. Mr. Cookworthy's Discovery of Kaolin and
Petuntse, and Patent. Sold to Mr. Champion resold to the New Hall Com. Extension of
Term. IX., Blue Printed Pottery. Mr. Turner, Mr. Spode (1), Mr. Baddeley, Mr. Spode
(2), Messrs. Turner, Mr. Wood, Mr. Wilson, Mr. Minton. Great Change in Patterns of Blue
Printed. X., Introduction of Lustre Pottery. Improvements in Pottery and Porcelain
subsequent to 1800.
Press Opinions.
"There is much curious and useful information in the work, and the publishers have rendered
the public a service in reissuing it." Burton Mail.
"
Copies of the original work are now of considerable value, and the facsimile reprint now
issued cannot but prove of considerable interest to all interested in the great industry." Derby
Mercury.
" The book will be of pottery manu-
especially welcomed at a time when interest in the art
facture commands a more widespread and general interest than at any previous time.'
Wolvcrhampton Chronicle.
"This work is all the more valuable because it gives one an idea of the condition of affairs
existing in the north of Staffordshire before the great increase in work and population
due to
modern developments." Western Morning News.
"... The History gives a graphic picture of North Staffordshire at the end of the last and
the beginning of the present century, and states that in 1829 there was a busy and enterprising
'
community in the Potteries of fifty thousand persons. ... We commend it to our readers <^s
'
most entertaining and instructive publication." Staffordshire Sentinel.

20
A Reissue of
THE CHEMISTRY OF THE SEVERAL NATURAL
AND ARTIFICIAL HETEROGENEOUS COM-
POUNDS USED IN MANUFACTURING POR-
CELAIN, GLASS AND POTTERY. By SIMEON SHAW.
(Originally published in
1837.) 750 pp. 1900. Price 14s. ;
India and
Colonies, 'l 5s.
; Other Countries, 16s. 6d. ; strictly net, post free.
Contents.
PART I., ANALYSIS AND MATERIALS. Chapters I., Introduction Laboratory and :
Apparatus; Elements: Combinative Potencies, Manipulative Processes for Analysis and

Reagents, Pulverisation, Blow-pipe Analysis, Humid Analysis, Preparatory Manipulations,
General Analytic Processes, Compounds Soluble in Water, Compounds Soluble only in Acids,
Compounds (Mixed) Soluble in Water, Compounds (Mixed) Soluble in Acids, Compounds
(Mixed) Insoluble, Particular Analytic Processes. II., Temperature Coal, Steam Heat for
:
Printers' Stoves. III., Acids and Alkalies: Boracic Acid, Muriatic Acid, Nitric Acid, Sul-
phuric Acid, Potash, Soda, Lithia, Calculation of Chemical Separations. IV., The Earths :
Alumine, Clays, Silica, Flint, Lime, Plaster of Paris, Magnesia, Barytes, Felspar, Grauen (or
China Stone), China Clay, Chert. V., Metals : Reciprocal Combinative Potencies of the Metals,
Antimony, Arsenic, Chromium, Green Oxide, Cobalt, Chromic Acid, Humid Separation of
Nickel from Cobalt, Arsenite of Cobalt, Copper, Gold, Iron, Lead, Manganese, Platinum, Silver,
Tin, Zinc.
PART II., SYNTHESIS AND COMPOUNDS. Chapters I., Sketch of the Origin and
Progress of the Art. II., Science of Mixing Scientific Principles of the Manufacture, Com-
:
binative Potencies of the Earths. III., Bodies Porcelain Hard, Porcelain Fritted Bodies,
:
Porcelain Raw Bodies, Porcelain Soft, Fritted Bodies, Raw Bodies, Stone Bodies, Ironstone,
Dry Bodies, Chemical Utensils, Fritted Jasper, Fritted Pearl, Fritted Drab, Raw Chemical
Utensils, Raw Stone, Raw Jasper, Raw Pearl, Raw Mortar, Raw Drab, Raw Brown, Raw Fawn,
Raw Cane, Raw Red Porous, Raw Egyptian, Earthenware, Queen's Ware, Cream Colour, Blue
and Fancy Printed, Dipped and Mocha, Chalky, Rings, Stilts, etc. IV., Glazes Porcelain :
Hard Fritted, Porcelain Soft Fritted, Porcelain Soft Raw, Cream Colour Porcelain, Blue
Printed Porcelain, Fritted Glazes, Analysis of Fritt, Analysis of Glaze, Coloured Glazes, Dips,
Smears and Washes; Glasses: Flint Glass, Coloured Glasses, Artificial Garnet, Artificial
Emerald, Artificial Amethyst, Artificial Sapphire, Artificial Opal, Plate Glass, Crown Glass,
Broad Glass, Bottle Glass, Phosphoric Glass, British Steel Glass, Glass-Staining and Painting,
Engraving on Glass, Dr. Faraday's Experiments. V., Colours Colour Making, Fluxes or
:
Solvents, Components of the Colours; Reds, etc., from Gold, Carmine or Rose Colour,
Purple, Reds, etc., from Iron, Blues, Yellows, Greens, Blacks, White, Silver for Burnishing,
Gold for Burnishing, Printer's Oil, Lustres.
PART HI., TABLES OF THE CHARACTERISTICS OF CHEMICAL SUB-
STANCES. Preliminary Remarks, Oxygen (Tables), Sulphur and its Compounds, Nitrogen
ditto, Chlprineiditto, Bromine ditto, Iodine ditto, Fluorine ditto, Phosphorous ditto, Boron ditto,
Carbon ditto, Hydrogen ditto, Observations, Ammonium and its Compounds (Tables), Thorium
ditto, Zirconium ditto, Aluminium ditto, Yttrium ditto, Glucinum ditto, Magnesium ditto,
Calcium ditto, Strontium ditto, .Barium ditto, Lithium ditto, Sodium and its Compounds,
Potassium ditto, Observations, Selenium and its Compounds (Tables), Arsenic ditto, Chromium
ditto, Vanadium ditto, Molybdenum ditto, Tungsten ditto, Antimony ditto, Tellurium ditto,
Tantalum ditto, Titanium ditto, Silicium ditto, Osmium ditto, Gold ditto, Iridium ditto, Rhodium
ditto, Platinum ditto, Palladium ditto, Mercury ditto, Silver ditto, Copper ditto, Uranium ditto.
Bismuth and its Compounds, Tin ditto, Lead ditto, Cerium ditto, Cobalt ditto, Nickel ditto,
Iron ditto, Cadmium ditto, Zinc ditto, Manganese ditto, Observations, Isomorphous Groups,
Isomeric ditto, Metameric ditto, Polymeric ditto, Index.
Press Opinions.
"The atomic weights have been more accurately determined, and experiments in synthetic
chemistry have given us readier methods of producing certain materials requisite, but the
fundamental principles were always discovered, and for all practical purposes the book is a?
valuable now as when first published." Longton Times and Echo.
"This interesting volume has been kept from the pencil of the modern editor and reprinted
in its entirety by the enterprising publishers of The Pottery Ga zette and other trade journals.
.. .There is an excellent historical sketch of the origin'and progress of the art of pottery
which shows the intimate knowledge of classical as well as (the then) modern scientific litera-
ture possessed by the late Dr. Shaw; even the etymology of many of the Staffordshire place-
names is given." Glasgow Herald.
"The historical sketch of the origin and progress of pottery is very interesting and instruc-
tive. The science of mixing is a problem of great importance, and the query how the natural
products, alumina and silica can be compounded to form the best wares may be solved by the
aid of chemistry instead of by guesses, as was formerly the case. This portion of the book may
be most suggestive to the manufacturer, as also the chapters devoted to the subject of glazes,
glasses and colours." Birmingham Post.
"
Messrs. Scott, Greenwood & Co. are doing their best to place before the pottery trades
some really good books, likely to aid the Staffordshire manufacturers, and their spirited enter-
prise is worthy of encouragement, for the utility of technical literature bearing upon the
21
j.ractical side of potting goes without saying. .*f|They are to be congratulated on their . .
enterprise in republishing it, and we can only hope that they will meet with the support they
deserve. It seems to be a volume that is worth looking through by both manufacturers and
operatives alike, and all local institutions, at any rate, should secure copies." Staffordshire
Sentinel.
Paper Making.
THE DYEING OF PAPER PULP. Practical Treatise for A
the use of Papermakers, Paperstainers, Students and others. By
JULIUS ERFURT, Paper Mill. Translated into English
Manager of a
and Edited with Additions by JULIUS HUBNER, F.C.S., Lecturer on
Papermaking at the Manchester Municipal Technical School. With
Illustrations and 157 patterns of paper dyed in the pulp. Royal 8vo,
180 pp. 1901. Price 15s. India and Colonies, 16s. Other Countries, ; ;
20s. strictly net, post free.

;
Limited edition.
Contents.
I., Behaviour of the Paper Fibres during the Process of Dyeing, Theory of the
Mordant Cotton Flax and Hemp; Esparto; Jute; Straw Cellulose; Chemical and Mechani-
;
calWood Pulp; Mixed Fibres; Theory of Dyeing. II., Colour Fixing Mediums (Mordants)
Alum; Aluminium Sulphate; Aluminium Acetate; Tin Crystals (Stannous Chloride); Cop-
peras (Ferrous Sulphate); Nitrate of Iron (Ferric Sulphate) ; Pyrolignite of Iron (Acetate of
Iron) Action of Tannic Acid Importance of Materials containing Tannin Treatment with
: ; ;
Tannic Acid of Paper Pulp intended for dyeing Blue Stone (Copper Sulphate) Potassium ; ;
Bichromate; Sodium Bichromate; Chalk (Calcium Carbonate); Soda Crystals (Sodium Car-
bonate) Antimony Potassium Tartrate (Tartar Emetic). III., Influence of the Quality Of
;
the Water Used. IV., Inorganic Colours 1. Artificial Mineral Colours: Iron Buff; Man-
ganese Bronze Chrome Yellow (Chromate of Lead) Chrome Orange (Basic Chromate of
; ;
Lead); Red Lead; Chrome Green; Blue with Yellow Prussiate Prussian Blue; Method for ;
Producing Prussian Blue free from Acid; Ultramarine 2, Natural Mineral Colours (Earth
Colours): Yellow Earth Colours; Red Earth Colours; Brown Earth Colours; Green, Grey and
Black Earth Colours; White Earth Colours; White Clay (China Clay): White Gypsum;
Baryta; Magnesium Carbonate; Talc, Soapstone. V., Organic Colours I. Colours of
Vegetable and Animal Origin: (a) Substantive (Direct Dyeing) Colouring Matters: Annatto;
Turmeric Safflower (b) A djectire (Indirect Dyeing) Colouring Matters Redwood Cochineal
; ;
: ; ;
Weld Persian Berries Fustic Extract Quercitron Catechu (Cutch) Logwood Extract 2.
; ; ; ; ;
Artificial Organic (Coal Tar) Colours: Acid Colours; Basic Colours; Substanti\-e (Direct
00
Dyeing) Colours; Dissolving of the Coal Tar Colours; Auramine Naphthol Yellow S; ;
Quinoline Yellow Metanil Yellow Paper Yellow Azoflavine RS, S; Cotton Yellow
; : ;
GXX and Rxx; Orange 11; Chrysoidine A00 Vesuvine Extra 00 Vesuvine Fast , RL; ; BC;
Brown-, Naphthylamine Brown Water Blue IN Water Blue TB Victoria Blue B ; Methy ; ; ;
lene Blue MD 0: Nile Blue New Blue S :Indoine Blue R;

Eosine442 NX; Phloxine ; BB;
BBN Rhodamine
: Rhodamine B;
Naphthylamine Red G; Fast Red A; Cotton
2 R; Fast Ponceau G and
6G;
Scarlet Erythrine RR: Erythrine X; Erythrine P; Ponceau 00
;
B z Paper Scarlet
; Saffranine PP Magenta Powder A P; Acetate of Magenta 00 ; ; ;
Cerise D 10; Methyl Violet Crystal Violet

00
BB;
Acid Violet 3 BN, 4 R; Diamond ;
Green B Nigrosine Coal

: Black 00 Brilliant Black B. WL;
VI., Practical Application ;
of the Coal Tar Colours according to their Properties and their Behaviour towards
the Different Paper Fibres Coal Tar Colours, which rank foremost, as far as their fastness
to light is concerned Colour Combinations with which colourless or nearly colourless Back-
;
water is obtained Colours which do not bleed into White Fibres, for Blotting and Copying
;
Paper Pulp: Colours which produce the best results on Mechanical Wood and on Unbleached
Sulphite Wood; Dyeing of Cotton, Jute and Wool Half-stuff for Mottling White or Light
Coloured Papers; Colours suitable for Cotton; Colours specially suitable for Jute Dyeing;
Colours suitable for Wool Fibres. VII., Dyed Patterns on Various Pulp Mixtures-
Placard and Wrapping Papers: Black Wrapping and Cartridge Papers; Blotting Papers;
Mottled and Marbled Papers made with Coloured Linen, Cotton and Union Rags, or with
Cotton, Jute, Wool and Sulphite Wood Fibres, dyed specially for this purpose; Mottling with
Dark Blue Linen Mottling with Dark Blue Linen and Dark Blue Cotton Mottling with Dark
: :
Blue Cotton Mottling with Dark Blue and Red Cotton Mottling with Dark Red Cotton
; ; ;
Mottling of Bleached Stuff, with 3 to 4 per cent, of Dyed Cotton Fibres; Mottling with Dark
Blue Union (Linen and Wool or Cotton Warp with Wool Weft) Mottling with Blue Striped ;
Red Union Mottling of Bleached Stuff with 3 to 4 per cent, of Dyed Wool Fibres; Mottling
:
of Bleached Stuff with 3 to 4 per cent, of Dyed Jute Fibres: Mottling of Bleached Stuff with
3 to 4 per cent, of Dyed Sulphite Wood Fibres: Wall Papers: Packing Papers. VIII.,
Dyeing to Shade Index.
Press Opinion.
"The of actual patterns of dyed
great feature of the volume is undoubtedly the series
to the original German
papers, 157 in all twelve of which, made in England, have been added
22
series. Detailed formulae are given for the preparation of the pulp for each, and the tints of
the samples practically form a key, by means of which the accuracy 6f the student's or
practitioner's experiments can be tested. ... On the whole the publication is one of distinct
importance to the trade, and will no doubt speedily become a standard work of reference
amongst papermakers, both in the 'lab.' and the office, as well as being an excellent text-book
for the use of students in the increasing number of technical institutes in which papermaking
is taught." World's Paper Trade Review.
Enamelling on Metal.
ENAMELS AND ENAMELLING. An Introduction to the
Preparation and Application of all Kinds of Enamels for Technical and.
Artistic Purposes. For Enamel Makers, Workers in Gold and Silver,
and Manufacturers of Objects of Art. By PAUL RANDAU. Translated
from the German. With Sixteen Illustrations. 180 pp. 1900. Price
10s. 6d. India and Colonies, 11s.
;
Other Countries, 12s. strictly net,
; ;
post free.
Contents.
I., II., Composition and Properties of Glass.
Introduction. III., Raw
Materials for the
Manufacture of Enamels. IV., Substances Added to Produce Opacity. V., Fluxes. VI., Pig-
ments. VII., Decolorising Agents. VIII., Testing the Raw
Materials with the Blow-pipe
Flame. IX., Subsidiary Materials. X., Preparing the Materials for Enamel Making. XI.,
Mixing the Materials. XII., The Preparation of Technical Enamels, The Enamel Mass.
XIII., Appliances for Smelting the Enamel Mass. XIV., Smelting the Charge. XV., Com-
position of Enamel Masses. XVI., Composition of Masses for Ground Enamels. XVII.,
Composition of Cover Enamels. XVIII., Preparing the Articles for Enamelling. XIX.,
Applying the Enamel. XX., Firing the Ground Enamel. XXI., Applying and Firing the
Cover Enamel or Glaze. XXII., Repairing Defects in Enamelled Ware. XXIII.,
I., Enamellii
Enamelling
Articles of Sheet Metal. XXIV., Decorating Enamelled Ware. XXV., Specialities
alities in Er
Ena-
melling. XXVI., Dial-plate Enamelling. XXVII., Enamels for Artistic Purp
Purposes, Recipes
for Enamels of Various'Colours. Index"
Press Opinions.
" Should
prove of great service to all who are either engaged in or interested in the art of
enamelling." Jewellers and Watchmakers' Trade Ath-ertisct . .
" I must inform

you that this is the best book ever I have come across on enamels, and it is
worth double its cost." J. MINCHIS, Jr., Porto, Portugal, '22nd July, 1900.
"This is a very useful and thoroughly practical treatise, and deals with every branch of the
enameller's art. The manufacture of enamels of various colours and the methods of their
application are described in detail. Besides the commoner enamelling processes, some of the
more important special branches of the business, such as cloisonne work are dealt with. The
work is well got up, and the illustrations of apparatus are well executed. The translator is
evidently a man well acquainted both with the German language and the subject-matter of the
book." Invention.
"This is a most welcome volume, and one for which we have long waited in this country.
For years we have been teaching design applied to enamelling as well as to several other
crafts, but we have not risen to the scientific side of the question. Here is a handbook dealing
with the composition and making of enamels for application to metals for the most part, but
also for other allied purposes. It is written in a thoroughly practical way, and its author
Paul Randau has made its subject a very particular study. The result, like almost all things
which come from the German chemical expert, is a model of good workmanship and arrange-
ment, and no one who is in search of a handbook to enamelling, no matter whether he is a
craftsman producing his beautiful translucent colours on gold, silver and copper, or the hollow-
ware manufacturer making enamelled saucepans and kettles, can wish for a more useful
practical manual." Birmingham Gazette.
THE ART OF ENAMELLING ON METAL. By W.

NORMAN BROWN. Twenty-eight Illustrations. 60 pp. 1900. Price
2s. 6d. ; Abroad, 3s. ;
Contents.
Chapters I., History Cloisonne Champs Leve Translucent Enamel Surface Painted
Enamels. II., Cloisonne Champs Leves Translucent Painted. III., Painted Enamel
Apparatus Furnaces and Muffles for Firing. IV., The Copper Base or Plate Planishing
Cloisons Champ Leve Plates. V., Enamels Trituration Washing Coating a Plate with
Enamel Firing Ordinary Plaques for Painting Designing Squaring off. VI., Designs for
Cloisonne Designs for Painted Enamels Technical Processes Brushes, etc., Colours
Grisaille Full-coloured Designs.
23
Press Opinion.
"
The information conveyed in The A rt or Enamelling on Metal is as complete as can be ex-
pected in a manual of ordinary length, and is quite ample in all respects to start students in a
most interesting branch of decorative art. All necessary requisites are fully described and
illustrated, and the work is one, indeed, which any one may pursue with interest, for those who
are interested artistically in enamels are a numerous body." Hardware Metals and Machinery.
Books on Textile and Dyeing

Subjects.
THE TECHNICAL TESTING OF YARNS AND TEX-
TILE FABRICS. With Reference to Official Specifica-
tions. Translated from the German of Dr. J. HERZFELD. Sixty-nine
Illustrations. 200 pp. 1898. Price 10s. 6d. ;India and Colonies,
11s.; Other Countries, 12s.; strictly net, post free.
Contents.
Yarn Testing. III., Determining: th Yarn Number. IV., Testing the Length of
Yarns. V'., Examination of the Hxternal Appearance of Yarn. VI., Determining the
Twist of Yarn and Twist. VII.. Determination of Tensile Strength and Elasticity.
VIII., Estimating the Percentage of Fat in Yarn. IX., Determination of Moisture
(Conditioning). Appendix.
Press Opinions.
" It would be well if our
English manufacturers would avail themselves of this important
addition to the extensive list of German publications which, by the spread of technical infor-
mation, contribute in no small degree to the success, and sometimes to the supremacy, of
Germany in almost every branch of textile manufacture." Manchester Courier.
"This is probably the most exhaustive book published in English on the subject dealt with.
. . . We
have great confidence in recommending the purchase of this book by all manu-
facturers of textile goods of whatever kind, and are convinced that the concise and direct way
in which it is written, which has been admirably conserved by the translator, renders it
peculiarly adapted for the use of English readers." Textile Recorder.
" A
careful study of this book enables one to say with certainty that it is a standard work on
the subject. Its importance is enhanced greatly by the probability that we have here, for the
first time in our own language, in one volume, a full, accurate, and detailed account, by a prac-
tical expert, of the best technical methods for the testing of textile materials, whether in the
raw state or in the more or less finished product." Glasgow Herald.
"The author has endeavoured to collect and arrange in systematic form for the first time
all the data relating to both physical and chemical tests as used throughout the whole of the
textile industry, so that not only the commercial and textile chemist, who has frequently to
reply to questions on these matters, but also the practical manufacturer of textiles and his
subordinates, whether in spinning, weaving, dyeing, and finishing, are catered for. . . The
.
book is profusely illustrated, and the subjects of these illustrations are clearly described."
Textile Manufacturer.
DECORATIVE AND FANCY TEXTILE FABRICS.

With Designs and Illustrations. By R. T. LORD. A Valuable Book
for Manufacturers and Designers of Carpets, Damask, Dress and all
Textile Fabrics. 200pp. 1898. 132 Designs and Illustrations. Price
7s. 6d. India and Colonies, 8s. Other Countries, 8s. 6d. strictly net,
; ; ;
post free.
Contents.
Chapters I., A Few Hints on Designing Ornamental Textile Fabrics. II., A Few Hints on
Designing Ornamental Textile Fabrics (continued). III., A Few Hints on Designing Orna-
mental Textile Fabrics (continued). IV., A Few Hints on Designing Ornamental Textile
Fabrics (continued). V., Hints for Ruled-paper Draughtsmen. VI., The Jacquard Machine.
VII., Brussels and Wilton Carpets. VIII., Tapestry Carpets. IX., Ingrain Carpets. X.,
Axminster Carpets. XL, Damask and Tapestry Fabrics. XII., Scarf Silks and Ribbons.
XIII., Silk Handkerchiefs. XIV., Dress Fabrics. XV., Mantle Cloths. XVI., Figured Plush.
XVII., Bed Quilts. XVIII., Calico Printing.
Press Opinions.
"The book can be strongly recommended to studentsand practical men." Textile Coloutist
"Those engaged in the designing of dress, mantle tapestry, carpet and other ornamental
textiles will find this volume a useful work of reference." Leeds Mercury.
24
"The book is commended as a model manual, appearing at an opportune time, since

to be
every day is making known a growing desire for development in British industrial art."
Dundee A dvertiser.
"
Designers especially, who desire to make progress in their calling, will do well to take the
hints thrown out in the first four chapters on 'Designing Ornamental Textile Fabrics'."
Nottingham Daily Guardian.
"The writer's avocation is that of a designer for the trade, and he therefore knows what he
is writing about. The work is well printed and abundantly illustrated, and for the author's
. . .
share of the work we have nothing but commendation. It is a work which the student designei
will find thoroughly useful." Textile Mercury.
POWER-LOOM WEAVING AND YARN NUMBERING,

According to Various Systems, with Conversion Tables. An Auxiliary
and Text-book for Pupils of Weaving Schools, as well as for Self-
Instruction and for General Use by those engaged in the Weaving
Industry. Translated from the German of ANTHON GRUNER. With
Twenty-six Diagrams in Colours. 150 pp. 1900. Crown 8vo. Price
7s. 6d. India and Colonies, 8s. Other Countries, 8s. 6d.
; strictly net,
; ;
post free.
Contents.
I., Power-Loom Weaving in General. Various Systems of Looms. II., Mounting
and Starting- the Power-Loom. English Looms. Tappet or Treadle Looms. Dobbies.
III., General Remarks on the Numbering, Reeling and Packing of Yarn. Appendix.
Useful Hints. Calculating Warps. Weft Calculations. Calculations of Cost Price in Hanks.
Press Opinions.
"
\ long-felt want in the weaving industry has been suppliedjby the issue of a cheap volume
dealing with the subject." Belfast Evening Telegraph.
"The work has been clearly translated from the German and published with suitable
illustrations. The author has dealt very practically with the subject." Bradford Daily
. . .
Telegraph.
"The book, which contains a number of useful coloured diagrams, should prove invaluable
to the student, and its handy form will enable it to become a companion more than some cum-
brous work." Cotton f-'actory Times.
"The book has been prepared with great care, and is most usefully illustrated. It is a capital
text-book for use in the weaving schools or for self-instruction, while all engaged in the weaving
industry will find its suggestions helpful." Northern Daily Telegraph.
"The various systems are.treated in a careful manner; also the different looms and their
manufacture, as well as the whole processes of the work. Yarn numbering according to various
systems, with conversion tables and numerous coloured diagrams, materially assist to a clear
comprehension of the subject." Northern Whig.
"
It will be found most useful by those who have not time to go through the large standard
work, and the volume may be aptly described as a nutshell of power-loom weaving. Yarn
numbering according to various systems is dealt with, and conversion tables included, and we
have no hesitation in commending the book to our readers." Oldham Standard.
"
The ' inside managers of our textile mills in which the work is complex or greatly varied,
'
and where yarns of different materials are in use, will find this work convenient for reference in
case of novelty or difficulty. We
may also say the same in relation to the textile student. Its
description of the parts of the loom and their functions will be of use to the latter, being of the
most elementary kind." Textile Mercury.
"The author attempts to fill a gap in weaving literature caused by the neglect of many
obscure points connected with the industry. A short review is given of the power-loom as a
whole, followed by a description of the different parts of the machinery with their advantages
and defects. The book is severely technical, but must on that account be very valuable to
. . .
i'ho is determined to master this industrial art." Cheshire County .Veu'S.

clear and concise, and gives just that knowledge in quality and amount which any
student of the weaving industry ought to consider as a minimum necessary for his thorough
comprehension of his future profession. The handiness and variety of the information com-
prised in Section III., dealing with the numbering and reeling of yarns employed in the various
systems in different countries, struck us as particularly useful." North British Daily Mail.
"This work brings before weavers who are actually engaged in the various branches of
fabrics, as well as the technical student, the different parts of the general run of power-looms in
such a manner that the parts of the loom and their bearing to each other can be readily under-
stood. . The work should prove of much value, as it is in every sense practical, and is put
. .
before the reader in such a clear manner that it can be easily understood." Textile Industries.
"The book under notice is intended as an instructor to those engaged in power-loom weaving,
and, judging by its compilation, the author is a thorough master of the craft. It is not over-
loaded with details, and he manages to compress in a book of some 150 pages all that one can
possibly wish to know about the different parts of the machinery, whether of English or foreign
make, and for whatever kind of cloth required. A comprehensive summary is also included of
the various yarns and methods of numbering them, as well as a few useful hints and a number
25
of coloured diagrams tor mandarin weavings. The book is printed in bold, legible type, on
good paper, has a copious index, and is well and strongly bound." Ashton-under-Lyne Herald.
" In
dealing with the complicated parts of various classes of power-looms, the writer,' who is
one of the professors at the Royal Weaving School of Asch, brings to the work a thorough
knowledge of the subject, and, what is of great value, he has the gift of communicating his
knowledge in a way which is easily understood. The smallest details of loom-setting are
entered into, and a full explanation of problems, which are a source of anxiety to many en-
gaged in overlooking, is given. Students will find the work an admirable text-book, and all
who are interested in weaving will see in it a valuable addition to the literature on this subject.
. .The book is in small compass, and is crowded with valuable information." Bradford
.
Observer.
" A short and valuable review is
given of the power-loom as a whole, and this is followed by
a description of the mounting of the different parts of the machinery, with their advantages
and defects. In preference to illustrations the readers being presumed to already possess a
suitable acquaintance with the subject the various systems of numbering yarn are explained,
together with certain calculations useful in weaving. How power-loom weaving has
. . .
advanced in recent years is explained at some length in this book, which will prove invaluable
to intending students of practical weaving, and will also be found very useful to those whose
knowledge of the subject is more advanced, to whom the calculations, which give evidence
of careful study, will frequently come in handy." Stockport Advertiser.
COLOUR: A HANDBOOK OF THE THEORY OP

COLOUR. By GEORGE H. HURST, F.C.S. With Ten
Coloured Plates and Seventy-two Illustrations. 160 pp. 1900.
Price 7s. 6d. India
;
and Colonies, 8s. Other Countries, 8s. 6d. ;
;
Contents.
Chapters I., Colour and Its Production. Light, Colour, Dispersion of White Light
Methods of Producing the Spectrum, Glass Prism and Diffraction Grating Spectroscopes, The
Spectrum, Wave Motion of Light, Recomposition of White Light, Hue, Luminosity, Purity
of Colours, The Polariscope, Phosphorescence, Fluorescence, Interference. II., Cause of
Colour in Coloured Bodies. Transmitted Colours, Absorption Spectra of Colouring
Matters. III., Colour Phenomena and Theories. Mixing Colours, White Light from
Coloured Lights, Effect of Coloured Light on Colours, Complementary Colours, Young-
Helmholtz Theory, Brewster Theory, Supplementary Colours, Maxwell's Theory, Colour
Photography. IV., The Physiology of Light. Structure of the Eye, Persistence of Vision,
Subjective Colour Phenomena, Colour Blindness. V., Contrast. Contrast, Simultaneous
Contrast, Successive Contrast, Contrast of Tone Contrast of Colours, Modification of Colours
by Contrast, Colour Contrast in Decorative Design. VI., Colour in Decoration and
Design. Colour Harmonies, Colour Equivalents, Illumination and Colour, Colour and
Textile Fabrics, Surface Structure and Colour. VII., Measurement ofjColour. 'Colour
Patch Method, The Tintometer, Chromometer.
Press Opinions.
" This useful little book possesses considerable merit, and
will be of great utility to those for
whom it is primarily intended." Birmingham Post.
" It will be found to be of direct service to the
majority of dyers, calico printers and colour
mixers, to whom we confidently recommend it." Chemical Trade Journal.
" It is
thoroughly practical, and gives in simple language the why and wherefore of the many
colour phenomena which perplex the dyer and the colourist." Dyer and Calico Printer.
" We
have found the book very interesting, and can recommend it to all who wish to master
the different aspects of colour theory, with a view to a practical application of the knowledge so
gained." Chemist and Druggist.
"
Mr. Hurst's Handbook on the Theory of Colour will be found extremely useful, not only to
the art student, but also to the craftsman, whose business it is to manipulate pigments and
dyes." Nottingham Daily Guardian.
"This is a workmanlike technical manual, which explains the scientific theory of colour in
terms intelligible to everybody. ... It cannot but prove both interesting and instructive to ail
classes of workers in colour." Scotsman.
THE COLOUR PRINTING OF CARPET YARNS. A

Useful Manual for Colour Chemists and Textile Printers. By DAVID
PATERSON, F.C.S. Seventeen Illustrations. 132 pp. 1900. Price
7s. 6d.;
India and Colonies, 8s. Other Countries, 8s. 6d. strictly net,,
;
post free.
26
Contents.
Chapters Structure and Constitution of Wool Fibre. II., Yarn Scouring. III., Scouring
I.,
Materials. Water for Scouring. V., Bleaching Carpet Yarns. VI., Colour Making for
IV.,
Yarn VII., Colour Printing Pastes. VIII., Colour Recipes for Yarn Printing.
Printing.
IX., Science of Colour Mixing.-X., Matching of Colours.-XI., "Hank" Printing. XII.,
Printing Tapestry Carpet Yarns. XIII., Yarn Printing. XIV., Steaming Printed Yarns.
XV., Washing of Steamed Yarns. XVI., Aniline Colours Suitable for Yarn Printing.-XVII.,
Glossary of Dyes and Dye-wares used in Wood Yarn Printing. Appendix/
Press Opinions.
"The book is worthy the attention of the trade." Woraster Herald.
"The treatise is arranged with great care, and follows the processes described in a manner
at once clear and convincing." Glasgow Record.
"A most useful manual dealing in an intelligible and interesting manner with the colour
printing of carpet yarns." Kidderminster Times.
" An eminent order to make
expert himself, the author has evidently strained every effort in
his work the standard guide of its class." Leicester Post.
" The
book, which is admirably printed and illustrated, should fulfil the need of a practical
guide in the colour printing of carpet yarns. Nottingham Express.
"The subject is very exhaustively treated in all its branches. . .The work,
. which is very
well illustrated with designs, machines, and wool fibres, will be a useful addition to our textile
literature." Northern Whig.
" It an account of its which is both valuable and instructive in and likely
gives subject itself,
to be all the more welcome because books dealing with textile fabrics usually have little or
nothing to say about this way of decorating them." Scotsman.
"The work shows a thorough grasp of the leading characteristics as well as the minutse of
the industry, and gives a lucid description of its chief departments. ... As a text-book in
technical schools where this branch of industrial education is taught.jthe book is valuable, or
it may be perused with pleasure as well as profit by any one having an interest in textile in-
dustries." Dundee Courier.
" The book bears
every mark of an extensive practical knowledge of the subject in all its
bearings, and supplies a real want in technical literature. Chapters IX. and X., on the science
of colour mixing and colour matching respectively, are especially good, and we do not remem-
ber to have seen the bearing of various kinds of light, and of the changes from one kind of light
to another on the work of the colourist, so well treated elsewhere." Dyer and Calico Printer.
"
It is thoroughly practical, and contains much information which has not hitherto appeared
in book form. It is pleasing to note that the practical part is not crowded out with purely
practical recipes '. A few typical examples are given, and the rest is left to the common sense
'
and judgment of the printer or works' chemist. Another pleasing feature is the accounts given
here and there of the author's own researches on the subject. The work will be of interest to
printers of wool generally, and to those engaged in the dyeing of this fibre." Journal of the
Society of Dyers and Colourists.
A PRACTICAL TREATISE ON THE BLEACHING OP

LINEN AND COTTON YARN AND FABRICS. By
L. TAILFER,Chemical and Mechanical Engineer. Translated from the
French by JOHN GEDDES MC!NTOSH, Lecturer on Chemical Technology,
London. 1901. Price 12s. 6d. India and Colonies, 13s. 6d
;
Other ;
Countries, 15s. ; strictly net, post free.
Contents.
Chapter I. General Considerations on Bleaching.
Chapter II. Steeping. Chapter III
Washing: Its End and Importance Washing Machines Wash Wheel (Dash Wheel)
Roller
Stocks or Wash Squeezing. Chapter IV. Lye Boiling Lye Boiling with Milk of Lime
Mill
Lye Boiling with Soda Lyes Description of Lye Boiling Keirs Operations of Lye Boiling
Concentration of Lyes. Chapter V. Mather and Platt's Keir Description of the Keir
Saturation of the Fabrics Alkali used in Lye Boiling Examples of Processes. Chapter VI.
Soap Action of Soap in Bleaching Quality and Quantity of Soaps to use in the Lye Soap
Lyes or Scalds Soap Scouring Stocks. Chapter VII. Bleaching on Grass or on the Bleach-
ing Green or Lawn. Chapter VIII. Chemicking Remarks on Chlorides and their De-
colourising Action Chemicking Cisterns Chemicking Strengths, etc. Chapter IX. Sours
Properties of the Acids Effects Produced by Acids Souring Cisterns! Chapter X.
Drying Drying by Steam Drying by Hot Air Drying by Air. Chapter XI. Damages to
Fabrics in Bleaching Yarn Mildew Fermentation Iron Rust Spots Spots from Contact
with Wood Spots incurred on the Bleaching Green Damages arising from the Machines.
Chapter XII. Examples of Methods used in Bleaching Linen Cotton. Chapter XII). The
Valuation of Caustic and Carbonated Alkali (Soda) and General Information Regarding these
Bodies Object of Alkalimetry Titration of Carbonate of Soda Comparative Table of
Different Degrees of Alkalimetrical Strength Five Problems relative to Carbonate of Soda
Caustic Soda, its Properties and Uses Mixtures of Carbonated and Caustic Alkali Note
27
on a Process of Manufacturing Caustic Soda and .Mixtures of Caustic and Carbonated Alkali
(Soda). Chapter XIV. Chlorometry Titration Wagner's Chlorometric Method Prepara-
tion of Standard Solutions Apparatus for Chlorine Valuation Alkali in Excess in De-
colourising Chlorides. Chapter XV. Chlorine and Decolourising Chlorides Synopsis
Chlorine Chloride of Lime Hypochlorite of Soda Brochoki's Chlorozone Various De-
colourising Hypochlorites Comparison of Chloride of Lime and Hypochlorite of Soda.
Chapter XVI. Water Qualities of Water Hardness Dervaux's Purifier Testing the
Purified Water Different Plant for Purification Filters. Chapter XVII. Bleaching of
Yarn Weight of Yarn Lye Boiling Chemicking Washing Bleaching of Cotton Yarn.
Chapter XVI 1 1. The Installation of a Bleach Works -Water Supply-Steam Boilers-Steam
Distribution Pipes Engines Keirs Washing Machines Stocks Wash Wheels Chemick-
ing and Souring Cisterns Various Buildings. Chapter XIX. Addenda Energy of De-
colourising Chlorides and Bleaching by Electricity and Ozone Energy of Decolourising
Chlorides-ChloridesProduction of Chlorine and Hypochlorites by Electrolysis Lunge's
Process for increasing the intensity of the Bleaching Power of Chloride of Lime Trilfer's
Process for Removing the Excess of Lime or Soda from Decolourising Chlorides Bleaching
by Ozone.
THE SCIENCE OF COLOUR MIXING. A Manual in-

tended for the use of Dyers, Calico Printers and Colour Chemists. By
DAVID PATERSOX, F.C.S. Forty-one Illustrations, Five Coloured Plates,
and Four Plates showing Eleven Dyed Specimens of Fabrics. 1900.
Price 7s. 6d. India and Colonies, 8s.
;
Other Countries, 8s. 6d.
; ;

Contents.
Chapters I., Colour a Sensation; Colours of Illuminated Bodies; Colours of Opaque and
Transparent Bodies; Surface Colour. II., Analysis of Light; Spectrum; Homogeneous
Colours; Ready Method of Obtaining a Spectrum. III., Examination of Solar Spectrum;
The Spectroscope and Its Construction Colourists' Use of the Spectroscope. IV.. Colour by
;
Absorption Solutions and Dyed Fabrics; Dichroic Coloured Fabrics in Gaslight. V., Colour
;
Primaries of the Scientist versus the Dyer and Artist Colour Mixing by Rotation and Lye
;
Dyeing: Hue, Purity, Brightness; Tints; Shades, Scales, Tones, Sad and Sombre Colours.
VI., Colour Mixing; Pure and Impure Greens, Orange and Violets; Large Variety of Shades
from few Colours; Consideration of the Practical Primaries: Red, Yellow and Blue. VII.,
Secondary Colours; Nomenclature of Violet and Purple Group; Tints and Shades of Violet;
Changes in Artificial Light. VIII., Tertiary Shades Broken Hues: Absorption Spectra of
;
Tertiary Shades. Appendix Four Plates with Dyed Specimens Illustrating Text. Index.
:
Press Opinions.
"The work has evidently been prepared with great care, and, as far as we can judge, should
be very useful to the dyer and colourist." Halifax Courier.
"The volume, which is clearly and popularly written, should prove of the utmost service to
all who are concerned with the practical use of colours, whether as dyers or painters."
Scotsman.
"To the practical colourist, and also to technical students, Mr. Paterson's new work will be
very welcome We are often asked to recommend books on different subjects, and have no
hesitation in advising the purchase of the present volume by dyers and calico printers, as con-
taining a mass of most useful information at a nominal price." Irish Textile Journal.
"
.Mr. Paterson's work not only clearly deals with the theory of colour, but supplies lucid
directions for the practical application of the theory. His work will be found exceedingly
helpful, not only to the practical colourist, but also to students in our textile colleges, by
forming a useful complement to their class lectures. There are several exquisitely coloured
plates and a large number of other illustrations of theory and'practice in colour blending, and
also a series of plates with specimens of dyed fabrics attached, in explication of the author's
views." WakefielA Express.
"
Mr. Paterson has little to say upon the experimental aspect or on its aesthetics, but much
upon the theory of colour, especially as it bears upon the question an all-important one to
dyers, calico printers and artists, who have to produce such a variety of shades and tints of
the admixture of one colour upon another. . . The author is a dyer, and in his concluding
.
chapters keeps well before him the special wants and requirements of dyers. He writes
pleasantly and lucidly, and there is no difficulty in following him, although here ami there a
lapse into ambiguousness occurs. The book is well printed, generously supplied with coloured
plates, very nicely if not brightly got up; and the dyed patterns at the end enhance the value
of the book to the dyer." Textile Mercury.
"For some time the proprietors of The Oil and Colourman's Journal have been engaged in
the publication of a series of practical handbooks intended for the use of those interested in
certain branches of technology, and the present volume is the latest addition to their list.
The feature which the works have in common and it is an all-important one in treatises of
this sort is their eminently practical character. The primary aim of the publishers is to
provide scientific text-books which will be helpful to those who are either actively engaged in
28
the practice of the arts in question, or who are studying with that immediate end in view. . .
Mr. Paterson speaks with that assured knowledge of an expert, and in the present volume, as
in that which he has already contributed to the same series, he sets forth the true foundation
of the art of colouring in a manner at once comprehensive and judicious. . . For dyers,
.
calico printers and cofourists in general, whose desire it is to work with accuracy in their
respective branches, the treatise will prove an invaluable guide-book, provided the principles
and methods it describes are studied with intelligence and care. To this end, every encourage-
ment has been given that well-chosen examples, carefully executed plates and diagrams, and
an exhaustive index can supply." Glasgow Herald.
COLOUR MATCHING ON TEXTILES. A Manual in-

tended for the use of Students of Colour Chemistry, Dyeing and
Textile Printing. By DAVID PATERSON, F.C.S. Coloured Frontis-
piece. Twenty-eight Illustrations and Fifteen Specimens of Dyed
Fabrics Illustrating Text. [/;.-
the Press.
Contents.
Chapters I., Colour Vision and Structure of the Eye Perception of Colour Primary
and Complementary Colour Sensations. II., Daylight for Colour Matching Selection of a
Good Pure Light Diffused Daylight, Direct Sunlight, Blue Skylight, Variability of Daylight,
etc., etc. III., Matching of Hues Purity and Luminosity of Colours Matching Bright Hues
Aid of Tinted Films Matching Difficulties Arising from Contrast. IV., Examination of
Colours by Reflected and Transmitted Lights Effect of Lustre and Transparency of Fibres
4n Colour Matching. V., Matching of Colours on Velvet Pile Optical Properties of Dye-
stuffs, Dichroism, Fluorescence. VI., Use of Tinted Mediums Orange Film Defects of the
Eye Yellowing of the Lens Colour Blindness, etc. VII., Matching of Dyed Silk Trimmings
and Linings and Bindings Its Difficulties Behaviour of Shades in Artificial Light Colour
Matching of Old Fabrics, etc. VIII., Examination of Dyed Colours under the Artificial Lights
Electric Arc, Magnesium and Dufton, Gardner Lights, Welsbach, Acetylene, etc. Testing
Qualities of an Illuminant. IX., Influence of the Absorption Spectrum in Changes of Hue
under the Artificial Lights Study of the Causes of Abnormal Modifications of Hue, etc.
THE DYEING OF COTTON FABRICS: A Practical

Handbook for the Dyer and Student. By FRANKLIN BEECH. Forty-
four Illustrations. [In the Press.
Contents.
Chapters I., Structure and Chemistry of the Cotton Fibre. II., Scouring and Bleaching of
Cotton. III., Dyeing Machinery and Dyeing Manipulations. IV., Principals and Practice of
Cotton Dyeing 1, Direct Dyeing; 2, Direct Dyeing followed by Fixation with Metallic Salts;
3, Direct Dyeing followed by Fixation with Developers; 4, Direct Dyeing followed by Fixation
with Couplers 5, Dyeing on Tannic Mordant 6, Dyeing on Metallic Mordant 7, Production
; ; ;
of Colour Direct upon Cotton Fibres 8 Dyeing Cotton by Impregnation with Dye-stuff Solu-
;
tion. V.. Dyeing Union (Mixed Cotton and Wool) Fabrics. VI., Dyeing Half Silk (Cotton-
Silk, Satin) Fabrics. VII., Operations following Dyeing Washing, Soaping, Drying. VIII.,
Testing of the Colour of Dyed Fabrics. IX., Experimental Dyeing and Comparative Dye
Testing. Index.
Books for Mining Engineers

and Steam Users.
BECOVERY WORK AFTER PIT FIRES. A Description
of the Principal Methods Pursued, especially in Fiery Mines, and of
the Various Appliances Employed, such as Respiratory and Rescue
Apparatus, Dams, etc. By ROBERT LAMPRECHT, Mining Engineer and
Manager. Translated from the German. Illustrated by Six large
Plates, containing Seventy-six Illustrations. 175 pp., demy 8vo. 1901.
Price 10s. 6d. India and Colonies, 11s.; Other Countries, 12s.;
;

Contents.
Preface. I., Causes of Pit Fires: 1, Fires Resulting from the Spontaneous Ignition of
Coal: 2, Fires Caused by Burning Timber; 3, Fires Caused by Fire-damp Explosions. II.,
Preventive Regulations: 1, The Outbreak and Rapid Extension of a Shaft Fire can be
most reliably prevented by Employing little or no Combustible Material in the Construction of
the Shaft 2, Precautions for Rapidly Localising an Outbreak of Fire in the Shaft 3, Pre-
; ;
29
cautions to be Adopted in case those under 1 and 2 Fail or Prove Inefficient Precautions
against Spontaneous Ignition of Coal. Precautions for Preventing Explosions of Fire-damp
and Coal Dust. Employment of Electricity in Mining, particularly in Fiery Pits. Experiments
on the Ignition of Fire-damp Mixtures and Clouds of Coal Dust by Electricity. III., Indica-
tions of an Existing or Incipient Fire. IV., Appliances for Working in Irrespirable
Gases 1, Respiratory Apparatus: 2, Apparatus with Air Supply Pipes, (a) The Bremen Smoke
:
Helmet, (b) The Muller Smoke Helmet, (c) The Stolz Rescue Mask; 3, Reservoir Apparatus;
4, Oxygen Apparatus. The Schwann Respiratory Apparatus. The Fleuss Respiratory Ap-
paratus. The Improved Walcher-Giirtner Pneumatophor, (a) The Single Bottle Apparatus,
Instructions for Using the Pneumatophor, Taking to Pieces and Resetting the Apparatus
ready for Use (b) Two Bottle Apparatus (Shamrock Type). The .Neupert Rescue Apparatus
;
(The Mayer-Pilar System). V. Extinguishing Pit Fires: (a)[Chemical Means; (b) Extinction
with Water. Dragging down the Burning Masses and Packing with Clay; (c) Insulating the
Seat of the Fire by Dams. Dam Building. Dam Work in the Fiery Pits of Southern Hungary :
(a) Cross-dams of Clay; (6) Masonry Dams, Gallery Linings. Wagner's Portable Safety Dam.
Analyses of Fire Gases. Isolating the Seat of a Fire with Dams: Working in Irrespirable
Gases ("Gas-diving ") 1, Air-Lock Work (Horizontal Advance) on the Mayer System as Pur-
:
sued at Karwin in 1894 2, Air-Lock Work (Horizontal Advance) by the Mauerhofer Modified
;
System. Vertical Advance. Mayer System. Completee Isolation of the Pit. Floodin: Flooding
Burning Section isolated by means of Dams. Wooden Dams: (a) Upright Balk Dams; (6>
Horizontal Balk Dams (c) Wedge Dams, Masonry;
iry Dams. Examples of Cylindrical and Do
Dome-
shaped Dams. Dam Doors: Flooding the Whole Pit. VI., Rescue Stations: (a) Stations
above Ground; (b) Underground Rescue Stations. VII., Spontaneous Ignition of Coal in
Bulk. Index.
Illustrations.
Sheet Respiratory and Rescue Appliances Precautions against Fire. Figs. 1,
I.,
Smoke Hlmet 2, Miiller's Smoke Helmet; 3, Low-pressure Respiration Apparatus: 4, High-
;
pressure Respiration Apparatus 5, The Stolz Mask for Rescue Work 6, Precautions against
; ;
Fire. Sheet II., Respiratory and Rescue Apparatus. Figs. 1, Recovery Work with
Miiller's Smoke Helmet after a Fire; 2-8, The Fleuss Respiration Apparatus: 9, The Walcher-
Gartner Pneumatophor: 10-12, Pneumatophor (Shamrock Type). Sheet III., Respiratory
and Rescue Apparatus Stretchers. Figs. 1-8, Rescue Apparatus manufactured by O.
Neupert 's Successor (Mayer-Pilar System) 1, Front View 2, Section through Bag and Mask
; ; ;
3, Rear View 4, Apparatus and Mask laid out Flat (view from above)
; 5, Apparatus and Mask
;
laid out Flat (view from below); 6, Locking Device for Closing Bag: 7, Apparatus Complete,
Mounted for Rescue Work; 8, Improved Valve in the Respiration Tubes; 9-12, Stretchers.
Fig. 9, Stretcher Covered with Brown Canvas 10, Stretcher Covered with Brown Canvas,
:
fitted with Adjustable Head-rest: 11, Folding Stretcher Covered with Brown Canvas: 12,
Rupprecht's Stretcher Covered with Brown Canvas 13, Dr. Riihlmann's Stretcher. Sheet
:
IV., Dams. Figs. 1-7, R. Wagner's Portable Safety Dam. Sheet V., Signalling Appliances
Dam Construction Cable Laying. Figs. 1-3, Signalling Appliances: 1, Small Induction
Apparatus for Pit Work; 2, Bell Signal for Pit Work; 3, Pit Telephone; 4-18, Dam Con-
struction; 4, 5, Upright Timber Dam: 6, 7, Timber Dam with Wooden Door: 8, 9, Dome-
shaped Dams; 10, 11, Dome-shaped Dam with Iron Door; 12, 13, The Wenker and Berninghaus
Locking Device for Dam Doors; 14-17, Dam Construction; 18, Damming a Gallery Lined with
Iron 19, Support for Cable. Sheet VI., Working with Diving Gear in Irrespirable Gases
;
Gallery Work. Figs. 1-4, Air-Lock Work (Mayer System): 5-7. Air-Lock (Mauerhofer's
Modification of the Mayer System); 8-11, Construction of Dams at the Pluto Shaft. Sheet
VII., Working with Diving Gear in Irrespirable Gases (Mayer System) Appliances in
the Shaft. Figs. 1, 2, Sections of Shaft and Air Apparatus; 3, Salzmann Reducing Valve for
Reserve Air Supply 4, 5, L. v. Bremen's Respiration Apparatus with Karwin Reserve Ap-
:
pliance 6, Cross Section of the Franziska Shaft; 7, Method of Supplying Air to Main Pipe
;
and Winding same on Drum 8, Clamp. ;
Press Opinions.
"This book is, in a manner, unique. The literature of mining accidents is fairly extensive,
but consists largely of departmental Blue Books." Sheffield Daily Telegraph.
it
"A concise and lucid description of the principal methods pursued, especially in fiery
mines, and of the various appliances employed, such as respiratory and rescue apparatus,
dams, etc." Staffs Advertiser.
"The prevention of spontaneous combustion in collieries and the extinction of underground
fires are duties that fall heavily on many colliery managers. They should, therefore, welcome
this translation of Mr. Lamprecht's German treatise." Ironmonger.
"The book under notice supplies the needed full description, drawings, and mode of using
these new appliances in actual fires, and should be studied by every colliery manager, seeing
that even our best managed collieries have not been free from fires, more or less disastrous
to life and property. Colliery .Manager.
" Herr
Lamprecht has collated such a vast mass of useful information that it can never
fail to be of utility to the mine manager, even though, on occasion, it should only be in the
direction of inducing measures to prevent a recurrence of similar calamities." Xcvcastle
Chronicle.
" It is the
only existing work which deals exclusively with the branch of the miner's art
indicated by its title. . The author presents his subject in a clear, practical manner, and
. .
seems to leave nothing unexplained that is necessary to make the book a thoroughly useful
and easily assimilated authority, on which pit managers and others may rely for guidance
in case of catastrophe." Wigan Examiner.
30
GAS AND COAL DUST FIRING. A Critical Review of

the Various Appliances Patented in Germany for this purpose since
1885. By ALBERT PUTSCH. 130 pp., demy 8vo. 1901. Translated
from the German. With 103 Illustrations. Price 7s. 6d. India and :
Colonies, 8s. Other Countries, 8s. 6d. strictly net, post free.
; ;
Contents.
Generators Generators Employing Steam Stirring and Feed Regulating Appliances
Direct Generators Burners Regenerators and Recuperators Glass Smelting Furnaces
Metallurgical Furnaces Pottery Furnace Coal Dust Firing.
Press Opinions.
" The work is worthy of perusal by all consumers of fuel. It is exceedingly well printed
and illustrated. "Chemical Trade Journal.
"
The hook will appeal with force to the manufacturer as well as to the technical student,
whilst also of far more than average interest to the general reader." Halifax Guardian.
it is
"The importance that gas and coal dust firing have attained of recent years, and especially
the great interest attaching of late to the question of coal dust firing, makes the appearance
of the present volume most opportune." Iron and Coal Trades Review.
"The German author has long followed the development of various systems of gas firing,
and in the present treatise he discusses the merits of appliances patented since 1885. His text
and the numerous illustrations indispensable to it will be found useful by all who are engaged
in practical work in the same field." North British Daily Mail.
" It has been a
pleasure to read this little book, and though the author has to admit on the
last page that no important novel ideas have appeared of late in connection with the subject
'
of gas firing,' one feels that the translation has not been made in vain. The volume forms . . .
a useful aid to the would-be inventor of generators, as it warns him what to avoid and gives
some hints as to what to aim at." Gas World.
Books on Plumbing, Decorating,

Metal Work, etc., etc.
EXTERNAL PLUMBING WORK. A Treatise on Lead
\York for Roofs. By JOHN W. HART, R.P.C. 180 Illustrations. 270
pp. 1896. Price 7s. 6d. ;
India and Colonies, 8s. ; Other Countries,
8s. 6d.; strictly net, post free.
Contents.
Chapters I., Cast Sheet Lead. II., Milled Sheet Lead. III., Root Cesspools. IV., Socket
Pipes. V., Drips. VI., Gutters. VII., Gutters (continued). VIII., Breaks. IX., Circular
Breaks. X., Flats. XI., Flats (continued). XII., Rolls on Flats. XIII., Roll Ends. XIV.,
Roll Intersections.-XV., Seam Rolls. XVI., Seam Rolls (continued).-XVII., Tack Fixings.
XVIII., Step Flashings. XIX., Step Flashings (continued). XX., Secret Gutters.-XXI.,
Soakers. XXII., Hip and Valley Soakers. XXIII., Dormer Windows. XXIV., Dormer
Windows (continued). XXV., Dormer Tops. XXVI., Internal Dormers. XXVII., Skylights.
XXVIII., Hips and Ridging.-XXIX., Hips and Ridging (continued).-XXX., Fixings for
Hips and Ridging. XXXI., Ornamental Ridging. XXXI I., Ornamental Curb Rolls. XXXIII.,
Curb Rolls. XXXIV., Cornices. XXXV., Towers and Finials. XXXVI., Towers and Finials
(continued).-XXXVII.,Towersand Finials(continued).-XXXVIII., Domes.-XXXIX., Domes
(continued). XL., Ornamental Lead Work. XLI., Rain Water Heads. XLII., Rain Water
Heads (continued). XLIII., Rain Water Heads (continued).
Press Opinions.
"This is an eminently practical and well-illustrated volume on the management of external
ead work." Birmingham Daily Post.
It is thoroughly practical, containing many valuable hints, and cannot fail to be of great
''
benefit to those who have not had large experience." Sanitary Journal.
"Works on sanitary plumbing are by no means rare, but treatises dealing with external
plumbing work are sufficiently scarce to ensure for Mr. Hart's new publication a hearty recep-
tion.''?^ Ironmonger.
"With Mr. Hart's treatise in his hands the young plumber need not be afraid of tackling
outside work. He would do well to study its pages at leisure, so that he may be ready for it
when called upon." Ironmongery.
"The publication of this book will do much to stimulate attention and study to external
plumbing work, for it is a book which we can heartily recommend to every plumber, both old
and young, who desires to make himself proficient in the several branches of his trade We
can heartily recommend the book to plumbers and architects." Sanitary Record.
31
HINTS TO PLUMBERS ON JOINT WIPING, PIPE

BENDING AND LEAD BURNING. Third Edition,
Revised and Corrected. By JOHN W. HART, R.P.C. 184 Illustrations.
313 pp. 1901. Price 7s. 6d. India and Colonies, 8s.
; ;
Other Countries,
8s. 6d.;strictly net, post free.
Contents.
Introduction. Chapters I., Pipe Bending. II., Pipe Bending (continued). III., Pipe
Bending (continued). IV., Square Pipe Bendings. V., Half-circular Elbows. VI., Curved
Bends on Square Pipe. VII., Bossed Bends. VIII., Curved Plinth Bends. IX., Rain-water
Shoes on Square Pipe. X., Curved and Angle Bends. XI., Square Pipe Fixings. XII., Joint-
wiping. XIII., Substitutes for Wiped Joints. XIV., Preparing Wiped Joints. XV., Joint
Join Fixings. XVIII., Use of "Touch" in Solder-
Fixings. XVI., Plumbing Irons. XVII., Joint
.
ing. XIX., Underhand Joints. XX., Blownn and Copper Bit Joints. XXI., Branch Joints.
XXII., Branch Joints (continued). XXIII., Block Joints. XXIV., Block Joints (continued).
,
XXV., Block Fixings. XXVI., Astragal Joints Pipe Fixings. I., -XXVI
Large Branch
Joints.-XXVIII., Large Underhand Joints. XXIX., Solders. XXX., Autogenous Soldering
or Lead Burning. Index.
Press Opinions.
" Rich in useful diagrams as well as in hints." Liverpool Mercury.
"The papers are eminently practical, and go much farther into the mysteries they describe
than the title Hints' properly suggests." Scotsman.
'
" The articles are

apparently written by a thoroughly practical man. As a practical guide
the book will doubtless be of much service." Glasgow Herald.
" A well
got-up and well-done practical book. It is freely illustrated and is a reliable help in
respect of some of the most awkward work the young plumber has to perform." The Iron-
monger.
" So far as the
practical hints in this work are concerned.it will be useful to apprentices and
students in technical schools, as it deals mainly with the most important or difficult branches
of the plumber's craft, viz., joint wiping, pipe bending and lead burning. 'Hints' are the
. . .
most useful things to an apprentice, and there are many in this work which are not to be found
in some of the text-books." English Mechanic.
" It is a book for the
intelligent operative first of all, not a mere manual of instruction for
the beginner, nor yet a scientific treatise on the whole art of sanitary plumbing. The special
subject with which it deals is joint-making, the most important branch of the operative's work,
and into this topic the author goes with a thoroughness that is full of suggestion to even the
most experienced workman. There is no one who has to do with plumbing but could read the
book with profit." Ironmongery.
"22 PRYME STREET, HULL, 24th November, 1894.
"
Gentlemen, Your books to hand for which accept my best thanks, also for circulars. I
myself got one of J. W. Hart's books on Plumbing from your traveller, and having looked
through the same I can safely recommend it as being the best book 1 have seen. .Mr. J. W.
Hart treats exhaustively upon soldering and pipe bending, which are two of the most essential
branches in the plumbing trade."
THE PRINCIPLES AND PRACTICE OF DIPPING,

BURNISHING, LACQUERING AND BRONZING
BRASS WARE. By W. NORMAN BROWN. 35 pp. 1900.
Price 2s. ; Abroad, 2s. 6d. ;
Contents.
Chapters I., Cleansing and Dipping; Boiling up and Cleansing; Dipping. II., Scratch-
ushing and Burnishing; Polishing; Burnishing. III., Lacquering; Tools; Lacquers.
brush
IV ., Bronzing; Black Bronzing; Florentine Red Bronzing; Green Bronzing. Index.
Press Opinions.
" Mr. Brown is
clearly a master of his craft, and has also the immense advantage
of being
able to convey his instructions in a manner at once clear and concise." Leicester Post.
"A thoroughly practical little treatise on the subject in all its branches, and one which
should be in the hands of every tradesman or amateur who has lacquering to do." Irish Builder.
"A successful endeavour has been made to show in the course of four chapters of compara-
tively few words the most scientific and economical methods
of treating brass ware. The . . .
book is prefaced with a contents list, and concludes with a complete index. It is substantially
bound, and should prove invaluable to gasfitters, decorators and ironmongers in country
towns, who at spring time and during the redecorating of a house undertake the work of
renovating the brass fittings." H cirdii'cireman.
32
HOUSE DECORATING AND PAINTING. By W.

NORMAN BROWN. Eighty-eight Illustrations. 150 pp. 1900. Price
3s. 6d. ; Indiaând Colonies, 4s. Other Countries, 4s. 6d.
; ;
strictly net,
post free.
Contents.
Chapters I., Tools and Appliances. II., Colours and Their Harmony. III., Pigments and
Media. IV., Pigments and Media. V., Pigments and Media. VI., Pigments and Media.
VII., Preparation of Work, etc. VIII., Application of Ordinary Colour. IX., Graining.
X., Graining. XI., Graining. XII., Gilding. XIII., Writing and Lettering. XIV., Sign
Painting. XV., Internal Decoration. Index.
Press Opinion.
"The author is evidently very thoroughly at home in regard to the technical subjects he has
set himself to elucidate, from the mechanical rather than the artistic point of view, although
the matter of correctness of taste is by no means ignored. Mr. Brown's style is directness
itself, and there is no tyro in the painting trade, however mentally ungifted, who could fail to
carry away a clearer grasp of the details of the subject after going over the performance."
Building Industries.
A HISTORY OF DECORATIVE ART. By W. NORMAN

BROWN. Thirty-nine Illustrations. 96 pp. 1900. Price 2s. 6d. ;
Abroad, 3s. ; strictly net, post free.
Contents.
Chapters I., Primitive and Premstoric Art. II., Egyptian Art. III.,' Assyrian Art. IV.,
The Art of Asia Minor. V., Etruscan Art. VI., Greek Art. VII., Roman Art.-VIIL,
Byzantine Art. IX., Lombard or Romanesque Art. X., Gothic Art. XI., Renaissance Art.
XII., The Victorian Period. Index.
Press Opinion.
"In the course of a hundred pages with some forty illustrations Mr. Brown gives a very
interesting and comprehensive survey of the progress and development of decorative art. It
cannot, of course, be pretended that in the limited space named the subject is treated ex-
haustively and in full detail, but it is sufficiently complete to satisfy any ordinary reader ;
indeed, for general purposes, it is, perhaps, more acceptable than a more elaborate treatise."
Midland Counties Herald.:
THE PRINCIPLES OF HOT WATER SUPPLY. By

JOHN W. HART, R.P.C. With 129 Illustrations. 1900. 177 pp., demy
8vo. Price 7s. 6d. ;
India and Colonies, 8s. Other Countries, 8s. 6d.
; ;
Contents.
Chapters I., Water Circulation.--!!., The Tank System. III., Pipes and Joints. IV., The
Cylinder System. V., Boilers for the Cylinder System. VI., The Cylinder System. VII., The
Combined Tank and Cylinder System. VIII., Combined Independent and Kitchen Boiler.
IX., Combined Cylinder and Tank System with Duplicate Boilers. X., Indirect Heating and
Boiler Explosions. XL, Pipe Boilers. XII., Safety Valves. XIII., Safety Valves. XIV., The
American System. XV., Heating Water by Steam. XVI., Steam Kettles'and Jets. XVII.,
Heating Power of Steam. XVIII., Covering for Hot Water Pipes. Index.
iPress Opinion.
j" If all plumbers were to read this book, and if they followed the instructions given, there
would, we are sure, be fewer accidents from household boiler explosions, and many lives might
be saved. No doubt the majority of householders know or care little about the subject, but
any one who wishes to adopt the most up-to-date system of supplying hot water throughout
his house will be able to do so if he reads Mr. Harfs book and follows the instruction given.
It is a work that all who have charge of domestic water supply should study. It is a practical
and profitable book." Wigav Observer.
33
Brewing and Botanical.

HOPS IN THEIR BOTANICAL, AGRICULTURAL
AND TECHNICAL ASPECT, AND AS AN ARTICLE
OF COMMERCE. By EMMANUEL GROSS, Professor at
the Higher Agricultural College, Tetschen-Liebwerd. Translated
from the German. Seventy-eight Illustrations. 1900. 340 pp Price
12s. 6d. India and Colonies, 13s. 6d. Other Countries, 15s. ;^strictly
; ;
net, post free.
Contents.
PART I., HISTORY OF THE HOP.
PART II., THE HOP PLANT. Introductory. The RootSr The Stem and Leaves.
Inflorescence and Flower: Inflorescence and Flower of the Male Hop; Inflorescence an-4
Flower of the Female Hop. The Fruit and its Glandular Structure The Fruit and Seed. :
Propagation and Selection of the Hop. Varieties of the Hop (a) Red Hops (6) Green Hops
:
; ;
ic) Pale Green Hops. Classification according to the Period of Ripening: 1. Early August
Hops; 2. Medium Early Hops: 3. Late Hops. Injuries to Growth Malformations; Diseases
:
Produced by Conditions of Soil and Climate: 1. Leaves Turning Yellow, 2. Summer or Sun-
brand, 3. Cones Dropping Off, 4. Honey Dew, 5. Damage from Wind, Hail and Ram Vegetable ;
Enemies of the Hop: Animal Enemies of the Hop. Beneficial Insects on Hops.
PART III., CULTIVATION. The Requirements of .the Hop in Respect of Climate, Soil
and Situation Climate; Soil: Situation. Selection of Variety and Cuttings. Planting a Hop
:
Garden: Drainage; Preparing the Ground; Marking-out for Planting; Planting; Cultivation
and Cropping of the Hop Garden in the First Year. Work to be Performed Annually in the
Hop Garden: Working the Ground; Cutting; The Non-cutting System; The Proper Per-
formance of the Operation of Cutting I. Method of Cutting Close Cutting, Ordinary Cutting,
: :
The Long Cut, The Topping Cut: II. Proper Season for Cutting: Autumn Cutting, Spring
Cutting: Manuring: Training the Hop Plant: Poled Gardens, Frame Training; Principal
Types of Frames Pruning, Cropping, Topping, and Leaf Stripping the Hop Plant Picking,
: ;
Drying and Bagging. Principal and Subsidiary Utilisation of Hops and Hop Gardens. Life
of a Hop Garden Subsequent Cropping. Cost of Production, Yield and Selling Prices.
:
PART IV. Preservation and Storage. Physical and Chemical Structure of the Hop Cone.
Judging the Value of Hops.
PART V. Statistics of Production. The Hop Trade. Index.
PressÔpinions.
"The subject is dealt with fully in every little detail consequently, even the veriest tyro can
;
take
"
away some useful information from its pages." Irish Farming World.
Farmers are but little given to reading but nowadays brewers have to study their trade
;
and keep abreast of its every aspect, and as far as regards our trade, to them this book
especially appeals, and will be especially useful." Licensed Victuallers' Gazette.
" Like an oasis in the desert comes a volume
upon the above subject, by the Professor at
the Higher Agricultural College, Tetschen-Liebwerd, Germany, who has been fortunate
enough to obtain an excellent translator from the German in the person of Mr. Charles
Salter. The paucity of works upon the history and cultivation of hops is surprising con-
sidering the scope it gives for an interesting and useful work." Hereford Times.
"We can safely say that this book deals more comprehensively and thoroughly with the
subject of hops than any work previously published in this country. No one interested in
. . .
the hop industry can fail to extract a large amount of information from Professor Gross's
pages, which, although primarily intended for Continental readers, yet bear very closely on
what may be termed the cosmopolitan aspects of the science of hop production." South
Eastern Gazette.
"This is, in our opinion, the most scholarly and exhaustive treatise on the subject of hops,
their culture and preservation, etc., that has been published, and to the hop grower especially
will its information and recommendations prove valuable. Brewers, too, will find the chapter
'
devoted to Judging the Value of Hops full of useful hints, while the whole scope and tenor of
'
the book bear testimony to the studious and careful manner in which its contents have been
elaborated." Brewers' Journal.
[See next Page.
34
"Considering the extent to which this country draws its hop supplies from abroad, this
translation of -Professor Gross's volume will prove an interesting and instructive addition to
the library of any brewer or brewers' chemist, the more so as the work of translation has been
admirably carried out in simple and vigorous English. . The volume is one of a valuable
. .
series of special technical works for trades and professions the publishers are issuing, and is
the first so far dealing with the brewing industry." Burton .Mail.
" A work
upon the above subject must be welcomed if for no other reason than the dearth
of books dealing with so interesting a theme, but fortunately apart from this the book will
afford excellent reading to all interested in hops and their culture. Professor Gross takes one
over the whole field, by commencing with the earliest history of the plant so far back as the
days of ancient Greece and from both practical, theoretical and scientific standpoints, deals
with the cultivation, classification and formation of the hop. ... In speaking of the produc-
tion of new varieties sound information is given, and should be of value to those who are
always in search of improvements." Hereford Journal.
"This work is, without doubt, the most thorough and extensive compilation on hops ever
yet offered to the public, and for this reason should be warmly welcomed and appreciated by
men interested in the subject. Although primarily written for those engaged in the industry
abroad, and mainly Continental in theory and practice, it nevertheless appeals to those con-
nected with the hop growing and brewing business in England, not only by way of a com-
parison, but also as an instruction. The volume is at once practical and scientific, is well
got up, and teems with illustrations and statistics. In a word, it is a book that should find
its way into the hands of all who are occupied in hop production and distribution at home ;
and it also contains valuable information and suggestions for the brewers themselves."
Brewers' Guardian.
"The value of a comprehensible and reliable text-book must be clearly apparent to every
scientific hop grower, and in this county of Kent the chief hop-producing district of England,
for over 400,000 cwts. were grown here last season alone its advice regarding the cultivation,
preservation and storage of the cones will be found extremely useful. Year by year scientific
education is becoming more and more essential to the training in common with the re-
mainder of agriculturalists of the hop planter. Continental and American competition, the
higher price and scarcity of hand labour and many other causes make it necessary that the
utmost should be extracted from a limited area of land. To accomplish this end all sorts of
devices must be resorted to in the matter of cultivation. The lesson imparted in this treatise
deals exhaustively with these devices '. And therein lies the basis of its value whereas one
'
:
man's life is 'made up of fails and successes,' here is to be found the collective successes,
tabulated results and logical inferences drawn from sources extending over the whole hop-
growing area of the world." Kentish Gazette.
Public Libraries.
BRITISH LIBRARY YEAR BOOK, 1900-1901. A Record
of Library Progress and Work. 54 Illustrations. Crown 8vo, 345 pp.
1900. Edited by THOMAS GREENWOOD. Price 3s. abroad, 3s. 6d.
; ;
Contents.
Notes for Library Committees. Contributed Articles The Library Rate. Some Points in
:
Library Planning Mr. Burgoyne. Library Classification Mr. Jast. Developments in Lib-
rary Cataloguing Mr. Quinn. Children and Public Libraries Mr. Ballinger. Fire Prevention
and Insurance Mr. Davis. The Educational Work of the Library Association Mr. Roberts.
The Library Assistants' Association Mr. Chambers. British .Municipal Libraries established
under the various Public Libraries or Special Acts, and those supported out of Municipal Funds,
giving particulars of Establishment, Organisation, Staff, Methods and Librarians. Table
showing the Rate, Income, Work and Hours of the Rate-supported Libraries. Statistical
Abstracts. British non-Municipal Libraries, Endowed, Collegiate, Proprietary and others,
showing date of Establishment, number of Volumes, Particula/s of Administration, and Lib-
rarians. Library Associations and Kindred Societies.
Press Opinions.
"The book promises to be a really useful compendium of information which ought to be of
importance to everybody." Athentriitn.
" This valuable reference book is in every respect what a year book should be. ... The
production of the volume is excellent." \eu'sagent. Bookseller and Stationer.
"This is a handbook which tells the reader everything about public libraries, great and
small, in the United Kingdom. . The book is decidedly one of the best arranged volumes ever
. .
published, and there is no doubt that the editor has been at great pains to obtain the latest
and most accurate information from all places. County, district and parish councils,
ministers of religion, and schoolmasters everywhere should make themselves acquainted with
its contents. Its perusal cannot fail to serve the ends of the library movement. The illustra-
tions, of which there is a large number, are very good." Western (Cardiff) Mail.
35
WORKS IN PREPARATION.
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TREATISE ON CLOTH FINISHING. By ROBERT

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THE EXAMINATION OF MATERIALS USED IN DYE-
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EVAPORATION, CONDENSATION AND COOLING.
Calculations of Dimensions of Apparatus. By E. HAUSBRAND.
Tables. For Chemists, Chemical and Mechanical Engineers.
THE CHEMISTRY OF SPINNING. Spinning, Washing,

Bleaching, Dyeing, Printing and Finishing. By Dr. G. VON
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EMILLE BOURRY. Translated and Edited by WILTON P. Rix, Ceramic
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THE LIBRARY

OTHER SALTS OF ALUMINA AND IRON

ie Publishers wish it to be distinctly understood that

i5 series of books is supplied on such terms as prohibit

WITH 195 ILLV

D. VAN NOSTRAND COMPANY.

TRANSLATED FROM THE FRENCH BY CHAS. SALTER

WITH 195 ILLUSTRATIONS

D. VAN NQSTRAND COMPANY,

IN compiling the present work, the author has endeavoured to

facture of the sulphates of alumina and iron, and- combine with

1. A Theoretical Study of Iron, Aluminium, and their Com-

seeking for information on theoretical points connected with

practical procedure ; and, furthermore, simplifies the subsequent

composition and origin of the minerals, the reactions employed,

facturing aluminium sulphate, the various alums, normal ferrous

or lent by the proprietors of the works described.

4. The Analysis of the Iron and Aluminium Compounds: this

part containing, in addition to the usual tests, examples of the

engaged in the various chemical industries producing or using

THEORETICAL STUDY OF ALUMINIUM, IRON, AND COMPOUNDS OF

MANUFACTURE OF ALUMINIUM SULPHATE AND SULPHATES OF IRON

MANUFACTURE OF ALUMINIUM SULPHATE AND THE ALUMS

Conjoint Manufacture of Ferrous Sulphate and

. Treatment of Pyritic Lignites 193

USES OF THE SULPHATES OF ALUMINIUM AND IRON

1. Application to the Art of Dyeing .

2. Employment in the Manufacture of Pigments 290

USES AND APPLICATIONS OF FERROUS SULPHATE AND FERRIC SULPHATES

27 and 28. Albite crystals

361038. Ferro-ferric oxide crystals . . . .

54 to 57. Crystals of pyrites

7 5 and 76. Peridot . .128

84 to 86. Almandin garnet . .

93. Reverberatory evaporator used in aluminium sulphate manufacture Cross

98. Grinding mill . .146

101. Collector ...

102 and 103. Rectangular vat in plan and longitudinal section

105. Concentrating the liquor

111. Reverberatory furnace for roasting alunite

114. Preparing the mineral

119. Transverse sections

133 and 134. Details of wooden pump . . . . ... 221

137. Plan of the washing tank (turbine) 223

(a) collected .....

Alum washing and draining tank

150. Alum re-crystallising plant . . .

165 and 166. Soldered lapped butt joint in leaden sheets . . .

175. ,, ,, ,, inaccessible from the back . .

187. ,, ,, Present form . . .

Plan of a series of isolated and independent

THEORETICAL STUDY OF ALUMINIUM, IRON, AND

ALUMINIUM AND ITS COMPOUNDS

I. ALUMINIUM (Al = 27)

i. Preparation in the Laboratory. HISTORICAL. Aluminium

reacting on purified aluminium bromide with sodium in a

1. xxxvi. c. Ixvi. 195), mention a workman who discovered a

springs in Italy, it is not impossible that the method consisted in

The discovery of aluminium would thus appear to date back