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A HANDBOOK
FOB
CEMENT WORKS CHEMISTS

CHARLES GRIFFIN AND CO. LTD. PUBLISHERS
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CALCAREOUS CEMENTS
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:
Their Nature, Preparation

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LONDON : CHARLES GBIFFIN AND Co. LTD. EXETEE ST. STEAND
TO 15E HAD OF J. B. LlPPINCOTT COMPANY. PHILADELPHIA

A HANDBOOK
FOR
CEMENT WORKS CHEMISTS

BY
FRANK B. GATEHOUSE,
,
F.C.S.
ASSOCIATE OF THE MERCHANT VENTURERS* TECHNICAL COLLEGE, BRISTOL
FORMERLY CHEMIST AT J. AND B. WHITE, BROS. (A.P.C.M. LTD ),
SWANSCOMBE, KENT RESEARCH CHEMIST TO H. W.
;
ANDERSON, ESQ., C.E. CHEMIST AT THE XEM

;
HARTFORD CEMENT WORKS
WITH ILLUSTRA TIO.\S
LONDON
CHARLES GRIFFIN AND COMPANY, LIMITED
PHILADELPHIA : J. B. LIPPINCOTT COMPANY
1908
[AU rights reserved]

THE Author \vishes to acknowledge his indebtedness
to Messrs. H. W. Anderson, C.E., H. K. G. Bamber,
F.C.S., J. W. Gatehouse, F.I.C., H. H. Slater, F.I.C.,
J. T. Stiff, the authors of the volumes consulted,
and others who have materially assisted him during
the preparation of this handbook.
KINGSTON-ON-THAMES,
1908.
179721
CONTENTS
CHAPTER I
INTRODUCTION
Prologue Equivalent
Books consulted
Solutions
........
Chemicals and Apparatus required
pp. 1-4
CHAPTER II
ANALYSIS OP RAW MATERIALS

Sampling : Moisture Loss on Ignition Silica and
Chalk or Limestone ; ; ;
Insoluble Alumina and Iron Oxide Lime ; Volumetric Determination

; ;
of CaO Lime as CaS0 4 Magnesia Sulphates Accurate Estimation of

; ; ; ;
Carbon Dioxide Rapid Estimation of C0 2 Marls, Gault Clay, Calcareous

;
Shales Clay Estimation of Iron by Means of Standard Permanganate

and Standard Bichromate Loss on Ignition Total Sulphur Sulphur
Present as Sulphate Alkalies Separation of Soda and Potash Soluble
Chloride Shales, Sandstones, and Slates Natural Cement Rock-
Slags Phosphorus and Sulphur pp. 5-37
CHAPTER III
CALCULATION OF PROPORTION OP RAW
MATERIALS
Limestones Clay, Shales, &c. Slurry Moisture Fineness ; Estimation
: ;
of CaC0 3
; Preparation
of a Standard Dry Slurry or Raw Meal ; Slater's
Calcimeter; Bamber's Calcimeter ; To Calculate Percentage of CaC0 3 ;
Estimation of CaC0 3
Loss on Ignition
; ; Calculated CaC0 3 Control
and Alteration of the Raw Mixture pp. 38-55
CHAPTER IV
ANALYSIS OP FUEL, LUBRICANTS, WATER,
AND KILN GASES
Coal :
Moisture; Ash; Volatile Matter : Fixed Carbon; Coke; Sulphur; Ana-
lysis of Ash Analysis of Coke Power of Fuel Fineness
Calorific
vii
viii CONTENTS
Lubricants Loss or Gain in Weight Specific Gravity Viscosity Flash
:
; ; ;
Point Free Mineral Acids Free Fatty Acid Separation of Fatty and
; ; ;
Mineral Oils Water Analysis Collection of Samples Colour, Odour,

:
;
Reaction ; Sediment and Suspended Matter Total Solids Chlorine as

; ;
Chlorides Hardness, Temporary and Permanent

;
Contamination ;
:
Standard Ammonium Chloride, Nessler's Reagent, Alkaline Perman-

ganate, Estimation of Free Ammonia, Albuminoid Ammonia Estima- ;
tion of Oxygen required to Oxidise Organic Matter Estimation of ;
Nitrates + Nitrites Poisonous Metals ; Water Softening Gas Ana-

;
lysis Collection of Samples ; Analysis of Gases in the Hempel Appara-

:
tus Filling the Burette Estimation of Carbon Dioxide, Oxygen, Carbon

; ;
Monoxide, Nitrogen, Combustible Gases ; Analysis with the Orsat

Apparatus Condition of Combustion in a Rotary Kiln
; pp. 56-90 .
CHAPTER V
CEMENT ANALYSIS
Accurate Methods Alumina and Ferric Oxide Lime Magnesia
Alkalies Ordinary Method of Analysis for Technical Purposes
Insoluble Residue Sulphuric Anhydride Sulphur as Sulphide Loss
on Ignition Carbon Dioxide Rapid Method for Estimation of Lime in
a Cement Analysis of Gypsum, Plaster, Keene's Cement, &c.
Estimation of Caustic Lime (CaO) in Burnt Lime, &c. pp. 91-103 .
APPENDIX
Examples of Calculations occurring during Analysis Directions for
Making up Solutions Tables Typical Analyses Useful Data for
Testing Room pp. 107-135
INDICES .... ... pp. 137-142

CHAPTER I
INTRODUCTION
As indicated by its title, this book is intended
primarily for Cement Works Chemists, although it
is hoped that it may be found of use in other

laboratories. It has been the aim of the compiler,
in order to keep the book within reasonable limits,
to include only essential details of manipulation
where this was
possible without ambiguity. Each
separate process will be found in a numbered para-
graph, and a method once described is indicated in
the text by that number when
has again to be it
carried out. An epitome of most of the processes

will be found at the foot of the fuller description.
In this the book may be of use as a guide to
way
younger and less experienced chemists, often found
on cement works, as well as for reference purposes
by the experienced,
For the sake of uniformity the strengths and
volumes of the solutions employed are stated accord-
ing to Reddrop's system as described and followed
by Phillips in his Engineering CJiemistry.
Atable will be found in the Appendix giving
instructions for making all the necessary reagents
2 CEMENT CHEMISTS HANDBOOK 1
and strength in terms of E, this being

their
the symbol used to denote the equivalent or
equivalents of the reagent by weight, in grams
per litre. These reagents need not be made with
the same degree of accuracy as those employed in
volumetric analysis. For fuller particulars reference
should be made to the work mentioned.
The following is a list of chemicals and apparatus
required for the processes described in this hand-
book :
CHEMICALS REQUIRED.
Pure hydrochloric acid. Soda lime.
Commercial Potassium bichromate.
Pure nitric acid. chromate.
sulphuric acid. ferricyanide.
acetic acid.
ferrocyanide.
hydrofluoric acid. nitrate (powder).
Oleic acid.
permanganate.
Oxalic acid. carbonate.
Pyrogallol. hydrate.
Pure ammonium hydrate (-880). bisulphate.
j> oxalate. ,,
chlorate.
?? ,, thiocyanate. Ferrous ammonium sulphate.
Ammonium carbonate. Magnesium chloride.
chloride. oxide.
molybdate. Manganese carbonate.

Sodium carbonate (anhydrous). Copper sulphate.
? ,, (crystals). oxide.
bicarbonate. turnings,
hydrogen phosphate. Silver nitrate.
thiosulphate. Ferrous sulphide.
,, hydrate,, Piano wire.
., acetate. Pumice stone.
sulphite. Indigo.
INTRODUCTION
CHEMICALS REQUIRED (contimted).
Mercuric chloride. Lead nitrate.

Bromine. Pure zinc.
Distilled water. Litmus.

Cotton wool. Methyl orange.
Calcium chloride. Phenolphthalein.
carbonate. Alcohol.
Iceland spar. Ether.
Barium chloride. Paraffin.
Platinum chloride. Petroleum ether.
APPARATUS REQUIRED.
Abel's flash point apparatus. Desiccator.
Absorption apparatus. Drying tubes.

Accurate balance and weights. Erlenmeyer flasks.
Agate pestle and mortar. Evaporating basins.
Air oven. File.
Argand burners. Filter paper (Schleicher and

Barometer. Schull).
Battery. Flasks.
Beakers. Funnels.
Bellows. Gas analysis apparatus.
Blowpipe. Retort stands.
Bottles. Glass tubing and rod.
Bunsen burners . Graduated flasks.
Burette holders. Grease pencil.
Burettes. Hot plate.
Calcimeters. India-rubber tubing.
Calorimeter. Iron pestle and mortar.
Clips. Measuring tubes.
Clock glasses. Microscope.
Condensers. Muffle furnace.
Cork borer. Nitrometer.
Corks. Phillips beakers
Crucibles. Pipe-clay triangles
4 CEMENT CHEMISTS' HANDBOOK
APPARATUS REQUIRED (continued).
Pipettes. Spatulas.
Platinum crucible and capsule. Spotting tile.
Reagent bottles. Thermometers.
Retorts. Test-tubes.
Rough balance. Viscosimeter.

Rubber bungs. Ware pestle and mortar.
Sample jars. Wash bottles.
Sieves. Watch-glasses.
Specific gravity bottles. Weighing bottles.
The following works have been consulted in com-

pilation of this book, and are recommended for
reference purposes :
AUTHORS. BOOK.
Phillips. Engineering Chemistry.

Stanger and Blount. Reprint from J.S.C.I. on Cement
Analysis.
Clowes and Coleman. Quantitative Analysis.
C. and J. J. Beringer. A Text Book on Assaying.
Dennis. Hempel's Gas Analysis.
Kenwood. Public Health Laboratory Work.
Bayley. Chemist's Pocket Book.
Meade. (U.S.A.) Portland Cement.
Eckel. ,, Limes, Plasters, and Cements.
Taylor. Cement Testing.
Orton. Hydraulic Cements (Ohio Survey,
vol. iii.).
CHAPTER II
ANALYSIS OF RAW MATERIALS

Sampling. When
sampling a new supply, or
possible source, of raw materials, great care must
be taken to obtain an accurate average sample.
When possible the sampling should be supervised
by the chemist or other competent person. The
plan to be followed necessarily varies with the
situation and material, and must be left to the
discretion of those on the spot. If possible, samples
should be taken at different depths as well as in
on the surface of a deposit. Each
different places
sample should be carefully numbered and labelled

for reference purposes. Distinct geological layers
should be specially sampled and separately analysed.
All the samples should be examined separately,
and an average sample of the lot should also be
made and analysed. In the case of large samples of
fairlydry materials, such as limestone, the material
should be reduced to a convenient size, thoroughly
"
mixed, made into a heap, and sampled by quarter-
"
ing ;
that is, the heap is divided into four equal
parts diagonally, and an equal amount taken from
each part ;
if necessary, this may be repeated until
a convenient weight or bulk is obtained. In the
case of wet clays, etc., greater difficulty will be
experienced, and these are

more readily sampled
after being allowed to partially dry. If the per-
centage of moisture in sample is required, however,

this should be done approximately on as large a
sample as possible, as well as more accurately in

smaller quantities as described later.
(1) Chalk or Limestone. If sufficiently dry,

break up the sample in a clean iron mortar, and,
by quartering, obtain a portion for examination
weighing about 300 grams. Store the remainder
in a numbered and labelled jar or large bottle for
reference purposes. Grind the smaller portion by
hand or in a clean sample mill to all passes through
the 90-mesh sieve, and place in a clean, dry, stoppered
bottle for analysis (A).
(2) Moisture. If very wet and difficult to

reduce to powder, weigh up on a "decimal" or
other balance as large a quantity as possible, say
5000 grams, of the roughly crushed sample. Place
in a large tin dish or tray and dry over the hot
plate, taking care that the temperature does not

rise above 110 to 120 C. When
apparently
quite dry allow to nearly cool, and weigh.
Loss in weigh t = approximate moisture.
Repeat if
necessary, calculate to percentage.
As a rule a very approximate estimation of the
moisture only is
necessary. Treat the dry sample
as in (1).
ANALYSIS OF RAW MATERIALS 7
(3) If fairly dry and readily powdered, an accu-

rate estimation of moisture may be made as follows.
Weigh out accurately into a flat porcelain weighed

dish or capsule 5 grams of the sample (A) and place
in a steam or hot airoven at a temperature of
100 to 105 C. for one hour. Remove from oven
and place in a desiccator ;
when
quite cool weigh
rapidly ; note weight. Generally one hour's dry-
ing is sufficient, but the result should be checked
by replacing in the oven for another twenty minutes,
cooling and weighing as before.
Loss in weight x 20 = percentage of moisture
at 100 C.
Place the dried materials in a clean, dry, stoppered
weighing tube, and use for analysis.
Epitome.
Break up sample roughly.
" "
Quarter to about 300 grams.
"Approximate moisture" on hot plate.
Accurate moisture in oven at 105 C.
Reserve large sample for reference, dried
material for analysis.
(4) Loss on Ignition. Into a weighed platinum

capsule or crucible weigh out 0*5 gram of the dry
material and place in a gas muffle at a bright red
heat for twenty minutes. It is sometimes necessary
to cover the capsule with a crucible lid during the
first five minutes of heating to avoid loss by "spurt-
ing." At the end of the twenty minutes remove
from muffle and allow to cool in a desiccator ;
weigh.
Loss in weight x 200
= loss on ignition (or
C0 2 + H 2 and organic matter).
Reserve residue for analysis.
Epitome.
0'5 gram in muffle for twenty minutes.
Cool in desiccator and weigh.
(5) Silica and Insoluble. Brush the ignited

residue from (4) into a 6- or 7-inch evaporating dish,
flat form. Cautiously add a.bout 15 c.c. of dis-
water, rotate to prevent formation of lumps,
tilled
and add 25 c.c. of 10E HC1 wash out the platinum

;
dish with a little acid into the big dish, and place
latter on the cooler part of a hot plate or on a water
bath.
Evaporate very carefully to dry ness to avoid

spurting, and then cover with a clock glass and re-
move to the hottest part of plate and allow to bake
for one hour. Remove from hot plate, allow to cool
for five minutes and add 25 c.c. of 10E HC1 and
warm very gently until the residue is free from
colour due to iron compounds. Wash down clock
glass and interior of dish with boiling water from a
wash bottle. Filter through a 9- or 12-cm. black
band paper into a 30-oz. Phillips beaker, retaining
as much as possible of the residue in the dish wash ;
by decantation thus three times at least, and then

wash residue into the filter, clean out the dish by
means of a rubber-tipped glass rod, and finally with

the tip of the finger, until every trace of residue is
contained in the filter paper.
When has run through, place the funnel
filtrate
and contents, which, as well as all other apparatus
used, should be distinguished by a number or mark,
in a drying cone on the hot plate or oven to dry.
Carefully transfer paper and contents to a weighed
and marked porcelain crucible, burn off paper over
a burner or in the mouth of the muffle furnace, then
ignite in muffle for one hour. Cool in desiccator
and weigh.
It is convenient to retain all ppts. obtained during
analysis for ignition together later.
Weight weight of crucible = insoluble + filter
ash.
Insoluble filter ash x 200 = per cent, silica +
insoluble.
Epitome.
To residue from (4) add 25 c.c. 10E HC1 and
evaporate to dry ness.
Take up with 25 c.c. HC1. Filter, wash, weigh.
Reserve filtrate for (7).
(6) It not generally necessary to separately

is
estimate the soluble and insoluble Si0 2 but this ,
may be done on another portion of the original

material as follows. Weigh out 0'5 gram into a
5 -inch evaporating dish, add water as before, and
cautiously add 25 c.c. 10E HC1, covering the dish

as much as possible with a clock glass to prevent
loss. Warm on a hot plate until all soluble matter

is in solution, then filter this through 9-cm. black
band paper and wash by decantation, retaining the
residue in the dish. The filtrate is used for SO 3
estimation (13).
Invert the funnel over the dish and wash out any
trace of residue in the paper. Add 10 c.c. 3E
C0
Na 2 3 solution and boil for ten to fifteen
minutes, filter rapidly through the paper previously

used and wash with boiling water until free from
alkali or until a drop of filtrate evaporated on a watch-
glass leaves no residue. Dry, ignite, and weigh.
Weight ash x 200 = per cent, insoluble residue.
It may be necessary to estimate H 2 3

in the
"
insoluble residue by fusion."
Epitome.
0'5 gram treated with 25 c.c. HC1 warm.
Filter by decantation, wash.
Boil residue with 10 c.c. sodium carbonate solu-
tion.
Filter, wash, dry, weigh.
(7) Alumina and Iron Oxide. The filtrate

from (5) is returned to the dish and warmed until
nearly boiling upon the hot plate or over an argand
burner. When nearly boiling add a drop or two of
bromine water continue to warm, but do not boil,
;
and add carefully 10E 4

NH
OH until a ppt. forms ;
stir with glass rod and add Allow

slight excess.
to remain on hot plate until free from odour
nearly
ANALYSIS OP RAW MATERIALS 11
of ammonia, or about fifteen minutes. Filter through

a 15-cm. black band paper rapidlyând wash with
boiling water, churning up the ppt. on the filter
paper with the water jet, until a. drop of the filtrate
gives no indication of the presence of chloride when
E
tested with AgNO 3 solution. Dry and ignite in
muffle one hour, cool in desiccator, and weigh.
Weight of ppt. x by200=percent.ofAl 2 O 3 + Fe 2 3
.
The amount of A1 2 O 3 + Fe 2 O 3 in a limestone is

gene-
rally so small as to render separation unnecessary.
Epitome.
Filtrate from (5) ; nearly boil.
Oxidise with bromine water and ppt. with

ammonia.
Warm for fifteen minutes, filter, wash, ignite,
weigh.
(8) Lime. The filtrate from (7) is brought

nearly to boiling-point in a large (40-oz.) Phillips
beaker. Add a few c.c. of 5E 4
NH OH
and boil ;
whilst boiling, add 50 c.c. of boiling -^- Am. oxalate

o
solution, place a watch-glass over beaker and allow

to steadily boil for five minutes. Remove from the
direct heat and allow to settle, if possible in a warm
place, for one hour or longer.
Filter through a Swedish or white band 15-cm.
paper into a large bottle or beaker, wash the ppt.,
first
by decantation with warm but not boiling
12 CEMENT CHEMISTS HANDBOOK
1
water then wash ppt. into the filter paper,

; removing
any traces adhering to sides of the beaker by means
of a rubber-tipped glass rod.
The lime may be determined volumetrically by
means of standard permanganate (9) or gravimet- ;
rically, most conveniently as CaS0 4 (10). The

filtrate is used for determination of MgO (11).
(9) Volumetric Determination of CaO. In

order to avoid accumulation of a bulky filtrate for
MgO determination, continue washing the calcium

oxalate ppt. on the paper into another vessel until a
drop of the filtrate will not discolour a little distilled

water rendered just pink with a trace of perman-
ganate solution acidified with 5E 2
S0 4 H .
Then carefully remove the paper and its contents

from the funnel, open it out over a
large ordinary
beaker, and wash the ppt. from the paper into the
beaker it is better to complete this operation by
;
using a small wash bottle containing 5E 2

SO 4 H .
Add 15 to 20 c.c. of this acid, make up the contents

of beaker with water to about 250 c.c., and bring to
boiling-point.
Titrate with standard
permanganate solution,
whose strength is known in terms of CaO, until a
permanent pink colouration is obtained.
Number of c.c. used x factor x 200 = percentage of
CaO.
Per cent. CaO x J 5 6 - = CaC0 3<>
.
(lo) Lime as 4
CaSO
Wash calcium oxalate
.
ppt. until free from chlorides, dry, place in weighed

ANALYSIS,OF RAW MATERIALS 13
platinum crucible with a lid, and ignite gently over

a bunsen burner to burn off filter paper.
Remove from burner, allow to cool, and add by
means of a pipette or glass tube with a fine point,
drop by drop, pure strong (36E) H.2 S0 4 holding the ,
lidover the crucible whilst so doing, until the whole

of the ppt. is moistened with the acid. Heat the
uncovered crucible over an argand or bunsen burner
with a rose top, using a very small flame, in a
draught cupboard until no fumes are evolved. Re-
place the lid and heat just to redness over a burner
for about thirty seconds, cool and weigh as CaSO 4 .
Weight of CaS0 4 x TV ('4117) x 200 = per cent.

CaO or use table (see Appendix
;
24 A). Calculate
to CaC0 3 as in (9).
Epitome.
(8) Boil filtrate (7) ;

add ammonia + 50 cc.
boiling Am. ox. ;

allow to settle, filter, wash.
(9) Dissolve in 5E H SO2 4 + H 2 O, boil, titrate
with standard potassium permanganate.
(10) Dry, ignite, add sulphuric acid in platinum
crucible, drive off sulphuric acid, weigh as
CaS0 4 .
(n) Magnesia. Evaporate the filtrate from (8)

nearly to dr} ness in the large dish add 30 c.c. 16E
r
;
HNO 3
and heat on hot plate in draught cupboard
until no more ammoniacal salts are volatilised.
Remove from plate, allow to cool then add about ;
10E HC1 and about 20 c.c. of water. Warm

5 c.c. of
and add slight excess of 10E NH 4 OH filter off ;
the small ppt. of Si0 2 ,Al 2 3 ,Fe 2 3 through a 5-cm.
black band paper and wash. This may generally be
to impurities in the reagents
ignored as being due
and from the vessels used.
To the filtrate, which should not exceed 100 c.c.
or so, when cool add at least 10 c.c. of 20E NH 4 OH,
9TT
then 5 c.c. of -Q- Na 2 HPO 4 solution. Stir well with
a rubber- tipped rod, but avoid touching the sides of

the beaker as much as possible, and place in a dish
of water or other cool place to settle for twelve hours
(over night) if time permits.
When the ppt. has completely settled, filter
through a 7- or 9-cm. Swedish or white band filter
paper, wash by decantation, using 5E 4

then NH OH ;
transfer ppt. to the paper, rub out carefully any
particles adhering to side of beaker, and wash on the

paper until a drop of the filtrate, when acidified with
Tfi
nitric acid gives no ppt. with AgNO 3 solution.

-^
It isimportant that the washing should be com-

plete, but not excessive.
Ignite, best in a platinum crucible, first at a low
temperature over a bunsen burner and then at a

higher temperature or in a muffle furnace for twenty
;
minutes. Cool in a desiccator and weigh as Mg 2 P 2 O 7 .
Weight of Mg 2 P 2 O 7 x T r T or ('3619) x 200 = per

4
cent. MgO ;
or use table (Appendix 25 A).
Per cent. MgO x f ==
per cent. MgC0 3 .
Epitome.
Evaporate lime filtrate to dry ness.
Add 30 c.c. 16E HN0 3 and drive off ammonium
compounds.
Take up with 5 cc. hydrochloric acid, ppt. with
10E NH 4 OH.
Filter, wash, cool. Add 20 c.c. 10E NH OH 4
and 5 cc. sodium phosphate solution, stir.
Allow to settle, filter, wash with 5E NH OH.4
Dry, ignite, weigh as Mg 2 P 2 7

.
Calculate to MgO or MgC0 3 .
(12) Alkalies are generally estimated by differ-
ence, but the method described under Clay (31) or

Cement (122) may be adopted if necessary.
(13) Sulphates. Boil the filtrate from (6) and,

whilst still boiling, add 10 c.c. of E BaCl 2 solution ;
after five minutes allow to settle in a warm place
for a few hours. through a 7-cm. No. 417A
Filter
Max DreverhofFs paper, wash with warm water
until free from chloride, dry, ignite, and weigh as
BaS0 4 .
Weight of BaS0 4 x -gfo x 200 = per cent, of

S0 3 (see Appendix 26 A).
Epitome.
Filtrate from (6). Boil, add 10 c.c. E BaCl 2 .
Allow to settle, filter, wash, ignite, weigh as

BaS0 4 .
Accurate Estimation of Carbon Di-
(14)
oxide. One gram of the limestone is decomposed by
the carbon dioxide
hydrochloric acid in a flask,
evolved is absorbed by potassium hydrate solution,
after passing over various reagents, and weighed.
The following apparatus must be fitted up. The
lettering refers to the illustration. (Fig 1.)
Afairly wide-mouthed flask (A) is fitted with a
three-holed rubber bung ; through one hole is passed
a stoppered funnel (b) ; containing soda-
a tube (a),
lime, is passed through one of the other holes and ;
the remaining one is fitted with a glass tube which

isconnected to the absorption apparatus. two- A
holed bung may be used, in which case the funnel
issubstituted by a pipette connected at the upper
end with the soda-lime tube, a Mohr's clip being
placed on the connecting rubber, and this is released
when the acid has to enter the flask. The tube
leading from the flask is connected by rubber, first
with bulbs (.Z?) containing strong sulphuric acid ;
secondly, to a U-tube ((7), the nearer limb of which

with copper sulphate pumice, and the other
is filled
limb with solid calcium chloride. Connected to

this tube are the potash bulbs (D), in which the
GO 2 has to be absorbed and weighed ; arid these
are in turn connected to a straight calcium chloride
tube, which is also weighed with the bulbs.
The absorption bulbs should be filled with 5E KOH
solution in sufficient quantity to fill the lower half
of the bulbs and to be contained in the large pear-
shaped bulb should there be any back pressure.
The whole apparatus is connected with an aspirator

made from a Winchester quart bottle as shown.
Instead of potash bulbs, a U-tube containing

soda-lime may be used.
Stoppered U -tubes
are to be preferred to corked
ones ;
if the latter are used, they should be made
air-tight with paraffin \vax.
A little
cotton-wool should be placed before and
after the CaCJ 2 and pumice-stone in the tubes, to
dust.
prevent the passage of fine
All rubber connections should be wired on and
the apparatus tested before use. When the appa-
ratus is ready for use, detach the absorption bulbs
or tube arid the CaCl 2 straight tube stop up the ;
open end of the rubber tube by means of a bit of

glass rod. See that the bulbs and tube are quite
dry, and weigh.
Weigh out into the flask gram of the material,
1
cover it with water. Place 50 c.c. of 5E HC1 in the

funnel or pipette, and reconnect up the whole appa-
ratus, except the aspirator. Close the air inlet
through the soda-lime tube.
Allow acid to drop slowly on the carbonate so
that the bubbles of air driven from the apparatus
may be easily counted as they pass through the
sulphuric acid continue addition of the acid until
;
effervescence ceases.
Close the stopper of the funnel, or, if a pipette,
carefully push the point under the surface of the
liquid, attach the aspirator and set it in action.
Place an argand burner under the flask and warm
gently. Open the air inlet tube so that a current
of air is made to pass through the apparatus until
quite half the water in the aspirator has run out.

Then stop the operation, disconnect and stopper up
the weighed bulbs, allow to get quite cool, and

weigh.
Increase in weight x 100 = per cent. CO 2 .
Epitome.
One gram decomposed by hydrochloric acid in
the absorption apparatus.
C0 2 absorbed in potash or soda-lime, and
weighed.
(15) Rapid Estimation of CO 2

. A rapid and
Yi&. 2. APPABATUS FOE RAPID ESTIMATION OF C0.2 .
fairly accurate estimation of carbon dioxide may be

made in the apparatus represented in Fig. 2.
Fit a wide-mouthed 4-oz. flask with a rubber
bung. Through one hole place a piece of glass

tube attached to a straight Cad 2 tube. Through
the other hole run a piece of glass tubing closed at

the outer end with a small piece of rubber tubing
and glass rod.
A small piece of cotton-wool is first placed in the
bulb tube, and the bulb is then filled with dehy-
drated copper sulphate pumice followed by granular
CaCl 2 in the straight part another piece of wool
;
is then inserted and the tube closed with a cork

bearing a small glass tube.
Thoroughly dry the apparatus, weigh out 1
gram
of the carbonate and brush it into the flask ; cover
with water, and then lower a small glass or gutta-
percha test-tube containing about 7 c.c. of 5E HC1
into the flask by means of a piece of cotton. Insert
the stopper so that the cotton from which the test
tube is suspended is held in place.
Weigh the whole apparatus and contents. Slightly
tip the apparatus so that the acid is caused to leave
the test-tube a little at a time. When effervescence
has ceased, warm the flask over an argand burner
for about five minutes allow it to cool somewhat,
;
and then draw, by means of an aspirator as in (14)

or by the mouth, a current of air
through the appa-
ratus, for this purpose removing the rubber cap of
the inlet tube. Allow the apparatus to cool, see
that the exterior is quite dry, and weigh
complete
as before.
Loss in weight x 100 = per cent. C0 2 .
A determination can be made in about thirty

minutes.
Epitome.
Weigh into prepared flask

gram. 1
Decompose with hydrochloric acid, warm, cool,
weigh.
The an ordinary chalk or lime-

total carbonate in
stone may be rapidly estimated as CaCO 3 upon one
of the calcimeters described in chapter iii., and
especially conveniently upon Slater's instrument,
using the Tables given in Appendix (27 A" and 28A).
A dolomite or magnesian limestone is insoluble
in cold hydrochloric acid, and therefore the C0 2
cannot be estimated upon a calcimeter. Of course,
for Portland cement manufacture to standard
speci-
fications such limestones are useless, and therefore
of no importance.
Should an analysis of such material be required,
the methods previously described (5, 6, 7, 8) may
be used but care must be taken that throughout
;
the analysis there a sufficient quantity of ammo-

is
nium chloride present to prevent the precipitation

of magnesium Mg(OH) 2 by ammonia.
as
In reporting the result of an analysis of a chalk
or limestone, generally sufficient to state total
it is
lime as CaO, and its equivalent of CaC0 3 separately,

MgO, loss on ignition (which includes CO 2 2 O, and ,
H
organic matter), silica, ferric oxide and alumina and ;
alkalies by difference.
$2 CEMENT CHEMISTS' HANDBOOK
MARLS, GAUL/T CLAY, CALCAREOUS
SHALES. These materials, as found in the
British Isles,are intermediate in chemical com-
position between limestones and true clays and

shales.
The method adopted for analysis must largely
depend upon the particular material under exami-
nation ; when the calcium carbonate
present in
is
the proportion of 70 to 75 per cent., the processes

described under Limestone (1 and following) may be
used. When the CaC0 3 does not exceed 25 per
cent., the methods to be described for clays and
shales may be used, care being taken that, after
treatment with sulphuric acid, sufficient 10E HC1
is used to take
up all the CaS0 4 formed, or this will
be included erroneously in the " insoluble."
The following method giving total Si0 2 Fe 2 O 3 , ,
3 GaO, and MgO may be used in most cases

A1 2 ,
satisfactorily.
(16) Weigh into a capacious p ] atinum crucible or
capsule '5 gram of the dry sample (3), and ignite in

muffle at a good red heat for twenty minutes. Cool
in desiccator and
weigh rapidly.
Loss in weight x 200 = percentage loss on
ignition.
(17) Mix the ignited residue with about 5 grams

of fusion mixture
(K 2 C0 3 ,Na 2 CO 3 ) in the platinum
crucible or large capsule,
using the smooth end of a
glass rod to incorporate the contents.
Heat carefully over a bunsen burner for about
ten minutes, and then over a blast burner or in a
muffle until the mixture is in a state of quiet, com-
plete Rotate the crucible to spread the

fusion.
fused mass as much as possible, and then allow to
cool rapidly by standing in a little cold water or on
a cold slab. Place in a large evaporating basin,
cover with distilled water and digest on hot plate
until the mass has broken up and the crucible and
lid can be washed clean. If necessary, a little 5E
HC1 may be used to ensure the crucible being clean.
Then add sufficient 10E HC1, a
at a time,
little
covering the dish as far as possible with a clock

glass to prevent loss, until a clear solution is
obtained.
Evaporate slowly on the hot plate or air bath

almost to dryness, remove and add about 10 c.c. of
10E HC1, and wash any material from the clock
glass and sides down into the bottom of dish.
Evaporate slowly to dryness, if necessary breaking

up any lumps that form with the end of a glass
rod when dry, bake on the hot plate for at least
;
one hour.
Remove from the hot plate and, when nearly
cool, add 25 c.c. 10E HC1 and sufficient water to
dissolve the chlorides formed.
Filter through a 12^-cm. black band paper and
wash well. After fusion, all the washings require
to be very thorough. Repeat the evaporation and
filter off any trace of Si0 2 and add to that first
,
obtained.
Dry, ignite, and weigh.

Weight
- filter ash x 200 = per cent. SiO 2 .
Estimate Al 2 O 3 + Fe 2 3 as in (7); but if Fe 2 O 3

,
is
required separately, take
1
gram of substance
for analysis and follow the plan described under
Clay (24), making the solution up to a known

volume, and divide into two portions, using one
portion for volumetric determination of Fe 2 3 (25,
26, 27).
Estimate CaO as in (8) and MgO as in (11).
Epitome.
Fuse '5 or 1
gram with fusion mixture.
Dissolve mass in water and hydrochloric acid.
Evaporate to dryness, bake, cool, take up with
water and hydrochloric acid.
Filter, wash, and weigh Si0 2 .
Ppt. A1 2 3 Fe 2 3 with ammonium hydrate

, (7).
Filter, wash, weigh.
Ppt. CaO with ammonium oxalate (8).

Filter, wash, estimate.
Evaporate to dryness, add 30 c.c. nitric acid.
Estimate MgO as Mg 2 P 2 7 (11).
(18) CLAY. A
mechanical analysis of clay,
except brickmaking, is not often required.
for
When necessary it must be carried out on the
undried samples by elutriation. For this purpose
an apparatus specially made may be used, or a
series of bottles or iars can be fitted up as
follows.
Choose three wide-mouthed bottles and fit them

with sound corks, each bored with two holes to
carry fairly large glass tubing, in each case one
piece being carried to the bottom of the vessel and
the other just through the cork. The longer tube
of the first bottle is connected to a water tap, the
smaller piece to the succeeding bottle, and so on, so
that a stream of water may be run through the
whole apparatus, the overflow from the last bottle
being caught in a large jar or pail.
A weighed amount, say 100 grams, of the clay is
placed in the bottle attached to the tap and a gentle
stream caused to circulate through the apparatus
until the overflow water comes over quite clean.
The water is and the material in
then turned off,
the bottles allowed to subside. The bulk of the

water is poured away, and the solid matter washed
out into a weighed dish, dried, and weighed. The
residues being reported as coarse (sand), medium,
fine, and very fine by difference. If necessary, the
fineness of each portion upon standard sieves may
be taken. As
stated previously, however, upon a
cement works using modern machinery the physical
condition of the raw material is of little importance
compared with the chemical composition.

The moisture should be " approximately esti-
"
mated (2), and the whole sample, when dry,
powdered. A
smaller sample obtained by quarter-
ing should then be dried in the air oven and
kept for analysis in a weighing tube or stoppered
bottle.
(19) Estimation (sand), A1 2 3 Fe 2 3
of Si0 2 ,
O ,
CaO, and MgO. Weigh into a large porcelain or
platinum dish 1 gram of the dry powdered clay

and cover with 20 2 S0 4
c.c. 36E H
rotate cautiously;
to break up any lumps, cover with a clock glass,

and heat very gently best over an argand burner
for 10 hours (over night).In the morning remove
the clock glass and increase the heat sufficiently to
steadily drive off the sulphuric acid.
When no more fumes are driven off, place on
the hot plate for about twenty minutes. Remove
from the hot plate, allow to cool somewhat, and
then add 25 c.c. of 10E HC1 and a little distilled
water.
Filter through a 12 '5 -cm. black band
paper,
retaining the insoluble matter in the dish. Add
another 25 c.c. of hydrochloric acid, digest on the
hot plate for a few minutes, add water, and filter
as before.
Repeat this operation, using altogether 75 c.c. of

acid, then wash by decantation until free from
chlorides, and when cold make filtrate up to 500
c.c.
(24).
Wash any material upon the filter paper back
into the dish and boil with 25 c.c. of 5E Na 2 CO 3
solution or with 1
gram sodium carbonate
of
crystals and sufficient water, for about fifteen
minutes. Filter, whilst still hot, through a 12'5-
cm. black band paper, and wash with boiling water
until quite free from Reserve
any trace of alkali.
filtrate for SiO 2 estimation (23).
Dry residue, ignite in platinum crucible, and

weigh.
Weight ash x 100 = per cent, insoluble, sand, &c.
(20) After weighing, treat the insoluble matter

in the platinum crucible with about 5 c.c. of hydro-
fluoric acid and a few drops of 36E 2 S0 4
warm H ,
over a small argand flame in a good draught cupboard

until no further fumes are evolved. Repeat three
times, when there should be only a small residue
remaining.
Treat this residue with 10E HC1, warm in a
small dish or beaker, and filter through a 7-cm.
paper, wash, dry, ignite, and weigh as TiO 2 .
Weight- ash x 100 = per cent. TiO 2 .
(21) In the filtrate from above, estimate (7)

A1 2 3 ,
Fe 2 3 (R 2 3 ).
Weight ash x 100 = per cent. R O in

2 3
insoluble.
It is usual then to calculate the R O 2 3 to felspar
6SiO 2 .Al 2 O 3 .Na 2 O thus :
Per cent. R 2 O 3 x 3*5 = per cent. SiO 2 .
Per cent. R 2 O 3 x *6 = per cent. Na 2 O.

Per cent, insoluble -(Si0 2 + R 2 O 3 + Na 2 O + TiO 2 )
= per cent, quartz. (See Appendix for example.)
The insoluble matter can then be reported as shown
in Appendix [1A]. The result thus obtained is not
absolutely accurate, but suffices for most purposes.
(22) Instead of treating the residue (19) with

hydrofluoric acid, the SiO 2 and A1 2 O 3 can be esti-
mated by fusion as in (17).
(23) Acidify with 10E HC1 the alkaline filtrate
from the insoluble estimation (19), and evaporate
dish
carefully to dryness in a platinum or porcelain ;
bake for half an hour, allow to cool, and then take

up with water and a little 10E HC1, filter through
a 12 "5 -cm. paper and wash till free from chloride.
Dry, ignite in muffle for one hour, and weigh.

Weight filter ash x 100 = per cent. Si0 2 .
(24) The which has been made up to 500

filtrate,
c.c., is divided into equal portions of 250 c.c. In one

part the A1 2 3 Fe 2 3 CaO, and MgO are esti-
, ,
mated as in (7) (8) and (1 1). If small in amount the

calcium oxalate ppt. may be converted into CaO over
a blast burner or in the muffle and weighed as such.
(25) Estimation of Fe 2 3 . The A1 2 3 Fe 2 3

,
is pptd. as in (7), filtered and washed slightly it ;
is then redissolved in dilute acid and the iron

estimated after
reduction, using
volumetrically
standard potassium permanganate or bichromate
solution.
(26) Estimation of Iron by means of

Standard Permanganate. Dissolve the ppt. of
A1 2 3 Fe 2 O 3 in 5E H 2 S0 4 and wash into an
,
Erlenmeyer flask, add fair excess of the acid and a

few small pieces of pure zinc. Fit the flask with a
cork bearing a bunsen valve, i.e., a piece of glass
tube to which is attached a piece of rubber tubing
having a longitudinal slit and closed with a glass
rod or clip, and place in a slightly warm place until
reduction is
complete. This is
approximately indi-
cated by the solution becoming colourless, when a

drop should be withdrawn on the end of a glass
rod and tested by means of ammonium or potas-
sium sulphocyanide solution, the reduction being
complete when there is no pink colouration with
that reagent.
Filter the reduced iron solution rapidly and wash
into a clean flask if necessary, add more sul-
;
phuric acid and titrate with standard permanganate

;
[17 A] solution until a permanent pink colour is

obtained.
No. of c.c. x Fe 2 3
factor x 200 = per cent. Fe 2 3
.
Subtract from A1 2 O 3 Fe 2 , 3
found (24) = A1 2 O 3 .
(27) Estimation of Iron by means of

Standard Bichromate. Dissolve the ppt. of
A1 2 3 Fe 2 O 3 in 5E HC1, as small a quantity as
,
possible, wash an Erlenmeyer

into flask fitted with
bunsen valve, dilute to about 200 c.c., and add 20
c.c. of 2E Na 2 SO 3 . Boil for twenty minutes or
until free from S0 2 . Cool as quickly as possible
and test as above ;
if reduction is
complete, titrate
with the standard bichromate [ISA]. On a clean
spotting tile have ready a number of drops of freshly
prepared, very dilute potassium ferricyanide solu-
tion, run the bichromate solution, at first a few c.c,
at a time, later drop by drop, into the iron solution ;
after every addition abstract a drop by means of a
glass rod and place in contact with the "spots" of

ferricyanide. The reaction is complete when no
blue or green tint is produced with the ferricyanide.
No. of c.c. x Fe 2 3
factor x 200 = per cent. Fe 2 O 3 .
Epitome.
Treat 1 grain for ten hours with 36E H 2
S0 4 ,
dry and bake.

Take up with three portions 10E HC1, filter,
wash.
Residue = SiO 2 and insoluble.
Boil residue with 25 c.c. 3E Na 2 CO 3 .
Filter, wash, residue = insoluble.

Filtrate, acidify, evaporate = SiO2 .
Filtrate from insoluble = A1 2 O 3 Fe 2 O 3 CaO,

, ,
MgO(7, 8, 11,25).
(28) Loss on Ignition. Ignite '5 grarn of the

powdered and dry sample twenty minutes in a
for
muffle. Cool in desiccator and weigh rapidly.
Loss in weight x 200 = per cent, loss on ignition.
If an ultimate analysis only is required this
residue (28) may be treated as (17) and the
11 "
rational method (19) omitted.
Total Sulphur. One gram of the dry

(29)
sample is mixed with 10 grams of a finely powdered
mixture of Na 2 CO 3
(10 parts) and 3 (1 part)
KNO
and heated to quiet fusion in a covered platinum
crucible.
The fused mass is dissolved in water, acidified
with 10E HC1, and filtered, if necessary. The
filtrate is boiled and to it, whilst still gently boiling,
is added 10 c.c. of E BaCl 2 after a few minutes the
;
ppt. is allowed to settle in a warm place for some

hours, filtered through an S0 3 paper, washed, dried,

and ignited and weighed as BaS0 4 .
Weight of BaS0 4 x *137 x 100 = per cent, sulphur.

This may be calculated to iron pyrites FeS 2 .
Epitome.
Fuse with sodium carbonate and potassium
nitrate.
Take up with hydrochloric acid, filter, wash.
Ppt. with barium chloride solution, weigh as

BaS0 4 .
(30) Sulphur present as Sulphate. Weigh

out gram of the sample into an evaporating dish,
1
add a little water and 25 c.c. of 10E HC1, warm

twenty to thirty minutes, then add 10 cc. of 10E
HC1 and water. Filter and wash. Treat the
filtrate as in (29).
Weight of BaSO 4 x -343 x 100 = per cent. S0 3 .
If this is calculated to CaSO 4 its equivalent of

CaO must be deducted from the amount found.
Thus per cent. SO 3 x 17 = per cent. CaS0 4 .
For each TO per cent. CaSO 4 deduct '41 per

cent, from CaO.
The sulphur present as sulphate must be deducted

from total sulphur found, in order to obtain sulphur
present as sulphide.
(31) Alkalies. Soda and potash may conven-

iently be estimated as follows this method being
known as Laurence Smith's :
Mix in an agate mortar 1 gram of the dry clay

with its own weight of pure ammonium chloride and
6 grams of pure precipitated chalk should there be ;
any calcium carbonate present in the clay, this must

be allowed for. Place the mixture in a platinum
crucible and heat gently at first over a buiisen burner
and then for one hour at a red heat, keeping the
crucible covered cool, turn the mass out into an
;
evaporating dish, and wash out the crucible with

distilled water into the dish. Dilute somewhat, heat
to boiling, filter, and wash into a beaker. Add 1*5
grams of solid ammonium carbonate, evaporate to
about 50 c.c., add a little more carbonate +
ammonia ;
then filter and wash.
Evaporate the
filtrate to dryness in a weighed platinum dish, heat
gently at first to drive off ammonium chloride and

then to a dull redness ;
cool in desiccator and weigh.
The weight = KC1 + NaCl.
(3ia) Separation of Soda and Potash.

Dissolve the mixed chlorides in about 5 c.c. of water
and add sufficient E PtCl 4 to convert into the double
chlorides, assuming the whole to be NaCl, 117 grams
of which require 336*38 grains of PtCl 4 . One c.c. of
E PtCl 4 solution contains '0841 gram. The mixture
isthen taken nearly to dryness on the water bath and
15 c.c. of alcohol added the dish is then allowed to
;
stand for three hours with an occasional rotation.

When the ppt. has well settled, the clear liquid is
poured off through a filter paper which has been

dried and weighed, the ppt. is washed by decantation
with alcohol and thus transferred to the filter paper
and again washed, using a small wash bottle con-
taining alcohol until filtrate is colourless. The paper
and K 2 PtCl 6 are then dried in an air or steam oven
at 100 C., cooled in a desiccator, and weighed.
Weight -weight of filter paper x -3070 = KC1.

Subtract this from weight of mixed chlorides =
NaCl.
KC1 x -63204 x 100 = per cent. 2 O. K
NaCl x -53077 x 100 = per cent. Na 2 0.
Epitome.
(31) Fuse with ammonium chloride and calcium
carbonate.
Digest with water, and wash.

filter,
Add ammonium carbonate, filter, and wash.
Evaporate to dryness.
Ignite, weigh.
(3ia) Dissolve in water, ppt. with PtCl 4 and

alcohol, filter.
Wash with alcohol, weigh on tared paper.
For cement-making purposes an accurate deter-
mination of K 2 and Na 2 O is not often necessary,
but an estimation of the soluble chloride (NaCl) is
sometimes useful.
(32) Soluble Chloride. Treat 5 grams, or

more if necessary, with distilled water in a flask or
beaker, and warm. Filter and wash well. Estimate
the chloride in the filtrate by means of standard
N as
7.
AgN0 3, using potassium chromate solution
indicator, as described under Water.

No. of c.c. x -00585 x 20 = per cent. Nad.
Shales, Sandstones, and Slates. The methods
adopted analysis of
for the these materials must
depend upon individual circumstances. As a rule

the following processes, already fully described, will
be found suitable :
Moisture (3), loss on ignition followed by (4),

fusion (17) and estimation of the Si0 2 (17),
A1 2 3
Fe 2 3 (7), CaO (8) and MgO (11).
Natural Cement Rock. This may generally

be treated as a limestone, carrying out the following
estimations :
Loss on ignition (4), silica and insoluble (5 and 6)

or a fusion of the insoluble may be made
(17), A1 2 3
Fe 2 3 (17), CaO (8 and 9),
magnesia (11), C0 2 (14 or 15) if necessary or

CaC0 3 and MgC0 3 may be obtained by cal-
culation ; sulphates (13) and sulphides (29).
(33) Slags. of the finely

Weigh out '5
gram
powdered sample into a platinum crucible and fuse
with 3 grams of fusion mixture separate the ;
SiO 2 ,
as in (17); but for accurate work it is
necessary to evaporate to dryness after filtering to

separate the remaining traces of Si0 2 .
(34) The filtrate from the silica is warmed in a
capacious beaker; a little solid and then 5E

Am C0 2 3 solution added until a ppt. just forms.
Then add a drop or two of 5E Acetic acid and

excess of 4E Sodium acetate solution. Boil gently
for ten minutes and filter, whilst still hot, through
a 15-cm. black band paper; wash.
The filtrate must be clear and colourless and is
used for manganese estimation (36).
(35) Kedissolve the pptd. basic acetates of iron

and alumina in 10E HC1 and ppt. with ammonia,
wash, dry, ignite, and weigh as A1 2 3, Fe 2 O 3 and
P2 O 5 if present (7).
(36) Add the second filtrate to that obtained from

the acetate separation (34) and concentrate some-
what, cool and then add 3 c.c. of bromine, and stir
until it has gone into solution, add 20 c.c. of
20E NH OH and boil for twenty minutes, filter,
4
wash, ignite, and weigh as Mn 3 O 4 .
Weihgt-ash x 7205 x 200 = per cent. Mn.

Or, calculate to MnO 2 or MnO.
Epitome.
Separate iron and alumina as basic acetates.

Add bromine and ammonia, filter, wash.
Weigh as Mn 3 O 4 .
(37) In the filtrate estimate CaO (8) and MgO

(a).
(38) The iron present should be estimated in

another portion of 1 gram by fusion, as in (33) the ;
iron should be separated as basic acetate, redissolved

in hydrochloric acid, reduced as in (27), estimated
by standard bichromate, and calculated

to ferrous
oxide.
No. of c.c. x FeO factor x 100 = per cent. FeO.
This must also be calculated toFe 2 O 3 ,and subtracted
from the weight of A1 2 and Fe 2 O 3 and P 2 5 found
3
(35), in order to obtain

A1 2 3 and P 2 5 if present.
Should the iron present both as ferric and ferrous
oxide be required, the process and apparatus recom-
mended by Averyand described in Phillips' B Engineer-
ing Chemistry, p. 108, maybe followed.

An alternative method is to make the filtrate from
Si0 2 (33) up bo a known bulk and then take half that
quantity for estimation of A1 2 3 Fe 2 3 CaO, and , ,
MgO, and use the other portion for estimation of

iron.
(39) Phosphorus and Sulphur. Fuse 2 grams

at least of the sample with sodium carbonate and
potassium nitrate, treat the melt with hot water

until it disintegrates, boil, filter off the bases, and
wash well. Allow the and make up
filtrate to cool
to 500 c.c. Divide into two portions (A) and (B).

Acidify A with HN0 3 and add a large excess of
ammonium molybdate solution, allow to stand for
twelve hours, at about 50 C. if the temperature ;
is allowed to rise, any arsenic

present will also be
pptd. Pour off the clear liquid through an S0 3
paper, and test with a little more molybdate
solution to ascertain whether all phosphate has
been pptd. if so, filter and wash any ppt. adhering
;
to beaker with E 3
HN0
Then, using a fresh.
beaker to collect the filtrate, dissolve the ppt. in

5E NH 4 OH, rinse out the beaker, and wash the
filter well.
paper
Add excess of magnesia mixture, treat as in (11).
Weight of Mg 2 P 2 O 7 x -638 x 100 = per cent.

PA.
Epitome.
Fuse with sodium carbonate and potassium
nitrate.
Dissolve in water, acidify with nitric acid,
ppt. with ammonium molybdate, dissolve in
ammonia, ppt. with magnesia mixture.

Subtract from A1 2 O 3 + P 2 5 and Fe 2 O 3 (35).
(40) Sulphur. Acidify (B) with 10E HOI, add

10 c.c. E BaCl 2 solution, treat as in (29).
BaS0 4 x -137 x 100 = per cent, sulphur.
CHAPTER III
CALCULATION OF PROPORTION
OF RAW MATERIALS
FROM the analysis of any given material it is
for cement
possible to estimate its usefulness
making within With entirely untried
certain limits.
materials actual tests on as large a scale as possible
should be carried out.
Any of the larger English and American text-
books on cement manufacture contain full informa-
tion as to the ideal composition.
LIMESTONES. Unless a calcareous clay or

shale is to be used, the CaCO 3 content must reach
75 per cent. A
poor limestone may sometimes be
enriched by using a purer stone to raise the per-
centage of CaC0 3 About 2 per cent. MgO renders
.
the stone useless for cement making to standard

specification ;
it is desirable that only 1 per cent, or
less be present.
For use with rotary kilns, a sulphur as
little
sulphide or sulphate is immaterial either in the

stone or clay.
38
PROPORTION OF RAW MATERIALS 39
CLAY, SHALES, Etc. The proportion of

SiO 2 to A1 2 O 3 + Fe 2 3 should be 2 J or 3 to 1. That
is, per cent. SiO 2 should equal per cent. R 2 O 3
x 3,
unless working with a siliceous limestone or a stone
of nearly correct proportions which is only deficient
in one constituent.
A high percentage of Fe 2 3 is, for ordinary
purposes, undesirable. Very siliceous materials
produce a slow-setting cement and the mixture

requires burning at a high temperature. Highly
aluminous materials produce an easily burnt clinker,
but the cement is
generally very quick-setting and
otherwise unsatisfactory.
A clay containing nodules of iron pyrites should
be avoided, as a source of possible, if not probable,
trouble.
Calculation from Formulas. Several for-

mulas exist whereby the proportions may be cal-
culated in which raw materials should be mixed,
but even the best of these only serve as a rough
guide in actual practice. From experience
the most favourable data to work upon is
the of CaCO 3
percentage as this can be
,
readily checked and altered. The percentage of

CaC0 3 in a raw mixture never varies greatly from
75 per cent.
In order to obtain approximately the correct pro-
portions, proceed as follows. For example, see
Appendix [3 A].
(1) From per cent. CaCO 3 in limestone deduct 75
or per cent, required in mixture the result should
;
be the weight of clay or shale required.

(2) From 75 or per cent. CaC0 3 required
in
mixture deduct
per cent. CaC0 3 in clay or
shale ;
the result should be weight of limestone
required.
Of
course, the weights so obtained can be read
as grams, lb., cwts., tons, or any unit required. In
each case, when using raw damp material, the
moisture must be estimated and allowed for, as
obviously more will be required than when using
perfectly dry stone or clay.
As a result of researches into the composition of
an ideal Portland cement, various experimenters
have put forward formulas for preparing the raw
mixture when the composition of the materials is
known. The following will be found a good working
formula :
Multiply per cent. Si0 2 in limestone by 2*8

(1) ;
multiply per cent. A1 2 3 in limestone by I'l, and

add the products.
(2) Deduct result from per cent. CaO in stone =
per cent. CaO available for combination with

clay (y).
(3) Per cent. x 2'8 + A1 2 3 in clay x
Si0 2 in clay
1-1, gives CaO required by 100 parts of clay.
Deduct per cent. CaO in clay and remainder =
amount required to be added (x).
As the available CaO (2) in 100 parts of limestone
is known, by simple proportion, parts of limestone
to be added can easily be calculated. Thus let x =
amount of CaO required for 100 parts of clay, and

y = per cent, available in limestone ;
then - - = parts of stone to each 100 parts of clay.
For examples worked out, see Appendix [2A].
ANALYSIS OF SLURRY AND OTHER

RAW MIXTURES
SLURRY. In order to obtain an average
sample of the slurry being washed, the constant
supervision of the chemist or of a trustworthy
assistant is absolutely essential. Owing to different
prevailing conditions, it is impossible to lay down

any fixed plan of sampling. As a rule, samples
should be taken at regular short intervals as the
slurry leaves the grinding plant these should, at ;
longer intervals, be thoroughly mixed and a smaller

average sample taken for examination.
For sampling slurry-mixing tanks or silos various
devices exist, the simplest, perhaps, being a tin can
with a perforated lid the can is weighted at the
:
bottom and attached at the a long pole or

lid to
piece of cord. The body of the can is fitted to the

lid and held firmly by a simple bayonet clip or in
the same way that incandescent electric lamps are
fitted to their holders.
The is lowered into the tank at different
vessel
depths and then slowly raised as it is withdrawn

;
the semi-liquid rushes in through the perforations

and a sample is thus obtained. More elaborate
in many English
apparatus will be found figured
and American works on cement manufacture. A
single sample taken at one depth
should never be
"
used for analysis. A
grain sampler" will be
found
very useful for sampling dry raw meal or cement.

Samples of slurry that have been allowed to
stand, even a short time, must be well shaken
before examination.
(41) Moisture. Into a dry and tared flat-

bottomed porcelain dish weigh out 5 grams of the
well-mixed slurry, place in a hot air oven or on a
hot plate at about 110 to 120 C. until quite dry,
cool in a desiccator and weigh rapidly.
Loss in weight x 20 = per cent, moisture.
(42) Remove the dried material from the dish

with a spatula, powder finely in an agate mortar,
and place in a stoppered weighing tube. Dried
slurry very quickly absorbs moisture, so it is better
to place the powdered material in the oven for a
short time before bottling.
(43) Analysis. Ignite 0*5 gram in a platinum

crucible in the muffle for fifteen to twenty minutes
at a good red heat. Cool in desiccator and weigh.
Loss in weight x 200 = loss on ignition.
(44) Upon the ignited sample carry out the

analysis as described under Limestone, SiO 2 and
Insol. (5 and 6) ;
Insol. (6); A1 2 O 3 + Fe 2 O 3 (7) ; CaO
(8) ; and MgO (11) ;
CO 2 (14) or (15) ;
sulphur and
sulphates (13) ; and (29) if
necessary.
(45) The excess of the

on ignition over the
loss
C0 2 estimated or found by calculation from CaO and
MgO may be stated as "organic matter" without
any grave inaccuracy.
For works routine the following determinations
are of great importance. Moisture (as in 41).
" Fineness."
(46) Weigh out 100 grams of the
wet slurry with fair accuracy, wash it with a gentle
stream of water from the tap into a 180-mesh sieve
especially kept for the purpose. Continue the
washing until the water that runs through is quite
clear. Then wash the residue up together, and
with a wash bottle transfer it to a small evaporat-
ing dish ;
place upon the hot plate or in an oven,
and dry.
Weigh the residue ;
calculate the percentage upon
the dried material thus :
Weight of residue x 100 = cent finenegs

per cent, moisture
With dry meal sift 50 or 100 grams in the usual
way, using 180-sieve, and weigh the residue:
Weight x 2 =
per cent, residue upon 180.
It is sometimes useful to estimate the chalk in
this residue by a rapid method.
(47) Estimation of CaCO 3
. In most works
in Englandthis constitutes the greatest part of the
daily routine, and as the production of a uniform

article largely depends upon the use of a regular
raw mixture, too much time and attention cannot
well be paid to this important item.
Owing to the use of calcimeters, the actual routine
determinations can generally be safely carried out
by untrained assistants who by continual practice
have become proficient in this part of the laboratory
"
work. Constant supervision and occasional check"
estimations by the chemist are necessary with even
the most conscientious workers, in order to keep
them up to the required standard of speedy
accuracy.
There are many good calcimeters on the market,
all more or less inaccurate but when once the error
;
is known, if it be constant, the actual accuracy of

the result is
practically unimportant, as the chemist
in
charge should know at what figure to work
with any given apparatus. Where more than one
machine is in constant use, they should be so regu-
lated as to give strictly comparable results. For
this purpose it is better to
prepare a standard raw
mixture by careful and accurate weighing of the
raw materials after analysis than to use powdered
and dry calcite.
Preparation of a Standard Dry Slurry

(48)
or Raw Meal. Carefully analyse a good sample
of the ordinary mixture that is known to produce
the best results in practice. Then dry a small
sample of each of the raw materials, reduce to the
necessary fineness, and accurately weigh up and
carefully mix in the proportions found by analysis
of raw materials and slurry.
A stoppered bottle of this should always be
kept
ready for use. When a check analysis is
required,
it only necessary to dry a little of the standard

is
slurry in the air oven at 105 C., and allow it to

cool in the desiccator.
(49) Calcimeters may also be standardised, using
dry pure calcitewhich has been powdered in an

agate mortar. With calcimeters upon which it is
usual to take *5 gram of slurry, it is convenient to
take only '375 gram of calcite, which should give a
result equivalent to 75 per cent. CaC0 3 after the
usual corrections.
(50) Slater's Calcimeter. This is an instru-

ment which deserves to be more widely known and
used than at present. It is fairly simple in con-
struction, and can readily be adjusted. It requires
perhaps rather more skilful manipulation than some

others, owing to the necessary alterations of the
amounts used at varying temperatures.
As shown in the illustration, it consists mainly of
two parts, the outer containing vessel A, and the
inner bulb and tube B. Upon the leg of this bulb
are graduations usually running by *5 from 70 to
80, which are read direct as percentages of CaC0 3 ,
as described later.
Above the bulb is a zero mark to indicate the
amount of paraffin with which the instru-
correct
ment has to be filled before use. In the bulb a
small hydrometer float is placed bearing a scale as
shown in the enlarged sketch. The markings refer
to the height of the barometer in millimetres, the
usual markings commencing at 740 and rising to
780 by 2'5 mm. The top of the instrument is

closed by a cork, through which passes a thermo-
meter, dipping well into the mineral oil

and keeping
the bulb in position.
The bulb is attached, by a
FIG. 3. SLATER'S CALCIMETER.
leading tube of glass and a piece of rubber tubing,

to the generator bottle (D). The rubber used
should always be of the same diameter, J inch, and
length 1 foot, between the ends of the glass tube
and generator.
The instrument as sent out generally requires
standardisation. It is used as follows :
(1)Take the reading of the barometer in milli-

metres, and find the nearest corresponding mark on
the float.
(2) Take the temperature of the

oil in degrees C.
(3) Fromthe table (27A) ascertain the correct

weight of material to use in milligrams, and weigh
this out accurately..
(4) Transfer the weighed slurry to the generator

bottle (D), which must be quite dry.
(5) Eun from a burette 5 c.c. of dilute commercial
HC1 (1:1) into the test-tube, attached to the gene-
rator bottle stopper, by means of the hole in the side.
(6) Fit the leading tube from calcimeter to the

bottle, and slip the small piece of rubber over the
outlet hole.
(7)Tip the acid on to the slurry and shake well

to disengage C0 2 The float will then sink in the
.
paraffin, and the mark on the stem which is found

to correspond with the correct barometer reading on
the float should be the percentage of CaC0 3 in the
slurry or material taken.
The instrument may be adjusted by adding a
little oil when the reading obtained is
high, or vice
versd.
By making use of the table given in the Appen-

dix materials higher in CaCO 3 than 80 per cent,
may be estimated (2 8 A).
The following precautions should be observed in
using this apparatus :

(1) holding the generator in the hand

Avoid
than is absolutely necessary, and hold the
longer
neck and stopper of the bottle.
(2) See that the rubber is over the outlet hole
before spilling the acid, and that it is removed
before disconnecting generator.
(3) Spill the acid carefully so that none be forced

up the leading tube.
Use paraffin that has been placed over CaCl 2 and ,
has such a specific gravity that the hydrometer

mark on its stem. Use acid of the
sinks to the red
correct strength.
The and other calcimeters are
Schleibler, Faija,
so well known and have been so frequently described
and illustrated as not to warrant description here.
A modification of Schleibler's instrument introduced
by Mr. H. K. G. Bamber, F.C.S., and much used in

the A.P.C.M. Works, will be briefly described and
illustrated (Fig. 4).
Bamber's Calcimeter. Weigh out

accurately
5 gram of the dried and finely pulverised
slurry
and transfer to generator bottle (14). Eun into
the gutta-percha tube 8 c.c. of hydrochloric acid
(sp. gr. 1-125) and place carefully in bottle. Fill
measuring tubes with water from Woulff's bottle (6),

or reservoir, until water stands at zero mark on the
graduated tube.
Fix stopper to generator bottle and immerse to
the neck in the
running water which fills the lead-
lined wooden vat, until it is at the same temperature
as the water in the tubes 2 and 3. This is so when,
upon opening clip (13), the water in the tubes re-

mains at the same level.
Take the generator bottle in the right hand and
FIG. 4.
cautiously spill the acid in the

tube upon the slurry.
At the same time with the left hand release clip (7),
shake the bottle vigorously for about half a minute,
and replace under water During the
in the nest.
evolution of the gas care must be taken to keep the
level of the water in the plain tube (3) about an inch
above that in the measuring tube (2). Allow to cool
for about three minutes, adjust levels of water, and
take reading. Note temperature of water and also
barometric pressure.
To Calculate Percentage of CaCO 3
. To
calcimeter reading in c.c. add correction
for absorp-
tion of CO 2 by acid. This
may be obtained by per-
forming a check estimation, using Iceland spar or
standard slurry. The figure usually taken for this
instrument lies between 3*5 and 4 '2 c.c. By means
of Table (30 A) Pressure of aqueous vapour in
Appendix note deduction to be givenmade for
temperature from observed barometric pressure.

Refer to Table (31 A), and under the ascertained
temperature find the corrected calcimeter reading
(or nearest) in a line with this, denoted by
;
heavy type, will be found the reading at C.

The figure so obtained is now traced on Table
(32A) under the correct barometric pressure, and
in a horizontal line will be found in heavy type
the percentage of CaCO 3 at C. and 760 mm.
pressure.
"
By means of Table (29A) having performed a loss
on ignition," the calculated CaC0 3 (54) may be
obtained.
Estimation of
(52) 3 CaCO by means
of
Standard Acid and Alkali. The following is
an epitome of a method described by R. K. Meade.
(Portland Cement, p. 231) :
Prepare f N HC1 and f N

NaOH, and standardise
against a standard sample of slurry. The method
of standardisation and working is as follows :
Weigh 1 gram of sample into a 600-c.c. Erlenmeyer

flask and run in 50 c.c. of the standard acid. Close
the flask with a cork bearing a piece of glass tube
30 in. long and f in. diameter, which acts as an air
condenser. Heat the flask until steam just begins
to issue from the upper end of tube. This should
take about two minutes. Remove from heat and
rinse the tube down carefully with water, remove
cork and wash down sides of flask. Add a drop
or two of 1 in 1000 phenolphthalein or methyl
orange and titrate with standard alkali until just
neutral.
If the standard sample contains L per cent, of
CaC0 3 and d c.c. of alkali are required, then to find
percentage of CaC0 3 in other samples it is only
necessary to subtract the number of c.c. of alkali
required in their case from d, multiply by two, and
subtract from L ; if number of c.c. is greater than d,
subtract d from that number, multiply by two, and
subtract from L. Each c.c. of exactly f N
alkali is
equivalent to '02 gram or 2 per cent. CaC0 3 so ;
that, after standardisation, a table may be prepared

showing percentages of CaCO 3 corresponding to
different quantities of alkali. It is necessary to
prepare samples to same state of fineness for each

determination.
(53) Loss on Ignition, Calculated CaCO 3

and CaO in Slurry. When using materials con-
taining organic matter, such as peat, etc., it will
be found very useful to ascertain the CaC0 3 in the
meal after allowing for the organic matter present,
and this may be done as follows. Find the loss
upon ignition of *5 gram dry slurry or meal as
in (43).
Loss in weight x 200 = per cent. C0 2 + H 2 and
organic matter (A).
(54) Calculated CaCO 3

. Calculate the CaC0 3 ,
found upon calcimeter, into C0 2 by dividing thus,

CaCOo x 44
- = per cent. C0 2
1 ^~ (B).
Then,
Loss upon ignition (A) -- C0 2 (B)
= organic
matter (C).
And 100 -- organic matter (C)
= parts of
material in which the CaC0 3 exists after removing
the organic matter by ignition (D).
Thus,
per cent. CaCOo found x 100
- = calculated
j)
CaC0 3 .
The actual calculations only take a few seconds

if the tables in Appendix be used.
The residue obtained after ignition should be
(55)
reserved and the CaO present determined by the
rapid method as described in chapter v. (132);
after allowing for the lossupon ignition the CaO
found should be approximately the same as the
clinker made from this slurry will contain. Owing
to various circumstances, this is not always quite
the case in practice, but this serves as an excellent
check upon the calcimeter or other determinations.
The calculation is as follows :
Per cent, lime in slurry x 100

= calculated CaO.
100 -loss.
(56) Control and Alteration of the Raw

Mixture. Owing to the various systems in vogue
on different works, it is impossible to lay down any
hard and fast rules for the control and regulation
of the slurry or raw meal. The growth of the cement
industry in this and other countries has brought
about the successful use of raw materials differing
so widely in composition as to require in some cases
plant and methods of working of quite a distinct

and special character. Before finally deciding upon
a method of working, the chemist in charge should
assure himself that the routine proposed fulfils the
following requirements :
(1) That there is a regular supply of raw material

sufficient to keep the mills and kilns going con-
tinuously.
(2) That the unit loads of materials are of con-
stant weight or bulk.
(3) That it is possible to readily obtain a sample
of either raw material being used at any moment for
check analysis.
1
(4) That accurate returns of the quantity of

material used be sent to the laboratory at stated
periods, in order that any deviation
from the working
instructions may be at once noted. It is absolutely
essential that a responsible person be in charge of
each mill and be made answerable for any irregu-
larity ofworking either in the feeding or output.
In regard to alteration of the feed of raw
materials, it will generally be found most con-
venient to keep the clay or argillaceous supply
constant, and to vary the chalk or limestone.
The importance of being able to obtain an average
sample of the slurry or raw meal for routine

analysis has already been mentioned. In order
that this work be not interfered with, the samples
should be fetched by a laboratory assistant, marked
for reference; and immediately examined. All re-
sults should be carefully entered up for future
reference.
Before making an alteration in the raw supply at
any mill, the cause of the erratic behaviour should,
as far as possible, be ascertained and noted then ;
the desirability of making a temporary or permanent

alteration will at once be known and acted upon.
Time should be given for the alteration to have
effect before
again checking the output. It is un-
wise to irritate the mill hands by useless and
vexatious alterations and orders.
In working upon the dry system it is best to
keep a silo full of limestone or clay, and work so
as always to require
adjustment in one direction,
For this purpose, either wet or dry process, it is
well to have three tanks or silos for the raw meal :
one to run the make into, one that may be tested

and corrected, and one containing material of the
correct composition. should be impossible for
It
the kiln attendants to use any material but that
passed for use by, the chemist in charge even then
;
the meal, as fed into the kilns, should be regularly

sampled, checked, and the results entered in the
laboratory records. In a word, too much care
cannot well be given to this branch of the laboratory
work.
CHAPTER IV
ANALYSIS OF FUEL, LUBRICANTS,
WATER, AND KILN GASES
THE fuel used chiefly on a cement works is coal or
coke. Brief descriptions only are given of the
chief methods of analysis for fuller description,
;
especially of the calorific value determination, the

inexperienced reader is recommended to consult
larger works.
(57) COAL. In order to obtain an average

sample of the fuel, it is best to have a part of the
freight set apart asit is being unloaded, say one
barrow or grab full in ten, then have this well

mixed and reduced to a convenient bulk by the
method of quartering. When sampling a large
cargo will be found advisable to obtain several
it
samples and carry out check assays.

When not too large, the whole of the sample
brought to the laboratory should be coarsely
powdered and quartered, and the portion selected
for analysis all ground to pass at least the 90 in. -mesh
sieve must be reserved in a well- stoppered bottle
or jar.
56
ANALYSIS OF FUEL, ETC. 57
(58) Moisture. It is well to estimate the

moisture as soon after receiving the sample as
possible.
Weigh into a
weighed platinum capsule '5 or 1
gram of the powdered coal and heat in an air oven
at 105 C. for not more than one hour. Cool in a
desiccator and weigh rapidly, as dry coal is very
hygroscopic.
Loss in weight x 200 (or 100) = per cent,
moisture at 105.
Epitome.
"5 gram in oven at 105 0. for one hour.
(59) Ash. Gently ignite the dried coal over a

bunsen burner or in the muffle, first at a low tem-
perature, until all the carbonaceous matter has
burnt off. The colour of the ash sometimes indicates
its nature.
Cool in a desiccator and weigh.
Total weight weight of capsule x 200 = per cent,
ash.
Epitome.
'5
gram ignited in muffle.
(60) Volatile Matter. One gram of the sample

is placed in a large weighed platinum crucible
having a well-fitting cover. Heat the crucible with
lid on for two minutes over a bunsen burner, or
until no inflammable vapours are emitted, and then
for a further period of three minutes over a blast

burner. Allow to cool in a desiccator, and weigh.
Loss in weight x 100 = volatile matter + moisture
per cent.
Epitome.
One gram heated in closed crucible for two
minutes over bunsen, + three minutes over
blast burner.
In order to obtain concordant and comparable

necessary always to perform this opera-
results, it is
tion in exactly the same manner.
The per cent, moisture (56) subtracted from
volatile matter + moisture will give the volatile
matter.
"
(61) Fixed carbon," or better, fixed carbon-
aceous residue. This is obtained by difference.
100 - + volatile matter + ash) =
per cent, (moisture
"
fixed carbon."
(62) Coke. This is not, as a rule, of great

importance. The residue left after the determina-
tion of the volatile matter is, roughly speaking,
coke. It should be tested to see whether it is
friable or compact.
Coke may be more accurately determined by
placing 1 gram in a covered porcelain crucible placed
in a large Battersea round crucible and surrounded
and packed well in and covered with powdered
charcoal.
The the large pot is luted on with clay, and

lid of
the whole dried and heated in a wind or gas furnace
until it thoroughly hot.
is
After being allowed to cool, the porcelain crucible

and lid is carefully removed, and the coke brushed
out on to a watch glass and weighed.
Weight of coke x 100 = per cent. coke.
Epitome.
One gram heated in covered crucible in furnace.
(63) Sulphur. Mix 1 or 2 grams of the finely-

powdered coal with twice its weight of a mixture
consisting of 1 part dry K 2 C0 3 and 2 parts MgO
in a capacious platinum crucible and cover with a
little more of the fusion mixture place in muffle at a
;
red heat for half an hour, remove, allow to cool,

dissolve and acidulate with E HC1, evaporate to dry-
ness, take up with 10 c.c. of 10E HC1 and a little
water, filter off Si0 2 dilute filtrate somewhat, and
;
estimate S as BaS0 4 (13).
Epitome.
Fuse 1 or 2 grams with K C0
2 3
and MgO mix-
ture.
Dissolve in hydrochloric acid, remove Si0 2 .
Ppt. with barium chloride solution (13).
(64) Analysis of Ash. Ignite 10 grams or

more of the fuel in a platinum capsule until free
from carbonaceous material. Use of this 1 gram or
more, and determine SiO 2 A1 2 O 3 Fe 2 O 3 CaO, and

, , ,
MgO after fusion, as in (17) ; and, if necessary, upon

other portions S0 3 (30) and P2 5 (39).
(65) ANALYSIS OF COKE. The methods

described under Coal may be used for the determi-
nation of moisture (58), ash (59), volatile matter
and fixed carbon (60) and (61), and sulphur (63).
A mixture of MnC0 3 and Na 2 C0 3 may be used
(Neilson's method, Chemical Neivs, April 24, 1891, or
Phillips, p. 125), instead of the mixture used in (63).
(66) CALORIFIC POWER OF FUEL.

For this determination a calorimeter is
required.
One of the simplestLewis Thompson's but one of
is ;
the improved forms of this instrument using oxygen
gas and having electric ignition is more accurate

and satisfactory.
In the ordinary form a known weight (2 grams) of
the fuel is mixed with sufficient finely-powdered
ignition mixture (KC10 3 3 parts, KN0 3 1 part),

placed in the copper cylinder and ignited, when all
is by means of a fuse.
ready,
The cylinder and attachment is
immediately
plunged into 2000 c.c. of water at a known tempera-
ture contained in the special vessel. After combus-
tion the increase of temperature is noted. For
details consult Beringer, Phillips, or the instructions
given with the instrument.

In the improved forms the coal is made into a
pellet and ignited whilst under the water by mjeans
of an electric current.
As a rule each instrument requires the use of

special factors or corrections, but in every case the
result expressed as calories or the number of units
is
required to raise one unit of water through 1 C. ;
generally 1 gram is the unit used. The British

Thermal Unit is Ibs. of water raised 1 F. by 1 Ib.
of fuel.
.-. Calories B.T.U.

x.J'i
_ calories
and p-o
= evaporative power.
537 being the latent heat of steam.
For use in rotary kilns the character of the coal

when burning is of greater importance than the
actual calorific power.
(67) Fineness. This is determined in the same

way as with cement, the 100-sieve being used. To
obtain good results in a rotary kiln the residue should
not exceed 5 per cent., the coal should be quite dry
and low in ash, and easily combustible.
The methods given above can be used for any class
of coal, but it desirable to use a rather higher
is
temperature or heat for a longer period to estimate

the volatile matter in anthracite or steam coal.
"
Concerning the classification of coals, Analysis
of British Coals," Colliery Guardian, may be con-
sulted.
LUBRICANTS. The chief methods of exami-

nation only can be mentioned . If much important
work has done the chemist is recommended to

to be
consult Lewkowitsch's or other large work.
Lubricants may be very roughly divided into three
classes solid, semi-solid, and liquid. Only grease,
fats, or oils will be here dealt with, but it may be
mentioned that graphite, mineral, and compound
lubricants should be free from grit, acid, and alkaline
bodies or substances likely to decompose and produce
acids, &c.
Before reporting on a lubricant it is necessary to
know for what purpose it is intended to be used.
The following tests may be considered essential :
(68) Loss or Gain in Weight on Exposure.

Into a weighed watch-glass place 1
gram of the oil,
and expose an air or water bath at 100 C. for

in
twelve hours. Allow to cool in a desiccator and
weigh.
Loss (or gain) in weight x 100 = percentage loss
(or gain).
Good mineral oils rarely lose more than 1
per
cent. some vegetable oils increase in weight owing
;
to oxidation. The residue should not exhibit any

sticky or gummy properties.
Epitome.
1
gram at 100 for twelve hours.
(69) Specific Gravity. The sp. gr. of oils,

liquid at 15, may be fairly accurately determined
by the hydrometer or Westphal balance.
A specific gravity bottle may be
used for any oil
or fat at any temperature. the bottle with
Weigh
thermometer stopper, which should be pierced or
have a file mark cut to allow excess of oil to escape.
Fillwith previously boiled distilled water at the
temperature to be used. Dry perfectly cool and ;
weigh. The water content of the bottle will thus

be known (A).
By means of a tube or pipette carefully fill the
perfectly dry bottle with oil or molten fat, which
should be at a slightly lower temperature than that
__
at which the determination is to be made. Raise
to the required temperature.
Carefully wipe off excess, allow to cool, and

weigh (B).
Weight
o(B)
\ /
of oil -
Weight of water (A) at same temperature

gravity at stated temperature.
A convenient method to obtain the desired tem-
perature is to place the bottle in a small jar or
copper vessel on a hot-air oven.
(70) Viscosity. This is best determined in a

standardised Redwood viscosimeter. The viscosity
of an varies with the temperature at which it is
oil
determined. According to Phillips, for ordinary

machinery it should be determined at 15, 30, and
60 C. and for cylinder oil at 100, 120, and 150 0.
;
In order to obtain the viscosity of an oil, it is heated

in an air bath to the required temperature, and
poured into the apparatus up to the point of the

The outer vessel, which may be filled with
gauge.
water, any other convenient liquid,
oil, or then is
warmed until both it and the oil to be tested are at

the required temperature. A plug is then removed
and exactly 50 c.c. of oil allowed to runout, and the
time taken in seconds noted by means of a stop
watch. For comparative results consult tables pub-
lished by Redwood and others.
(71) Flash-Point. This may readily be ascer-

tained with Abel's flash-point apparatus. With a
little practice the principles of the determination
can soon be mastered. Full instructions are gene-
rally sold with the apparatus, or can be found

in
the Petroleum Acts or any work on oil analysis.

For oils flashing above 100 C. the air bath is heated
by means of a small bunsen burner or spirit lamp.
The flash-point of an oil should be higher than the
temperature that will be obtained during work.
(72) Free Mineral Acids. Shake up 50 grams

of the oil with water in a stop-
sufficient distilled
pered flask or bottle, and allow to stand for some

time; then separate the oil by means of a separating
funnel. To the aqueous extract add a drop of
methyl orange solution a pink colouration will indi-
;
cate the presence of free mineral acid. If sufficient

in amount, titrate back to the neutral tint with
.
- or - NaOH. The nature of the acid must be

10 100
determined by a qualitative analysis of the extract.
H 2
S0 4 is the acid most frequently found.
Epitome.
Agitate 50 grams of oil with distilled water.

Separate, add methyl orange, and titrate with
N r N M nTT
Na01L
10 Too
(73) Free Fatty Acid. Weigh out 50 grams

of the oil into a flask, and add 100 c.c. methylated
spirit rendered just slightly pink by the addition of
a drop or two of phenolphthalein and one drop of
E NaOH. Shake up together well. If free fatty
acid be present the solution will become colourless.
Titrate with standard

N NaOH until a permanent
pink colouration is obtained.

N NaOH =
One c.c. of '0282 gramoleic, '0256 gram
palmitic, or *0284 gram of stearic acid.

With palm oil use only 5 grams.
Epitome.
Agitate 50 grams of oil with alcohol and phenol-

phthalein solution.
Titrate with standard alkali.
Separation of Fatty and Mineral Oils.

(74)
Saponification equivalent. Weigh out 2*5 grams
of the oil into a strong flask or bottle add 25 c.c. of ;
- standard alcoholic KOH. Place the flask, with

M
the stopper loosely fitted, in a bath of cold water

and cause to boil. As soon as the contents of the
flask are seen to boil, fix the stopper in tightly and
wire it down ; replace in the bath, cause the water
to boil, and allow the flask to remain for about half
an hour, with occasional shaking. Remove from
bath and allow to cool ;
remove stopper and titrate
excess of KOH by means of 2i

HC1, using phenol-
phthalein as indicator.
Ablank experiment is conducted at the same
time, and thus the exact strength of the alcoholic
KOH is ascertained and the amount absorbed by
the oil calculated.
The mean percentage of KOH
absorbed by the
chief fatty oils has been found to be 20*08 per cent.
;
therefore 4*98 parts of fatty oil are saponified by 1
part of KOH. Then number of c.c. neutralised by

oil x 40 x 4'98 x '02805 = approx. per cent, of
oil.
fatty
The saponification equivalent is the number of
grams of oil decomposed by one litre of a normal
alkali (KOH or NaOH solution) ; therefore
2*5 x 2000
-^P 1
= sap. value.
No. of c.c.
Epitome.
Saponify 2'5 grams of oil with 25 c.c. of
KOH.
^
Titrate excess with HC1.
WATER ANALYSIS. The examination of
a water on a works is usually undertaken to ascer-
tain the suitability for use in boilers, &c., rather
than to judge of drinking and domestic
its fitness for
purposes. As a matter of fact, a works laboratory

is rarely suitably equipped or circumstanced to
permit of such an analysis being conducted with any
hope of obtaining reliable results. The processes
necessary to judge of the suitability of water for
drinking purposes are therefore only very briefly
described.
(75) Collection of Samples. Clear glass Win-

chester quart bottles are very suitable for collecting
arid storingwater samples. Before being filled with
the water to be tested, they should be thoroughly
washed until free from all traces of acid, ammonia,
&c., that they may have contained. Bottles which
have been used for acids should be preferred. Before
filling, the
bottles should be washed out well with
the water under examination the stopper should
;
be fastened firmly down with string or wire, and

sealed. It is well to take and keep sealed bottles
of the works water-supply, should there be any
possibility of future contamination by neighbouring
manufactories. Samples of the works outflow and
waste waters should also be kept.
(76) Colour, Odour, Reaction. The colour

can be judged by looking down through a tall glass
cylinder full of the water; tint or turbidity, if any,
should be noted. Odour should be observed ; this
will be more noticeable when the water is gently

warmed, or half a litre of it well shaken in a wide-
mouthed litre flask.
The reaction should be tested by means of a strip
of neutral litmus paper some waters give naturally
;
a slight alkaline reaction. Acidity would most

likely be due to contamination with chemical or
other works waste, although it is sometimes caused
by carbonic acid in solution, which will disappear
upon boiling. Waters passing through a peaty soil
may also give an acid reaction.
(77) Sediment and Suspended Matter.

The character of any sediment or suspended matter
should be noted. If necessary a little may be with-
drawn by means of a glass tube and examined under
the microscope.
The sediment should be well searched for the
lower forms of diatom acere and algse, some of
which cause a water to smell as if contaminated
with dead fish.
great amount of suspended matter may be
Any
estimated by filtration of one or two litres of the
water through a tared filter. The filter and contents
are dried at 100 C. and weighed.
Increase in weight = suspended matter per litre.
The inorganic matter in suspension may be

estimated by igniting the filter and contents in a
crucible recarbonate by adding a drop of ammonium
;
carbonate, and ignite again at a low temperature

and weigh.
Weight ash of filter = insoluble mineral matter

per litre.
Epitome.
Filter 1000 c.c. through tared paper and weigh.
Before proceeding with the chemical analysis it

iswell to ascertain whether to report as grains per
gallon or parts per 100,000. Most engineers will

probably prefer results in grains per gallon. It is
really unimportant, if the report is to be used by

intelligent men, as
only necessary to multiply
it is
grains per gallon by ten and divide by seven or

vice versa with parts per 100,000 to convert one into
the other.
(78) Total Solids. Evaporate 250 c.c. of the

water to dryness in a clean dry platinum or porcelain
weighed evaporating basin, at first over an argand
or bunsen burner, and finally on the water bath.
Allow to cool in a good desiccator and weigh
rapidly, as the solids are often very hygroscopic.
-
Weight weight of dish x 400 = parts per 100,000.
Epitome.
Evaporate 250 c.c. to dryness and weigh.
(79) A qualitative examination may be made of

the solids ;
if a quantitative analysis is required it
will be necessary to evaporate 1000 c.c. or more
of the water to dryness. Estimate SiO 2 ,
A1 2 O 3 ,
Fe 2 O 3 ,
P 2 O 5 CaO, MgO, CO 2 SO 3
, , ,
as in ordinary
analysis. (See paragraphs Nos. 5, 7, 8, 9, 11, 13, 14,
39.) NaCl will be found separately. Na and K may

be estimated or reported by difference. The chief
constituents are CaCO 3 ,
CaS0 4 MgC0 3 MgSO 4
, , ,
and organic matter in solution in the case of peaty

waters.
(80) Chlorine as Chlorides. A standard solu-

tion of silver nitrate containing 4790 grams per
litre will be required ;
also a dilute solution of
potassium chromate free from chloride. Measure

100 c.c. of the water to be tested into a clean flask
and add a drop or two of the chromate solution.
Run in the standard silver nitrate solution until a
permanent orange tint is obtained. To ascertain

the end point needs some little practice, and results
should always be duplicated.
Read off from the burette the number of c.c. of
silver nitrate used.
Number of c.c.= parts per 100,000 of 01.
Chlorine x l'65 = parts per 100,000 of NaCl.
Epitome.
Titrate 100 with standard silver nitrate,
c.c.
using potassium chromate as indicator.
(81) Hardness. The hardness of a water is a

factor of great importance on a works. Hardness
is divided into two classes
"
permanent," mainly :
due to sulphates of calcium and magnesium (and the

other alkaline earths) and " temporary," due to
;
UNIVERSITY
the carbonates of these metals, the latter being

removable by boiling.
(82) Estimation of hardness by standard soap

solution. The following standard solutions are re-
quired. Standard hard water made by dissolving
without loss 0*2 gram of powdered calcite (CaCO 3 )
in dilute hydrochloric acid and evaporating to dry-
ness on the water bath several times until quite
free from acid. The Ca01 2 is then dissolved and
made up to 1000 c.c. with pure distilled water.
One c.c. = "0002 gram of CaCO 3 or 20 parts per
100,000.
(83) Standard Soap Solution. A standard

potassium oleate soap solution may be readily pre-
pared by dissolving 80 grams of pure oleic acid in
" "
proof spirit and exactly neutralising wilh alcoholic
potassium hydrate solution, using a drop or two of
phenolphthalein as indicator. The solution is then
titrated with the standard hard water (82).
(84) Standardisation of the Soap Solution.

Measure 100 c.c. of standard hard water into a
clean glass-stoppered bottle, and run the soap solu-
tion into the bottle a few c.c. at a time until a
lather begins to form then add the soap solution
;
more cautiously, inserting the stopper and shaking

between each addition. When the reaction is near-
ing completion the contents of the bottle will only
give a faint dull sound. Soap solution must be
added until a permanent lather, which persists for
at least two minutes, is obtained. The soap solution
must be then so diluted that the 100 c.c. of water
require exactly 21 to produce a lather, the extra
c.c.
c.c. being required to produce a lather with 100 c.c.

of distilled water.
Suppose the water only requires 16 c.c. of soap,

then every 16 c.c. of the solution must be diluted
with a mixture of about 2 to 1 alcohol and water to
make 21 Rectified spirit or methylated spirit
c.c.
dehydrated over lime and redistilled must be used,

as ordinary methylated spirit produces a ppt. with
water.
of the standard soap solution will thus = 1
One c.c.
of hardness or 1 part of CaC0 3 per 100,000. If 70
c.c.of water are taken, results as expressed in degrees
on Clarke's scale will be obtained, i.e., grain 1=1
of CaC0 3 per gallon.
(85) To ascertain temporary and permanent

hardness of a water. Measure 100 c.c. of the water
under examination into the titration bottle or, if ;
the water is known to be very hard, take 50 c.c.

and dilute with distilled water. Run in the soap
solution cautiously as described until a permanent
lather is obtained ; deduct 1 c.c. from the amount
used ;
then number of c.c. = degrees of total
hardness.
Epitome.
Titrate 100 c.c. with standard soap.
(86) Permanent hardness. Boil, in a flask or

beaker, 100 c.c. of the water down to a volume of
ANALYSIS OP FUEL, ETC. 73
about 50 c.c. or rather less. Allow to cool, filter or
decant, and make up to 100 c.c. again. Titrate

with soap solution as before.
No. of = degrees of permanent hardness.
c.c.
Total permanent = temporary hardness.
Epitome.
Titrate 100 c.c., after boiling, with standard
soap.
(87) Estimation of hardness by Standard Acid

temporary. To 500 c.c. of the water, or less if
very hard, tinted with methyl orange, run in from a

burette
N H SO until a red colouration is
2 4 just
produced.
Number of c.c. used =
parts per 100,000 of
"
CaC0 3 as temporary hardness."
Permanent hardness. To 250 c.c. of the
N
water add 50 c.c. of TT, Na 2 C0 3 solution and boil for
10
about half an hour, or, if magnesium salts be
present, evaporate to dryness.
Filter off the ppt., or extract the residue with
boiled distilled water, filter and wash ;
when cool,
make the filtrate up to 250 c.c.
N
H S0
.
Titrate 50 c.c. of the filtrate with 2 4, using

-T-Q
methyl orange as indicator.

N
Since 10 c.c. of T NaCO 3 was present in every 50
of water, then 10
c.c. number of c.c. of acid used =
number of c.c. of soda removed. Call this x then ;
soda used by the 250 c.c. of water = (x x 5) ;

as 1 c.c.
of
N Na 2 CO 3 = -005 gram of CaC0 3 then (x x 5) x
,
TQ
005 x 400 = parts of CaCO 3 per 100,000 present as
permanent hardness.
(89) Estimation of hardness in a softened

water
or water containing soda. In a water that gives
an alkaline reaction to litmus or methyl orange there
can be no permanent hardness, as carbonates of cal-
cium and magnesium will be pptd. on boiling. Boil
250 c.c. or 500 c.c. of the water, filter off ppt., if any,
wash and make up filtrate to original bulk, titrate
N
whole or aliquot part of the solution with
^H 2 SO 4 ,
and calculate to Na 2 C0 3 parts per 100,000.

Number of c.c. of acid used x 200 (or 400) x
0053 = parts per 100,000 Na 2 C0 3 .
Contamination. To ascertain whether water

is contaminated with sewage or with the products
of animal or vegetable decomposition, it is necessary
to estimate the free or saline ammonia, and the
albuminoid ammonia which is derived from nitro-
genous matter, by boiling with alkaline permanga-
nate of potassium.
The following
special reagents are required. For
full particularsof the process involved a work on
water analysis should be consulted.
The estimation must be conducted under conditions
that admit of no contamination from fumes of am-
monia, &c. The apparatus and distilled water used
must also be quite free from any traces of ammonia
or ammonium salts.
(go) Standard Ammonium CJiloride. Dissolve

3*137 grams of pure ammonium chloride in ammonia-
free distilled water, make up to 1 litre and label as
"stock NH C1 solution."
4
Take 10 c.c. of (90) and dilute to 1000 c.c.
1 c.c. = -00001 gram of NH

3
.
(91) Nesslers Reagent. Dissolve 35 grams of

potassium iodide in about 250 c.c. of distilled water.
Then add gradually a cold saturated solution of
mercuric chloride, stirring constantly until a faint
permanent ppt. is formed allow to stand and decant
;
off. Then add a cool solution made by dissolving

150 grams of caustic potash in 150 c.c. of water. Add
a drop or two of mercuric chloride solution until a
slight ppt. is formed. Dilute to 1 litre and allow to
stand. Decant off a portion into a smaller bottle for
use, and always use a pipette or graduated tube to
measure out the required quantity of solution.
(92) Alkaline Permanganate. Dissolve 200 grams

of caustic potash in about 800 c.c. of ammonia-free
distilled water. Then add grams of potassium per-

8
manganate, allow this to dissolve and boil for a short

time when cool, make up to
;
1 litre.
(93) Estimation of "Free A mmonia." -- Distil

250 c.c. of the water, or less if very contaminated,
using a large flask fitted to a Liebig's condenser in
the usual way. The apparatus must first be well
cleaned and boiled out with ammonia-free water
until the distillate gives no reaction with Nessler's
reagent. The distillate from the water under exami-
nation is collected in a series of Nessler tubes, and
the operation continued as long as a colouration is
produced with 2 c.c. of the reagent (91).

Usually three cylinders are sufficient. To each
add 2 c.c. of the reagent and prepare a similar tube
using distilled water measure into it 1 c.c., or more, of

;
the standard ammonium chloride and then add 2 c.c.
of Nessler reagent. Tubes are thus prepared to match

the tint of each tube of distillate, and the total number
of c.c. of standard ammonium chloride required
noted.
Number of c.c. used x '00001 x 400 = parts of
ammonia per 100,000.
free
The Nessler reagent must always be added to the
ammonium chloride and not vice versd. Instead of a
flask and Liebig's condenser a large retort fitted to a
spherical condenser placed in a bath of water may

be used. Quite 100 c.c. of distillate is collected and
tested against standard ammonium chloride as de-
scribed.
Epitome.
Distil 250 c.c. of water.
Test distillate with Nessler reagent (91).
Albuminoid Ammonia.
(94) To the water re-
maining in flask or retort add 25 c.c. of the alkaline
permanganate (92) and continue the distillation as
long as possible. Then test the distillate as before,

and ascertain number of c.c. of ammonium chloride
solution required to match depth of tint. The
calculation is the same as above.
Epitome.
Add 25 c.c. of alkaline permanganate and re-
distil.
For interpretation of results consult a work on water

analysis. See Appendix 33 A for typical analyses.
(95) Estimation of Oxygen required to oxidise

Organic Matter. A standard solution of potassium
permanganate is required containing 0'395 gram
per litre. Then 1 c.c. = *0001 gram of oxygen.
Into a clean glass bottle or flask place 250 c.c. of

water to be tested then add, from a graduated
;
pipette or tube, 1 c.c. of the standard permanganate

solution and about 10 c.c. of dilute sulphuric acid,
to which has been added enough permanganate to
make it slightly pink. Allow to stand for fifteen
minutes at 15 C. If the pink colouration remains,
the oxygen absorbed is nil if it
disappears, add
;
another c.c. and continue until the colouration is

permanent for one hour.
If the water is likely to use a lot of perman-
ganate solution, take 250 c.c. in flask as before, and

250 c.c. of distilled water in another flask; add
10 c.c. of permanganate and 10 c.c. of the dilute
acid to each, and allow to stand for three hours
1
at the same temperature (15 0.). Then add a drop

or two of potassium iodide solution to the distilled
"
water as check," and titrate with a solution of
sodium thiosulphate containing 1 gram per 1000 c.c.,
using freshly made starch solution as indicator.

Note the number of of thiosulphate required to
c.c.
just remove the blue colour caused by the iodide

and starch. Repeat the titration in a similar way
with the water under examination.
Note number of c.c. of thiosulphate used. As
the distilled water uses up no permanganate, the
equivalent in terms of thiosulphate will be known.
(96) Estimation of Nitrates + Nitrites. The

total solids from 500 of water are taken up with
c.c.
a small quantity of distilled water, filtered, and

washed. The being evaporated to about
filtrate, after
2 c.c., is put into the cup of a nitrometer and then
carefully into the instrument, which must be full

of clean mercury. The beaker and cup are then
washed with a little water which is also allowed to
run into the graduated tube 6 c.c. of 36E
; 2 S0 4
H
free from nitrates are then carefully admitted, care
being taken not to admit air. Any air or C0 2

bubbles which may be produced are carefully driven
out by raising the other limb of the instrument.
The tap is again turned off, and the tube and
contents carefully but thoroughly shaken for about
ten minutes, or until there is no further increase in
the volume of gas collected. Allow to cool, and
then adjust the level of the mercury in both tubes
open tube is about one-tenth of the

until that in the
volume of the liquid above the mercury in the
closed tube. Bead off the volume of nitric oxide
(NO) and note temperature and barometric pres-
sure.
Calculate to volume at 0, and 760 mm. NO
contains halfits volume of nitrogen, so the gas thus
found represents nitrogen in 1000 parts. 1 c.c. of

nitrogen weighs -0012544 gram, therefore :
1 c.c. of N x -12544 = parts of N

(at NTP) per
100,000.
NX 4-5 = HN0 3
.
(97) Estimation of Nitrates using Standard

Indigo Solution.
The following standard solutions are required :
Indigo Solution. Digest 1 gram of pure solid

indigo with 10 c.c. of fuming sulphuric acid for
several hours on a water bath until all is dissolved.
Make the solution up to a volume of two litres with
distilled water.
Standard Nitrate. Dissolve 1'603 grams of pure

KNO 3
in one litre of distilled water. This contains
the equivalent of 1 gram per litre of HN0 3 ; for use
dilute ten times then ;
1000 c.c. = O'l gram HNO 3 .
To standardise Indigo. Take 10 c.c.

of the
dilute nitrate solution and 10 c.c. of distilled water
in a flask, add 20 c.c. of pure 36E H 2 S0 4 free from
nitrates, and immediately run in from a previously
filledburette the indigo solution, a few drops at a

time, until the first brown tint begins to become
darker, when the addition may be hastened. The
reaction complete when the solution assumes a
is
decidedly green tint, which is best seen upon dilu-

tion. With a little practice the end tint is soon
recognised.
-r
used
y = strength of indigo per c.c.
No. ot c.c.
To estimate Nitrate in Water. Take 20 c.c. of

the water and 20 c.c. of 36E H 2
SO 4 and titrate as
described. If the water contains more than 10
parts of HN0 3 per 100,000,
use 10 c.c. and dilute to
20 c.c. with distilled water.
No. of c.c. used x factor x 50,000 = parts per
100,000 of HN0 3
.
The indigo shouldoccasionally be checked, as it

deteriorates after a time. An estimation can be
carried out in less than five minutes.
(98) Poisonous Metals. A drinking water should

always be tested for lead, copper, etc., by passing
H S gas through a quantity of
2
the water contained
in a clear glass vessel. No dark colour should be
produced. If present, lead may be estimated by
evaporating several litres of the water to a small

bulk, acidifying slightly with hydrochloric acid and
ppt. with H S. 2
Filter, wash, convert into PbS0 4 and weigh or , ;
lead may be estimated colorimetricaliy by comparison

of the depth of tint produced by adding H 2
S to
a known amount of water, and also to a standard
dilute solution of lead nitrate.
Epitome.
Pass H 2
S through at least 1 litre of water.
Estimate as PbSO 4 or colorirnetrically.
Water softening. Many systems of water

softening are in vogue they are nearly all based
;
upon the removal of carbon dioxide and consequent

precipitation of calcium carbonate by means of lime,
or precipitation of carbonate and sulphates by means
of soda ash (Na 2 C0 3 ) or caustic soda (NaOH).
The following are the principal reactions in-
volved :
(1) CaC0 3 + C0 2 + Ca(OH) 2 = 2CaCO 3 + H 2

(2) MgC0 3 + C0 2 + 2Ca(OH) 9 =
2CaC0 3 + Mg(OH) 2 + H 2 O
(3) CaS0 4 + Na 2 CO 3 = CaCO 3 + Na 2 SO 4
(4) MgS0 4 + Ca(OH) 2 + Na 2 C0 3 =
CaC0 3 + Mg(OH) 2 + Na 2 S0 4
(5) CaC0 3 + 2NaOH = Ca(OH) 2 + Na2 CO 3
(6) CaSO 4 + 2NaOH = Ca(OH) 2 + Na 2 SO 4
The following illustrates the method of calcu-
lating the amount of lime required per 1000 gallons,
the CaC0 3 present being known from the temporary
hardness or by analysis of the total solids :
CaCO 3 + CO 2 + CaO = 2CaCO 3

100 + 56
100 parts of CaCO 3 requires 56 parts of quick-
lime (CaO).
The water has say 15 parts of CaCO 3 per 100,000.
1000 parts of water contain "15 of CaCO 3
. 56X-15
therefore require
.*. 56 x -15x70 . ,,
= grains CaO
-
-
of per gallon.
00
56 x -15x70x1000
-=
grams of CaO per 1000 gallons,
or 56 x -15 x 700 = 5880 grains ;
-
there are 7000 grains per Ib. (16 oz.) ^ QQQ
= oz. per 1000 gallons or as one equation.
;
56 x degrees of hardness x 16
1000
In actual calculations the percentage of CaO in the
lime used must be known (140) and allowed for.
Slaked lime is always used in practice ; the equation
then becomes
74 x degrees of hardness x 16 = oz. of Ca(OH) 2
1000
per 1000 gallons
_ 74 x hardness x 16 x 100
1000 x per cent, of Ca(OH) 2 in lime
= oz. per 1000 gallons of slaked lime required.
As the amount of C0 2 in the water always largely
exceeds that required to keep the CaC0 3 in solu-
tion, the above calculation will only give approxi-
mately the amount of lime to be actually used.

The following method of ascertaining the amount
of lime (CaO) required per million parts of an

ordinary water is taken from a paper by Mr. W. D.
Collins in the Engineering Record, February 16,
1907 (U.S.A.):
(99) Excess o/C0 2 . Titrate 100 c.c. of the water
with Na 2 C0 3 solution free from bicarbonate,

ou
using phenolphthalein as indicator.
No. of c.c. used x 10 = CaC0 3 equivalent of
CO 2 (a).
(100) Temporary hardness. Titrate 100 c.c. of
the water with

ou
H S0 2 4
in a 200-c.c. graduated
flask,using methyl orange as indicator.

No. of c.c. used x 10 = parts per million of
CaCO 3 (6).
(101) Magnesia. Heat to boiling in the 200-c.c.

flask the neutralised water (100); boil for fifteen
minutes, add 25 c.c. of saturated lime water. Make

up to 200 c.c. at temperature of room. Filter into
a graduated cylinder, reject first 50 c.c., titrate next
N
100 c.c. with ^r
ou
H S0
2 4, using methyl orange as
indicator.
Repeat, using distilled water.

Difference = amount of 2 SO 4 H
which has been
neutralised by Ca(OH) 2 required to ppt. MgO.
This No. of c.c. x 20 = parts per million of CaC0 3
equivalent to magnesia (c).
(102) Permanent hardness. Boil 250 c.c. of the

.
N
water in a porcelain dish. Add 25 c.c. of
^TT
soda
reagent (equal parts Na 2 CO 3 NaOH), and boil for ,
ten minutes. Filter, make up to 250 c.c., and titrate

N
100 c.c. with H 2
S0 4 .
Repeat, using distilled
water. Difference in number of c.c. of H S0 2 4
re-
=
quired soda reagent used.
This number x 10 = parts per million of CaCO 3 as
permanent hardness (d).
(103) Then a + b + cx '56 = parts per million of

CaO required to soften water.
d x 1*06 = parts per million of soda required to re-
move permanent hardness.
GAS ANALYSIS. Collection of Samples.

A sample
of rotary kiln or furnace gas can best
be obtained at the base of the shaft. For this
purpose a brass or copper tube sufficiently long
is introduced through an eye-hole or an opening
especially made.
The length of tube inserted in the furnace should
have holes pierced in the sides in order to obtain
a sample of the gas from as many different points
as possible.
In order to prevent corrosion by acid gases, the
tube may be dipped in a strong solution of borax
and dried upon becoming heated the borax fuses
;
and forms a protective glaze. Aspirators of metal

or glass may be purchased, but for ordinary use a
very effective one can be easily constructed from a

Winchester quart bottle as follows :
(104) Fit the bottle with a sound cork or rubber

bung pierced with two holes. The cork is fitted
with two glass tubes bent at right angles, one
being sufficiently long to reach to the bottom of
the bottle, the other only just passing through the
cork.
When the apparatus is to be used a glass or rubber
tube sufficiently long to reach below the level of
the bottom of the bottle is attached to the longer
interior tube, the bottle is filled with water and
suction applied to this tube the water is thus
;
syphoned off, and the gas enters the other tube and
fills the bottle. The rate of aspiration may be
regulated by placing a screw clamp on the rubber
connection. Bypreparing a number of bottles
fitted in a similar way, but the glass tubes bearing
glass stop-cocks, any number of samples of gas may

be obtained with the use of one aspirator.
(105) The apparatus is fitted up as fpllows

Place the sampling tube in the flue to the end
;
obtruding attach a wash bottle or a dust trap con-

sisting of a tube loosely packed with asbestos or
cotton wool connect this to the sample bottle and
;
that in turn to the aspirator, making sure before-

hand that all connections and stoppers are absolutely
gas tight. Before sealing off and disconnecting the
sample bottle, aspirate at least twice its volume of
gas through the apparatus in order to remove air
and to saturate the wash water with the gas under

examination.
Analysis of Gases in the Hempel Apparatus. In

kiln or furnace gas it is necessary to estimate the
following constituents when present : Carbon di-
oxide, carbon monoxide, oxygen, nitrogen, and

hydrocarbons. For a description of the apparatus,
mode of fitting together, and other details Hempel's
Gas Analysis should be consulted.
The following solutions for absorption are re-
quired :
(106) For Carbon Dioxide. Dissolve 160 grams

of KOH in 130 c.c. of distilled water.
(107) For Oxygen. Dissolve 10 grams of pyro-

gallol in 200 c.c. of potash solution (106).
(108) For Carbon Monoxide. Dissolve a mixture

of 86 grams of copper oxide (CuO) and 17
grams of
copper filings in 1086 grams (969 c.c.) of hydro-
chloric acid of sp. gr. 1'124,
adding the mixture to
the acid slowly with frequent stirring. Store in a
bottle containing metallic copper.
(109) Filling the Connect a piece of

Burette.
capillary glass tube to the top of the measuring
tube of the burette by means of a
piece of stout
rubber tubing, which should carry a
clip and be
wired on. Fill the pressure tube with water satu-
rated, if possible, with the gas under examination ;
raise the tube, thus
causing the water to enter the
measuring tube until it issues from the capillary
tube. Close the clip and connect to the aspirator
by means of another piece of short rubber tube.
All rubber connections should be wired on. Lower
the pressure tube and open the clips until the gas to
be analysed is drawn in and rather more than 100
c.c. are contained in the measuring tube.
Close the clips and disconnect from the aspirator,
which must, of course, be again securely sealed up.
Now close the long rubber tube between the pres-
sure and measuring tubes. liaise the pressure tube
and open the clip to allow water to flow into the
measuring tube until it just reaches the graduation.
Again close the clip on the connecting tube and
open the top of the measuring tube excess of gas
;
will escape, and exactly 100 c.c. will remain at
atmospheric pressure ; close the clips.

For technical work it is not necessary to note
barometric pressure or temperature, provided they
do not alter during the examination.
(HO) Estimation of Carbon Dioxide. Fill an

ordinary absorption burette with the potash solu-
tion (106) by means of a funnel attached to the tube
connected with the reservoir bulb. Then, by means
of suction, draw the solution into the other (absorp-
tion) bulb until it almost completely fills the capillary

tube ; thus practically all air is excluded from the
apparatus. Such an amount of reagent must be
used that be contained by the reservoir bulb
it will
when it is driven back by the gas from the pipette.

Having filled the burette, note the position of the
reagent in the capillary tube and bring it to the

same position between each reading. Attach the
pipette by means of the connecting capillary tube
and rubber joint.
Open the pinch-cocks and raise the pressure tube,
thus causing the gas to enter the burette. Allow
the water to fill the
connecting capillary tube, close
the pinch-cocks, and gently shake the contents of the
burette in order to present a larger surface of the
reagent to the gas. Allow to stand for at least five
minutes. Cause the gas to return to the pipette by
lowering the pressure tube, adjust the level of the
water, allow to stand for a few minutes, and then
read off the volume of the gas. Repeat the operation
until a constant volume is obtained.
100 --
reading
= volume of carbon dioxide per
cent.
Epitome.
Treat 100 c.c. with potash solution in gas pipette.
(111) Estimation of Oxygen. The pipette is re-

"
placed by a double" one containing alkaline pyro-
gallate solution (107), and the absorption process
repeated.
Diminution in volume = oxygen per cent.
(112) Estimationof Carbon Monoxide. The

pipette is
replaced by one containing acid cuprous
chloride (108), and the absorption process repeated.
Diminution in volume = carbon monoxide per

cent.
(113) Nitrogen. The residual gas is generally

taken as consisting of nitrogen, and this is the case
when the furnace is working properly. Should there
be an insufficient supply of air, there may be hydro-
carbons or hydrogen present.
(114) Estimation of Combustible Gases. About

30 c.c. of the residual gas are made up to 75 c.c. with
oxygen, and the exact volume noted. The mixture
is then fired in an
explosion pipette or eudiometer
by means of an electric spark. The contraction in
volume is noted and the gas passed into the pipette
containing potash solution (106), which absorbs the
CO 2 formed, and the volume again noted.
The volume of hydrogen and methane may be
calculated as follows :
Let x = contraction due to firing.

y = after absorption of CO 2 .
Vol. of hydrogen equals f (x Zy)

methane equals y.
The percentage is then calculated as follows :
Vol. of hydrogen or methane x

Vol. of residual gas .
x 100
Vol. taken for combustion
(115) Analysis with the Orsat Apparatus. This

is a portable apparatus consisting of a measuring
burette and absorption pipettes, which are filled with
the usual reagents. Some forms of the apparatus
also have a palladium tube for the determination of
the combustible gases. According to Hempel, there

are several sources of inaccuracy.
Full instructions are usually supplied with the
instrument. It is a convenient apparatus for con-
trol work.
(ll6) To determine Conditions q/ Combustion

in
a Hotary Kiln. Let N
= total per cent, of nitrogen
found by analysis, and = total per cent, of oxygen
found by analysis.
The amount of nitrogen (N x ) corresponding to
amount of air really useful in combustion is N a =
nitrogen 376 oxygen.
Without calculating the amount of air itself, we
can obtain a ratio between the air introduced and
the air used, thus :
100 N
N^- 376 oxygen
gives a value either more or less than 100. If a

ratio above 100 is found, it shows that excess of air
is being used, and vice versd, in which case com-
bustible and reducing gases will be found. In a

rotary kiln there should always be a slight excess of
oxygen to prevent the formation of ferrous com-
pounds in the clinker.
The above calculations are from vol. iii. Geo.
Survey Ohio, by Professor Orton.

CHAPTER V
CEMENT ANALYSIS
(117) Accurate Methods. Weigh out into a
6-in. flat porcelain or platinum dish 0'5
gram of the
cement. Add a little distilled water, and rotate
the dish to prevent setting; then add 25 c.c. of
pure 10E HC1, place on a sand or water bath, and
evaporate to dryness. Cover with a clock glass, and
bake on a hot plate at a temperature of 200 C. for
at least one hour. Remove from hot plate, and
allow to cool. Add 25 c.c. of 10E HC1 and about
the same amount of water, warm for a few minutes
on the sand or water bath until the insoluble matter
is quite free from iron compounds. Filter through
a 12'5-cm. black band filter paper, wash by decanta-
tion, remove every trace of silica adhering to the
dish by means of a rubber- tipped glass rod. Wash
with hot water until quite free from chloride. Re-
turn the filtrate to the dish, and again evaporate to
dryness on the sand bath.
Take up with 25 c.c. 10E HC1 and water, digest
if necessary, filter off any trace of silica through a
9 -cm. paper, and wash well. Dry and ignite the
91
two residues together for at least one hour in a good

muffle furnace.
Weight ash of filters x 200 = silica + insolu-

ble.
(118) Alumina and Ferric Oxide. Eeturn

the filtrate from (117) to the evaporating dish, add
a drop or two of bromine water, and bring nearly
to the boiling-point over an argand burner or on
a hot plate. Cautiously add a slight excess of
10E NH 4 OH, and gently heat until nearly all the
excess of ammonia has been driven off. Filter
through a 15-cm. black band paper, using a "cut

"
funnel wash slightly, and collect the filtrate in a
;
large Phillips beaker. Pierce a hole in the filter
paper and wash the ppt. back into the original

dish. Without removing paper from the funnel,
drop on to it 15 c.c. of 10E HC1, and wash down
into the dish with about 20 c.c. of hot water. Re-
precipitate the alumina and iron oxide as before,
filter, and wash thoroughly and rapidly, well churn-
ing up the ppt. Dry, and ignite in muffle for one

hour, cool in desiccator and weigh.
Weight
-- ash of filter x 200 = per cent, of
A1 2 O 3 + Fe 2 3 .
(119) Lime (CaO). Evaporate the filtrate (118)

somewhat, if necessary, and heat nearly to boiling ;
add about 20 c.c. of 5E NH

4 OH,
boil and add at
TT
least 30 c.c. of boiling ammonium oxalate solution,
o
and continue to boil for five minutes. Allow to
CEMENT ANALYSIS 93
stand in a warm place, if possible, for at least one
hour. Filter through a Swedish or white band
15-cm. paper and wash. The filtrate and first
washings are reserved for MgO determination (121).

Continue the washings until a drop of the filtrate
does not discolour an acidified very dilute solution
of potassium permanganate. Estimate CaO by
means of standard solution of permanganate, as
described in (9) ;
or as CaSO 4 (10).
(120) For very accurate work ignite the wet.ppt.

in a platinum crucible over a small bunsen burner.
Place in a large beaker, dissolve ppt. in redistilled
10E HC1, dilute with 150 c.c. of water, warm, add
slight excess of 10E NH 4 OH, filter off any traces
of alumina, reprecipitate with ammonium oxalate,
and estimate the CaO as before, or ignite in good
muffle to constant weight.
Weight of CaO - filter ash x 200 = per cent. CaO.
(121) Magnesia (MgO). The filtrate or filtrates

from (119) are evaporated nearly to dry ness in the
large dish. Add 30 c.c. of pure 16E 3 evapo-HNO ,
rate to dry ness, and continue heating on the hot plate

until all ammonium salts are volatilised. Remove
from plate and dissolve residue in 5 c.c. of 10E HC1
and about 20 c.c. of distilled water. Add one drop
of bromine water and slight excess of 10E NH 4 OH,
boil carefully for a few minutes and then filter off
any ppt. through a 5 -cm. black band paper. If not

exceeding 0'002 gram, ignore. Collect filtrate in
a 200-c.c. beaker, add 10 c.c. of 20E NH OH and

4
2E
5 c.c. of -^-
o
Na 2 HPO 4 solution. Stir well with a
rubber-tipped rod, and allow to stand in a cool

place over night.
Filter through a 7 or 9 cm. filter paper, wash by
decantation, using 5E 4
NH OH
then transfer ppt.
;
to the paper, remove by means of the rubber-tipped

glass rod any particles adhering to the sides of the
beaker, and continue to wash until free from
chlorides. The ppt. may be ignited while moist in
a platinum or porcelain crucible in the muffle furnace
or over a good burner for half an hour. Cool in a
desiccator and weigh as Mg 2 P 2 O 7
.
40
Weight of ppt. x r
T
x 20() =per cent, of MgO
(see Appendix, 25A). The ppt. before washing may be
dissolved in a little warm water and a drop of hydro-
chloric acid, and repptd. by addition of 1 c.c. of
o"P
-- Na 2 HPO 4 and excess of ammonia.
(122) Alkalies. These are generally estimated

by difference they may be estimated directly by
;
the Lawrence Smith method as described under

Clay
(31), or as follows.
Treat one gram of cement in a
large platinum
dish, as for ordinary analysis for estimation of Si0 2 ,
RO2 3, CaO. Evaporate filtrate from CaO deter-

mination to dryness in a platinum dish carefully.
Ignite residue until free from ammoniacal salts, cool,
then add 5 c.c. of water and brush in about 1
gram
CEMENT ANALYSIS 95
of powdered oxalic acid crystals. Evaporate care-
fully to dryness and ignite as before. Treat the
residue with about 20 c.c. of hot distilled water,
filter, and wash ;
residue consists of MgO and may
be weighed as such.
The filtrate is made acid with 10E HC1 and
evaporated to dryness very carefully in a weighed
platinum dish. Cool in a desiccator and weigh.
Weight = NaCl + KCl.

Na 2 O and KO2 can then be estimated as under 31 A.
Epitome.
Separate Si0 2 A1 2 O 3 Fe 2
, , 3, CaO.
Evaporate to dryness, add oxalic acid and water,
evaporate to dryness, take up with water, filter and
wash. Acidify filtrate with hydrochloric acid and
evaporate.
Separate KC1 and NaCl by means of platinum
chloride (see 31 A).
(123) Ordinary Method of Analysis for

Technical Purposes. Si02 and insoluble.
Weigh out 0*5 gram of cement into a 6 -inch porcelain
dish, add a little water, swirl round, and add 25 c.c.
10E HC1. Evaporate to dryness on hot plate, cover,
and bake for one hour. Remove from hot plate,
and when nearly cool take up with 25 c.c. 10E HC1
and water. Digest, if necessary filter off Si02 + ;
insoluble, clean dish, well wash, ignite and weigh.
Weight x 200 = per cent, silica and insoluble.

(124) AI Z
39
Fe 2 O3 .To filtrate from (123) con-
tained in the large dish add a drop or two of
bromine water and slight excess of 10E 4 NH OH ;
boil off excess of ammonia, filter through a

gently
black band rapid paper, wash well, ignite and weigh
=
Weight x 200 per cent. A1 2 3,
Fe 2 O 3 .
(125) CaO.Boil filtrate from (124) in a large

Phillips beaker, add slight excess of ammonia and
^T?
50 c.c. of boiling ammonium oxalate, boil for
o
three minutes, allow to stand for half an hour, filter,
wash well, and estimate by means of standard
permanganate (9).
(126) Evaporate filtrate from (125) nearly to

dryness, add 30 c.c. of 16E HN0 3 and drive off
ammonium compounds. Take up with a few drops
of hydrochloric acid and a little water. Add
slight excess of ammonia, filter off any ppt., to
9TT
filtrate add 10 c.c. 10E NH OH 4
and 5 c.c. of
3
Na 2 HPO 4 ,
stir well or shake in a stoppered bottle
vigorously, allow to settle, filter, wash with 5E

NH 4 OH, and weigh as Mg2 P O
2 7 (25A).
40
Weight x x 200 = per cent. MgO.
Epitome.
Treat 0'5 gram cement with 25 c.c. hydro-
chloric acid, and evaporate to dryness. Bake
one hour, allow to cool, take up with 25 c.c.
CEMENT ANALYSIS 97
hydrochloric acid. Filter, wash, and ignite,

weigh = SiO 2 4- insoluble. Ppt. A1 2 O 3 Fe 2 O 3 ,
with ammonia. Filter, wash, ignite, and
weigh = A1 2 O 3 Fe 2 O 3
, To filtrate add
.
boiling ammonium oxalate + ammonia.

Filter, wash, estimate = CaO. Evaporate
filtrate nearly to dryness, add 30 c.c. nitric
acid, drive off all Am. salts. Dissolve in dilute

hydrochloric acid, ppt. and filter off traces of
Al 2 O 3 ,Fe 2 O 3
;
ignore ppt. To filtrate add
ammonia + sodium phosphate, agitate, allow
to settle, filter, wash with 5E NH 4 OH, ignite
and weigh as Mg 2 P 2 O 7 ;
calculate to MgO.
(127) Insoluble Residue. Weigh out into a

5 -in. flat porcelain dish 0*5 gram of cement. Add a
water and rotate to prevent setting
little distilled ;
then add 10 of 10E HC1 and place on the hot

c.c.
plate for ten minutes or a quarter of an hour. It is

not essential that the contents of the dish should be
evaporated to dryness, but it is preferable to do so,
if time permits.
Add, in either case, 10 c.c. of 10E HC1 and about

25 c.c. of water, allow insoluble matter to settle,
filter through a 9-cm. black band paper, wash at
least three timesby decantation, allowing as little of
the insoluble matter as possible to leave the dish.
Finally, wash back into the dish any particles
adhering to the filter paper without removing latter
from the funnel. The filtrate is used for estimation
of SO 3 (128). To the contents of the dish add
10 c.c. of 3E Na 2 G0 3 solution and boil for ten

minutes. Filter the paper pre-
rapidly through
viously used, and wash with boiling
water until a
drop of the filtrate leaves no residue upon evapora-
tion. Dry, ignite, and weigh.
- filter ash x 200 = per cent, insoluble
Weight
residue.
The weight so obtained is subtracted from the
total Si0 2 and insoluble residue (123).
Epitome.
Treat 0*5 gram with warm
hydrochloric acid.
Filter, wash by decantation.
Boil residue with 10 c.c. sodium carbonate
solution.
Filter, wash, ignite, and weigh.
(128) Sulphuric Anhydride (SO 3 ). Boil in a

10-oz. Phillips beaker the filtrate from (127), and
whilst still
boiling add drop by drop 10 c.c. of
E BaCl 2 solution ;
after five minutes allow to
settle in a warm two hours, if
place for at least
possible. Filter through a 7-cm. No. 417A Max
Dreverhoff paper, wash with warm water until quite
free from chloride. Dry, ignite, and weigh as
BaS0 4 The damp paper may be placed in the
.
mouth of the muffle furnace and ignited therein

afterwards with out much fear of an inaccurate
result.
on
Weight of BaS0 4 x * 200 = per cent. S0 3 .
CEMENT ANALYSIS 99
Epitome,
Precipitate with barium chloride solution.

Wash, ignite, and weigh as BaSO 4 .
(129) Sulphur as
Sulphide. Sulphides, if
present in sufficient amount, may be estimated by
the following method. Treat 0'5 or 1 gram of
cement with a little water in the usual way, then
add 25 c.c. of 16E HNO 3 warm and evaporate ,
gently to dryness, allow to cool, and take up with

10 c.c. of 10E HC1 and water. Filter off silica and
wash.
To the filtrate add 10 c.c. of E BaCl 2 solution and
treat as in (128). From the weight of BaSO 4
obtained deduct the equi\r alent found when esti-
mating SO 3 The excess BaSO 4 x 0'137 x 200 (or
.
=
100) per cent, sulphur as sulphide.
Epitome.
Treat with nitric acid, evaporate, take up with
hydrochloric acid, filter and wash.
To filtrate add BaCl.2 solution, filter, wash, weigh
as BaSO 4 .
The sulphur found as sulphide may be calculated

to calcium sulphide,CaS, thus :
Weight x 0-30895 x 200 - CaS,

of BaS0 4
in which case the equivalent must be deducted from
the lime (CaO) found. One per cent, of CaS = 0'78
per cent. CaO. In like manner S0 3 may be con-
verted into CaS0 4 .
Weight of BaSO 4 x x 200 = CaSO 4 .
*||
For each 1
per cent, of CaSO 4 deduct 0'41 per cent,
from the CaO found.
(130) Loss on Ignition. 0'5 gram is

ignited in
a platinum minutes in a muffle
capsule for ten
furnace. The temperature should not exceed 800 C.,
or there will be a loss of S0 3 .
Loss in weight x 200 = loss on ignition (CO 2 + 2 0). H

Carbon Dioxide. If necessary this may be
estimated by treating 5 grams with hydrochloric
acid in the absorption apparatus as described in (14).
(131) R. K. Meade (Portland Cement) recom-

mends the use of a Shinier crucible. This consists
of a platinum crucible provided with a water-
jacketed stopper and reservoir for supplying water
to the latter. From 1 to 3 grams of cement are placed
in the crucible and covered with ignited asbestos.
The crucible is heated by means of a bunsen burner
water through the stopper.
after starting a flow of hot
The gas aspirated through potash bulbs and
is
calcium chloride tubes in the usual way. Finally

the crucible is heated over a blast burner. The
absorption apparatus is weighed increase of weight ;
equals C0 2 If the cement contains any unburnt

.
carbonaceous material this causes an error. The

carbon may be estimated by treating the cement
with acid, filtering through asbestos, and then
igniting residue in the crucible. For details see
work cited.
CEMENT ANALYSIS
(132) Rapid Method for Estimation of Lime
in a Cement. Weigh 0'5 gram of cement into a
dry wide-form 800-c.c. beaker, add about 10 c.c. of

distilled water, and rotate to prevent setting, then
add 20 c.c. of 10E HC1. Warm until solution is com-
plete. Dilute to about 250 c.c. with warm water,
boil for a few minutes, then exactly neutralise with
10E NH OH, using methyl orange as indicator.
4
To
^TT
the boiling solution add 10 c.c. of (concentrated)
oxalic acid solution, boil for one minute, then add
3E
70 c.c. of ammonium oxalate solution. Boil
5
for seven minutes, remove from heat, allow to settle,
and through a 15 -cm. black band paper.
filter
Wash several times by decantation, using plenty of

hot water then transfer to filter paper and wash
;
until a drop of the filtrate acidified with sulphuric

acid will not decolourise water faintly tinged with
permanganate. About 700 c.c. of wash water will

be required with practice, always using the same
;
quantity of reagents, one can readily gauge the

amount of warm water to use.
Remove the filter from the funnel, open and lay
against the sides of the beaker in which precipitation
was made. Wash ppt. from the paper into the
beaker. Add 30 c.c. or sufficient 5E 2 S0 4 warm, H ,
titratewith standard permanganate, of which the

strength in terms of CaO is known.
No. of c.c. used x factor x 200 = CaO.
102 CEMENt CHEMISTS' HANDBOOK
(133) The permanganate is best standardised
against pure Iceland spar, taking a known weight of
spar and following through the process described
(132). A
convenient strength is obtained by using
6-7 grams of permanganate per litre.
ANALYSIS OF GYPSUM, PLAS-

(134)
TER, KEENE'S CEMENT, Etc. All these
bodies consist of calcium sulphate in one form or
another. The necessary estimations include silica +
insoluble matter, alumina and iron oxide, lime, mag-
nesia, sulphuric anhydride, and water.
(135) Silica and Insoluble. Weigh out into

a porcelain or platinum dish 1 gram of the finely
powdered material. Add a little water and rotate
to prevent setting. Add 10 c.c. 10E HC1 and
evaporate carefully to dryness. Take up with 25 c.c.
of 10E HC1 and water. Digest, if necessary ;

filter
off through a small filterpaper any insoluble matter,

wash well, dry, ignite, and weigh.
Weight filter ash x 100 = per cent, insoluble.
(136) Make the filtrate up to 500 c.c. and divide

into two parts of 250 c.c. each.
Alumina + Ferric Oxide, Lime, and Mag-

nesia. In one portion estimate A1 2 O 3 Fe 2 O 3 CaO, , ,
and MgO by the ordinary methods.
(137) Sulphuric Anhydride. Place the other

portion of 250 c.c. in a fairly large beaker and bring
to the boil whilst gently boiling, add 20 c.c. of
;
CEMENT ANALYSIS 103
E BaCl 2 drop by drop. Allow ppt. to settle, filter,
wash, ignite, and weigh.

-
Weight filter ash x '34291 x 200 = per cent. S0 3 .
This may be converted into CaSO 4 as shown under

(129).
(138) Water. Ignite 0*5 gram in a platinum

crucible in the muffle at a temperature of about
400 C. for twenty minutes. Care must be taken to
avoid loss of SO 3 or reduction to sulphide.
Loss in weight x 200 = per cent. H
2 0.
(139) ESTIMATION OF CAUSTIC

LIME (CaO) IN BURNT LIME. The
material under examination should be
sampled,
crushed, and finely powdered as rapidly as possible.
The original sample should be stored in an air-tight
and the portion
receptacle, for analysis placed in a
dry weighing tube.
(140) Estimation of CaO. Transfer about 0*5

gram of the finely powdered sample into an Erlen-
meyer flask containing about 250 c.c. of air-free dis-
tilled water. Boil gently for five minutes, close tne
flask with a cork bearing a soda-lime tube, and allow
to cool. When titrate with

N
-~~
quite cold, HC1,
using phenolphthalein as indicator allow the flask

;
to remain some time to see if the pink colouration

returns.
No. of c.c.used x '0028 x 100
" = P er cent ' Ga -
weight taken
APPENDIX
APPENDIX
EXAMPLES OF CALCULATIONS
OCCURRING DURING ANALYSIS
(!A) Clay Analysis. Conversion of insoluble
into felspar (21).
Found. Insol. 12 '8 8 per cent, containing 171
per cent. RO
2 3
"
then 171 x 3'5 = 5 '98 per cent. SiO 2

171 x 0-6 = 1-02 Na 2
+ TiO 2 found 24
+ R2 O 3 ,, 171
8-95
12*88 -- 8-95 = 3-93 percent, of quartz.
Report as follows :
SiO 2 = 5-98
=5-98
A1 2 3
= 171 -felspar
Insoluble matter 12 '8 8 Na 2 O = 1-02.
TiOo = -24
Quartz =3'93
12-88
(2A) To ascertain proportions of limestone and

sbale to obtain desired mixture.
107
Ultimate Analysis.
Limestone. Shale,
SiO 2 = 5'96 4974

A1 2 O 3 = 2-00 15*98
Fe 2 3
= 0-90 8-00
CaO =49-38 9-08
MgO = 1-12 4-03

Loss on ignition =40'12 10'04
Alkalies and loss = 0'52 3*13
100-00 100-00
Calculation.
Limestone.
SiO 2 = 5-96x2-8 =16'688
ALOo = 2'OOx 1-1 = 2-200
18-888*
Shale.
Si0 2 = 49-74 x 2-8 = 139'272
A1 2 3 = 15-98x1-1 = 17-578
157-850
CaO = 49-380 157'85
-18-888* -CaO in shale 9'08
y =30-492 a =14877
14877x100
Then =487>9
30-492
Therefore 100 parts of shale should require 487'9
parts of limestone, or
Limestone 4 '8 parts
Shale ro part
APPENDIX 109
(3 A)To produce mixture containing 75 per cent.

CaCO 3 same materials.
;
CaCO 3 in limestone = 88*1 8 per cent.

Per cent, required =75*00 ,,
Shale required =13*18 parts.

- -
f
Per cent, required =75*00
CaCO 3
in shale =16*21
Limestone required = 58*79 parts.
or Limestone 4*4 parts.

Shale 1*0 part
(4A) Analysis of Slurry (54).
Example of calculation :
CaC0 3 = 75*2 per cent. = CO 2 33*08 per cent, (B).

Loss on ignition = 33*80 per cent. (A).
Then 33*80
-33*08
= 0*72 loss due to organic matter (C).
and 100 --
0*72 = 99*28 (D).
= 75*74 calculated CaCO 3 .
(5 A) Calculated CaO (55).

Lime in residue after ignition = 42*4 per cent.
Loss on ignition =33*8
oo. 8 = 64 per cent, calculated CaO in clinker.

1QQ
(GA) Directions for making up E Solutions.
= 10E HC1.
Hydrochloric acid (sp. gr. 1-16)
( 1-08) = 5E HC1.
200 c.c. of 5E HC1
diluted to 1 litre = E HCl
Nitric acid (sp. gr. 1-5) -24E HN0 3
.
( 1-42)
= 5EHN0 3 .
= 36E
Sulphuric acid (sp. gr. 1-842) H^SO^
Acetic acid (glacial) = 17E Ac.
294 c.c. 17E diluted to
1 litre = 5E Ac".
Oxalic acid 9 4 '5 grams dissolved

and diluted to make
3
1 litre
=2 Eox
'
Ammonium hydrate ('880)

= 20E NH OH 4
equal volumes
of 20E and
distilled water = 10E NH OH 4
oxalate 42*6 grams dis-

solved and diluted
o
to 1 litre = ^.E Am. ox.
carbonate 1967 grains

dissolved in 333*3 c.c.
of 5E NH OH 4
and
diluted to 1 litre = 5E Am C0 2 3
Sodium hydrate 200 grams dis-
solved to make 1 litre = 5E NaOH

,, carbonate 429 grams of
crystals to make 1 litre = 3E Na 2 C0 3

APPENDIX 111
Sodium hydrogen phosphate 119*3

grams of crystals dis-
solved to make 1 litre = E Na 2 HPO 4
o
sulphite 252 grams of
crystals to make 1 litre = 4E Na 2 SO 3

acetate 544 grams of
crystals to make 1 litre = 4E Na Ac.

Potassium hydrate 280 grams to
make 1 litre = 5E KOH
iodide 166 grams to
make 1 litre =E KI
chromate 97*25 grams
to make 1 litre =E K 2 Cr0 4
ferrocyanide 105*5
grams to make 1 litre =E K 4

FeC 6 N 6
,, ferri cyanide 109*7
grams to make 1 litre =E K 3 FeC 6 N 6
,,
sul phocy anide 9 7 grams
to make 1 litre = E KCNS
Bromine water water at 15*5 C.
pi
saturated with Br = Br water
2i
Barium chloride 122 grams dis-

solved to make 1 litre =E Ba'Cl 2
Silver nitrate 170 grams dissolved

to make 1 litre = E AgNO 3
34 grams dissolved
Tjl
to make 1 litre = ,,
Mercuric chloride 24 '2 grams dis-
2E
solved to make 1 litre = ^- HgCL
o
Copper sulphate 12475 grams of

crystals to make 1 litre = E CuSO 4
Platinic chloride 49*3 grams of Pt
converted into PtCl 4 and di-
luted to 1 litre = E PtCl 4
Magnesia mixture 68 grams
MgCl 2 6H 2 O in about 500 c.c.
H 2 O,
add 165 grams AmCl,
300 c.c. 5E NH 4 OH and dilute
to 1 litre = E Mg Mixt.
Ammonium molybdate. Dissolve 90 grams in 700

c.c. of water, allow to settle and decant dilute ;
to 1 litre.
Fusion mixture
106 grams of dry
"
Na 2 C0 3
138 K C0
2 3
well mixed and ground together.
Mixture for Hundeshagen's method (63) for sulphur

in fuels
MgO 2 parts by weight

K C0 3
2
1
part
dried and ground together.
Copper sulphate pumice for absorption (14) of HC1 +

H 0- 2
Soak some pieces of pumice stone free from dust

in a saturated solution of CuS0 4 . When
APPENDIX 113
thoroughly saturated, dry and ignite until free

from blue colour. Store in a well-stoppered
bottle.
PREPARATION OF STANDARD
SOLUTIONS
(7A) Normal Sodium Carbonate, N.Na 2 C0 3 .
Dissolve exactly 53 grams of Na 2 C0 3 (prepared

by igniting bicarbonate) in distilled water and make
up to 1000 c.c.
1 c.c. = '053 gram Na.2 CO 3

= '022 C0 2
N
(8A) Deci-normal Na 2 CO 3 = ^ Na 2 CO 3 .
Dissolve 5*3 grams in 1000 cc. of distilled water.

1 c.c. = -0053 gram Na 2 CO 3 .
(9A) Normal Sulphuric Acid, N.H 2 SO 4 .
Dilute about 30 c.c. of cone. H 2 SO 4 (sp. gr. 1-840)
to 1 litre. Add the acid to less than 1000 c.c. of

water, and, when cool, titrate against N.Na 2 C0 3 ,
using methyl orange as indicator. Then measure

the solution and dilute to correct bulk.
1 c.c. = -049 gram H 2
SO 4 .
N H
(lOA) Deci-normal Sulphuric Acid, TT; SO 2 4
.
Dilute 100 c.c. of normal H 2

SO 4 to 1000 c.c. and
N
standardise against
r^
Na 2 CO 3 .
1 c.c. = -0049 gram H SO2 4

.
(HA) Normal Hydrochloric Acid, N.HC1.
Dilute 150 c.c. of pure HC1 (sp. gr. 1-16) to 1000
c.c., titrate with N.Na 2 CO 3 and correct accordingly.
1 c.c. = '0365 gram HC1.
N
(12A) Deci-normal HOI, y^ HOL
Dilute 100 c.c. of N. HC1 to 1000 c.c. with distilled
water.
1 c.c. = '00365 gram HC1.
(13A) Normal Sodium Hydrate, N. NaOH.

Dissolve about 44 grams of stick NaOH, free from
carbonate, in about 1000 c.c. of distilled water.
Titrate, when cool, against normal 2
SO 4 and diluteH
accordingly ;
use methyl orange or phenolphthalein
as indicator.
1 c.c. = '040 gram NaOH.
(14A) Deci-normal NaOH.
Dilute 100 c.c. N. NaOH to 1000 c.c. with distilled
water.
1 c.c. = '0040 gram NaOH.
(15 A) Normal Potassium Hydrate, N. KOH.
Dissolve 56 grams in less than 1000 c.c. of water,
titrate against N. H 2 S0 4
and dilute accordingly.
,
For alcoholic KOH use 90 per cent, alcohol.

1 c.c. = -056 gram KOH.
(16A) Deci-normal KOH, ^ KOH.

Dilute 100 c.c. of normal KOH to 1000 c.c. and
standardise.
1 c.c. = -0056 gram KOH.
APPENDIX lis
(I?A) Deci-normal Potassium Permanga-

N
nate, ^ K 2 Mn 2 8
.
Dissolve 3*156 grams of potassium permanganate

in distilled water and dilute to 1000 c.c. Titrate
with pure iron wire, ferrous ammonium sulphate, or
oxalic acid.
N
1 c.c.
r^
K Mn 2 O =
2 8
-0056 gram Fe.
= -0072 FeO.
= -0080 Fe 2 O 3 .
(ISA) Deci-normal Potassium Bichromate,
^ K Cr 2 2 7
.
Dissolve 4 '9 13 grams of fused crystals in water

and make up to 1000 c.c.
1 c.c. = -0056 gram Fe.
This solution requires standardisation after a time.

Use potassium ferricyanide on a spotting tile as
indicator.
Deci-normal Silver Nitrate,

N
AgNO 3 .
Dissolve 16*998 grams in distilled water and make

up to 1000 c.c.
1 c.c. = -003545 gram 01.
1
INDICATORS.
(19 A) Litmus Solution. Digest the solid with dis-
tilled water for several hours. Decant or filter,
render neutral by means of acetic acid or ammonia.
Store in a bottle with access of air.
(20A) Methyl Orange. Dissolve about 1 gram of

the solid in distilled water and make up to 1 000 c.c.
(21 A) Phenolphthalein. Dissolve a little of the

solid in alcohol and dilute with alcohol and water.
(22A)TABLE OF ATOMIC WEIGHTS OF PRIN-

CIPAL ELEMENTS OCCURRING IN CEMENT
WORKS ANALYSIS.
Aluminium
APPENDIX 117
(23A) FACTORS FOR USE IN ANALYSIS,

Kequired. Known. Factor.
CaO CaC03 0*56043
CaC03 CaO 1-78431
C I
C0 2 0-27272
Fe Fe 2 3
0-69953
Fe 2 3
Fe 1*42933
H S02 4
BaS04 0-42007
S 0-13734
S0 3 0-34291
KO 2
K 2
PtCl 6 0-19411
KO 2
KC1 0-63204
Na 2 NaCl 0'53077
MgO Mg P 2 2 7
0-36242
P 0*63757
1
(24A) LIME IN CEMENT (119).
Milligrams
of
CaSO 4 .
APPENDIX 119
(25A) TABLE FOR ESTIMATION OF MgO IN

CEMENT (126).
MAGNESIA, USING '5 GRAM OF CEMENT.
Weight of
Mg2 P2 7.
CEMENT CHEMISTS HANDBOOK 1
(26A) TABLE FOR ESTIMATION OF SO 3

IN
CEMENT (128).
SO,, USING -5 GKAM OF CEMENT.
Weight of
BaS0 4 .
APPENDIX 121
co <M CM CM CM cq cq O O O O Oi O
CiGi
OOOOOOOOOOOOOOOOOOOOOOGOCOCOOOOOCO1>.I>.
s* opopoipoipoipopopoipppo
si
78
OOOOOOOOCOOOOOOOGOOOOOOOOOOOCOOOOOOOOO
O O T I <M (M CO CO
T I
CM CM <M <M <M (N (N (M

ft M
00
fcc J,
"^
-ft
3f ^S
io Ci O Ci O> Ci OlOoooooidiCiCidioooboo
cqcNi-Hr-iTiT
C5 C5 Ci O Oi 00 OO 00 CO 00 OO 00 00
^ o
P. .go
I'M
1
(28A) TABLE FOR USE WITH SLATER'S

CALCIMETER.
ESTIMATION OF CaC03 IN LIMESTONE.
Heading.
APPENDIX 123
(29A)TABLE OF CORRECTIONS TO BE ADDED

TO CALCIMETER READING FOR VARYING
AMOUNTS OF PEAT IN SLURRY.
RESULT = CALD. CaC0 3 (54).
CALCIMETER READING.
1
(30A) TABLE OF
PRESSURE OF AQUEOUS VAPOUR.
af
APPENDIX 125
(3lA) TEMPERATURE CORRECTION TABLE

XO5O5O5OiO5 '-ii I fM i I ^-H C<1 C<l C<l <M '
^^^ÔOOOOQDicboil>'l^l^t~t-XXXXC5O5C5C5C5C>-*
XXXXXXXX XXXXXXXXX XXX X X X X X X_X_Oj_Ci_C5_O5 OS O>
~f.
x :c x x x xx xxxxx x^ xxxxxxxxx -/ /. x x x xx x cy ?-
<*iOOOOOÔCDCDCOIr-l>'tÎ>'t^XXXXXO5C:O5C5C;
COeO^'*-^Tt<
XXXXXXXXX XXX XX X XJX_X_XJXJJC_XJX>_X_XJX X_X_Op_00
>
OP_X_05_05
X_X_X.X_X X X._X X XXXXXXXXXXXXX

cococococo^fj<oooioor--t--t--t^r xxxxxo55O5Oi
X^C X X_X X X X X X X X X X X X X X X X X X X X X X X X X XXX
>>
f. r.
xx x~ ss c: c: si ci"o O~o~ oo < i
XXXXXXX
t
XXX
X_Jc_X_XJX X X X X X_X X _X_X X X X X X X X X_X_X.
t'-t^t'-r^XXXXXCJCJCSCSC; O O OO-H-HI I^HI iC^C^Cê^C^COCOCOCOCO
XXXXXXXX X XXXXXXXXX X X X_X X X XXXXXXXXX X
__X.X_X__X_X_X.X XX X__X_X^X _X XXXXXXXXXXXXXXXXXX
"^^^^^c^c^^cococococo^T^-rtiT^TôoibiO'OOO?!;
xxxxxxxxxxxxxxxxxxxxxxxxo XX XXXXX
xxxxxxxxxxxxxxxxxxxx xxxxxxxxxxxxx
^^^C^<NC<ie<IC<ICOCOCOCOCO-^TfTt<-^'<*iOiOtOiCiOCDCDCDCDCOlr'I>l>l>l>'
XXXXXXXXXXXXXX eoco-^T^-^TtHTîbibibibibcbcbocbot^t^t-
XXXXXXXXXXXXXXXXXXXX
*
H CO IO t** Oi f~H CO lO l^* O5
-
X X X X* X X* X X X X X X X X X X ocb^Dcboot-
OO XXXXX XX
gggrss
xxxxxxxxxxxxxxxx x xaoxxxxxxxxx
X X X X X~ X X QO X X OD QO 00 QD X X X X X X X X X X X X X X X X X X X X
_x__x_x_x_x xx x xx x x "x x xx x x xxx xjc x

cocoj<^t<<>>i<
X X X X X X X X X X X _X X
XXXXXXXXXXXX X XXXXXXXX
1
(32A) BAROMETRIC PRESSURE CORRECTION

740.5
Mm.
APPENDIX 127
BAROMETRIC PRESSURE CORRECTION

CaCo3 ! 762
per cent. Mm.
CO O
O
o oo co o o C5
CO 00 Ol O **" rH O
o
Ol CO rH t^ <X> CO
b- 00
GO t^ Ol f-
O Ol O5 CC rH r
CO Ô
O
Ol
l oo 01 o-
I CO CO HH ~- I
rH O
CO
t^ <N
rH ^*
O
CO
w bl
CO
E O O CO GO O
O
>^. 03
o co
*
01 GO CO rH
COS
U
s
CO
CO
CO
Ol Ol CO OO
C5
CO -TfH O5
p ^tl
rH 6
O
O
?c|
5 O^-a *iid
ce '
S)
^J S-'l J
lllJlll
<
02 M pin hH i^ "S
APPENDIX 129
o^
oc x
oO6 cr.
II II II 7
o-S
oc
o o 5?,
-?
u os o
en
D
o
K
CJ
U wu -^g
2 O
86
^L-
.
c c
11
IT l|
yil
el SM^
2
, I O QO
<
o ^-i I * (M O "M I
3o
cj cj .
II! Hil IJtt

S 02 *$
*Sg
a o 01 o o GO o
W HK SOS"
(M CO
1
^ H
<frl
w s
3 a
2 Q 3 oo O
*< ~*
cs
s J H
CM
O ^ O
CO
H <M O
2 02
hJ
CO
W o TO
to rH n <M fa 3 i<0 Or-oOrH
2: >i
;
Ci
<M T- CP
cp p
O ^^-S ^
O
W rH o to o o to o t^
C5
0, -tt^Nj
TOOl'qO<>l
(f1 O O CO rH
rH O
O rH
CM
O
-4
fa
O TO
cu rH rH rH r-l
CO
CO
TO O -H GO CO 00 O (M h- 'M
o TO (>1 TO "^ O rJ H as O O .Li Ci TO
rH 4fl TO
^5
CO
|
CO
r-1
OQ .3
2 05 S o^
o
s1^
J
W^
< &
_CJ
FH F
03
o-
bJO.2
g
6
* o
fl
Q i-< O <
O f
^ "3
a
a as
S
sS J^ bDOi
il i J
APPENDIX
LLLON.
CEMENT CHEMISTS HANDBOOK
1
(34A)
TABLE FOR USE WITH BLOUNT'S FLASK,

SPECIFIC GRAVITY. USING 50 GRAMS OF
CEMENT AND 50 c.c. OF OIL.
Volume of oil
displaced.
APPENDIX 133
(3 5 A) Table for Use with Anderson's Specific Gravity

Bottle using 150 grams of Cement and 200 c.c. of Oil.
Displace-
ment.
USEFUL DATA FOR TESTING-ROOM.

For each neat briquette in British standard
mould take 130 grams of neat cement, and gauge
with correct proportions of water.
26 '0 c.c. water used = 20 per cent.

27-3 - 21
28-6 - 22
30-0 = 23
31-2 = 24
32-5 = 25
For each sand briquette take

37 grams of cement,
111 ,, standard sand.
10*5 c.c. water used = 7 per cent.

^ 55 5 J
^ J 5
13-5 - 9
lo'O = 10
For each Le Chatelier expansion test use

50 grams of cement.
APPENDIX 135
To convert
Lbs. per sq. inch into kilos per sq. centimetre

x by '0703
Kilos per sq. centimetre into Ibs. per sq. inch
x by 14-223
Holes per sq. centimetre into holes per sq. inch
x by 6'45
Holes per sq. inch into holes per sq. centimetre
x by '155
Grams into grains x by 15*43235
Grains into grams x by '0648
Fahrenheit
Degrees Centigrade into degrees (F.)
9
x - and add 32.
Fahrenheit into Centigrade (C.)

5
subtract 32 and x by <r.
INDEX
ALKALINE permanganate, 73 Engineering Record," 83
Ammonium chloride, Standard, 75 Equivalents, 2
Apparatus required, 3
Appendix, 107 FILLING gas burette, 86
Aspirator, 17, 85 Formulas, Calculation from, 39
Authors, consulted, 4 Fusion, 23
BAMBER'S calcirneter, 48 GAS burette, Filling, 86

Bayley, 4
Beringer, C. & J. J., 4 HBMPEL, 4, 86
Blount &; Stauger, 4 Hem pel's apparatus, 86
Books consulted, 4
British coals, Analyses of, 61 INDIGO, Solution of, 79
Introduction, 1
CALCDIETERS, 44 Iron, Estimation of, 28, 29
,, Bamber's, 48 pyrites in clay. 29
,, Slater's, 45
Calculation of proportions, 39 KILN gas, 90
lime in clinker, 52
Calorific power of fuel, 00 LEWKOWITSCH on oils, 02
Chemicals required, 2 Limestones for cement, 38
Clays for cement, 39
Clowes & Coleman, 4 MEADE, R. K. (Portland cement),
Coal, Fineness of, 61 by, 4, 51, 100
Collection of samples fuel, 50
gas, 84 XEILSON'S sulphur in coke, 05
ru\v mate- Sessler's reagent, 75
rials, 5
,, slurry,&c.,41 ORSAT gas apparatus, 89
water, 07 Orton, 4,90
Collins, W. D., 83
PHILLIP'S " Chemis-
Colliery Guardian," 01
'
Engineering
Combustion in rotary kiln, 90 try," 1
Control of raw mixture, 53 Potash for absorption, 80
Copper chloride solution, 80 Pjrogallol for absorption, 80
Copper sulphate, pumice, 10
QUARTERING, 5
DENNIS. 4
Dreverhoff. Max, filter-paper. 15 RAW materials, calculation of pro-
portion, 38
ECKEL, 4 Raw mixture, Control and alteration
Elutriation, 24 of, 53
*
Engineering Chemistry," 1 Reagents required,
137
138 INDEX
Keddrop's system, 1 Stanger and Blount, 4
Redwood's viscosimeter, 63 Strength of solutions, 1
SAPONIFICATION equivalent, 66
TAYLOR, 1
Separation of soda and potash. 32 Thermal units, 61
Shales for cement, 39
Thompson, Lewis, calorimeter, 60
Shinier crucible, 101
Slurry. Dry standard, 44, 45
Smith, Lawrence, 31 VOLUMETRIC determination of lime,
62 12
Specific gravity, oils,
Standard ammonium chloride, 7'> Volumetric determination of lime,
,, soap solution, 71 Rapid, 101
potassium nitrate, 79
,, permanganate, WATER softening, 81
102 , ,
Lime required, 83
INDEX TO ANALYTICAL PROCESSES
Paragraph
Analysis of Ash of coal

Calcareous shale . .
Loss on ignition
Silica .
Alumina and ferric oxide

Liine and magnesia .
Cement, Accurate . .
Technical
Loss on ignition
Silica and insoluble . .
Insoluble .
Alumina and ferric oxide

Lime . . .
Magnesia . .
Alkalies
Sulphuric anhydride . .
Sulphur as sulphide .
Carbon dioxide
Keene's
Loss on ignition
Silica and insoluble .
Alumina and ferric oxide .
Lime ,.
Sulphuric anhydride .
Chalk . . . .* .
Moisture
Loss on ignition
Silica and insoluble
....
.
Alumina and iron oxide .
Lime
Calcium carbonate .
Carbon dioxide
Magnesia.
Alkalies
Sulphates
. ..... .
:
.
.
.
Clay .
Moisture .....
.
Loss on ignition
.
. .
139
140 INDEX TO ANALYTICAL PROCESSES
INDEX TO ANALYTICAL PROCESSES 141
INDEX TO APPENDIX
Table
1A. Calculations occurring during clay analysis
2A. To ascertain proportions to obtain desired raw mixture
.... . .
rage
107
107
3A. To produce mixture containing certain percentage of CaCO 109
....
, .
;
'
F \ Calculations occurring during slurry analysis 109
6A. Directions for making up equivalent solutions, etc. . . 110-113

7A. Preparation of normal sodium carbonate solution . . .113
8A. Preparation of decinormal sodium carbonate solution . .113
9A. Preparation of normal sulphuric acid solution . . . .113
10A. Preparation of decinormal sulphuric acid solution . . .113
HA. Preparation of normal hydrochloric acid solution . . . 114
12A. Preparation of deciuormal hydrochloric acid solution . . .114
13A. Preparation of normal sodium hydrate solution . . . .114
14A. Preparation of decinormal sodium hydrate solution . . .114
15 A. Preparation of normal potassium hydrate solution . . .114
16A. Preparation of deciuormal potassium hydrate solution . .114
17A. Preparation of decinormal potassium permanganate solution . 115
ISA. Preparation of decinormal potassium bichromate solution . . 115
Preparation of decinormal silver nitrate solution . . . .115
19A. Preparation of litmus solution . . . . . . .116
20 A. Preparation of methyl orange solution . . . . .110
21 A. Preparation of phenolphthalein solution .116
..
. . . .
22A. Table of atomic weights . . . . . .116

23A. Factors for use in analysis . . . . . . .117
24A. Table for estimation of lime in cement . . . . .118
25A. Table for estimation of magnesia in cement . . . .119
26A. Table for estimation of sulphuric anhydride in cement .120
....
.
Tables for use with Slater's calcimeter 121-122

29A.
30A.
Table
Table of pressure of aqueous vapour
.....
for correction of calcimeter reading
. . . . . .124
122
31A. Table for temperature correction for Bamber's calcimeter . . 125

32A.
33A.
Table
Typical analyses, limestones, clays .....
for barometric correction for Bamber's calcimeter . . 126
128
..........
.
Typical analyses, shale, calcareous cla} , slag, puxzolanic

material 129
Typical analyses, waters ........

Typical analyses, raw meals, slurries, cements
34A. Table for use with Blount's specific gravity flask

. .
.
.
.
.130
. 132
131
Useful data for testing-room ......

35A. Table for use with Anderson's specinc gravity flask . . . 133
134.135
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PAGE PAGB
ADAMS (W. P.), Motor Mechanism, 33 . LAMBERT, Glue, Gelatine, &c., . . 81
AIT KEN, (T.), Road Making, 79
. . LARARl) (C. E.), Eng. Calculations, . 31
ALFORD (C. J.), Mining Law, LAWN
ALLINGHAM (W.), Meteorology,
ANDREWS (L.), Electricity Control, 48
57
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41
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(J. G.), Mine Accounts,
(F. H.), Acetylene,
LIVERSIDGE, Engine-Room Practice,
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... . 57
77
29
ANGLIN (S.), Design of Structures, 26 . MACKENZIE (T.), Mechanics, . 42
ARCH BUTT & DEELEY, Lubrication, 32 MACLEOD (W. A.) and WALKER
ATHERTON (Wm.), Design of Beams, 26 (
C.), Metallurgical Chemistry, . . 60
BARKER (D. W. Works by,), 40, 41
. McLAREN (R. S.), Elem. Mech. Eng., 33
BAUER (M.), Precious Stones, 68
. . MCMILLAN (W.G.),Electro-Metallurgy,67
BERINGER(J. J.&G.), Assaying, . 66 & BORCHERS, Electric Smelting, 67
BICHEL & LARSEN, Explosives, . 58 MCWILLIAM, Foundry Practice, 68 .
MIDDLETON (R. E.), Water Supply,

BILES
BJORLING,
(Prof.),
Design of Ships,
Peat
....
Marine Steam Turbine, 28
37
75
MILL Dr. R. H.), New Lands,
(
MILLAR W. J.), Latitude & Longitude,

(
.
77
53
43
.
BLACKMORE (E.), Mercantile Marine, 40 MITCHELL (C. A.), Flesh Foods, . 74

BLOUNT(B.)and BLOXAM (A.G.), &HEP WORTH (T. C.),Inks, . 81
Eng. and Manuf. Chemistry, 46, 71
MORGAN (J. J.), Metallurgical Tables, 66
.
BLYTH (A. Wynter), Foods and Poisons, 72 MUNRO & JAMIESON'S Elect.Pkt-bk.,49
BORCHERS (Dr.), Electric Smelting, 67 MUNRO(R. D.), Works by.. . . 32
BROUGH (B. H.), Mine-Surveying, 56 .
NA YLOR(W.), Trades' Waste, . 76 .
BRUCE (Robt.), Food Supply,

BURNS (D.), Colliery Electricity,
.53
BUCK (R. C.), Algebra <& Trigonometry, 42
56
.
NICHOLSON
NORTH (S.), Oil Fuel,
OPPENHEIMER
....
(W.), Smoke Abatement, 76
(C.), Works by, 74,75

61
BUTTERKIELD(W. J. A.), Gas, 77

.
.
OSMOND & STEAD, Micro. Analysis, 60
CAIN & THORPE, Synthetic Dyestuffs, 82
CARTER (H. R.), Long Fibre Spinning, 83
CAST ELL- EVANS, Chemical Tables, 79
PARK, (J.), Cyanide Process,
PE
Mining Geology,
ARC E (W.J.), Painting,
. ...
. 59
56
80
.
... . . .
CHATLEY (H.), Flight, PETTIGREW (W. F.), Loco. Eng., . 30

CLARK (J.), Soil Bacteria,
CLAYWORKER'S HANDBOOK,
... .
33
73
75
PHILLIPS &
POYNTINGJ&
BAUERM
THOMSON,
AN, Metallurgy, 60
Physics, 50 .
COLE (Prof. G. A. J.), Works by,

COLE (W. H.), Light Railways,
COLLINS, (H. F.), Lead and Silver,
.
PRAEGER
RAWSON, GARDNER, & LAYCOCK,
....
(R. L.), Open Air Botany, . 85
RANKINE'S Works, 35
COX (S. H.), Prospecting for Minerals, 53 Dictionary of Dyestuffs, .82

.
CROTCH, Telegraphic Systems, 49

REDGRAVE (G. R.), Cements, . . 76
CUNNINGHAM (B.), Works by,
. .
27
REDWOOD ( Sir Boverton), Petroleum, 61
DAVEY (H.), Pumping Machinery,
.
36 & THOMSON, Handbook, .61 .
DIXON (C.), Bird-Life,

.
REED (Sir E. J.), Stability of Ships, 37

...
.
. . 85
DON KIN (Bryan), Works,
.
28
REID(Geo., M.D.), Sanitation, .78 .
DUERR (Geo.), Bleaching, &c., 84

RICHMOND (H.D.), Works by, 73 .
DUNBAR (Prof.), Sewage Treatment,

. .
76
RIEMER (J.), Shaft Sinking, . . 58
DUPRft & HAKE, Manual of Chemistry,70 ROBERTS -AUSTEN, Metallurgy, 63 .
ROBINSON (Prof.), Hydraulics, . . 36

EICHHORN, Wireless Telegraphy, 49 .
ROSE (T. K.), Gold, Metallurgy of, 63
ENGLISH (T.), Set Squares, . . 46 ROTH WELL,
.
(C. F. S.), Textile Printing, 83

FARNSWORTH, Cons. Steel Work, . 26
SCH WACKHOFER, Fuel and Water, 46
FIDLER (Prof.), Bridge- Construction, 26
SCHWARTZ
FIELD (E. R.), Mining Report Book, . 57 (Dr. von), Fire Risks, . 77
KO8TE ft (Sir C. Le Neve), Works by, 54 SEATON (A. E.), Marine Engineering, 44
& ROUNTHWAITE,
GAIRNS (J. F.), Loco. Compounding,
GINSBURG
GOLDING
(Dr.), Shipmasters' Duties, 43
(H. A.), Bonus Tables,
30
Engineers' Pocket- Book,
SEXTON (Prof.), Works by,
... Marine
. 66,70
44
. 31
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SHELTON (W. V.), Mechanic's Guide, 36
GU RD EN (R.), Traverse Tables, . 31
SIN D ALL, Paper Technology, . . 81
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SMITH (Prof. R. H.), Works by, . . 45
H ANN AN (W. I.), Textile Fibres. 83 SMITH, (W. J.), Shipmaster's Med. Help, 4S
HARBORD(F. W.), Steel, . .
.
65
SOLOMON (H. G.), Electricity Meters, 48
HARRISON (J. W.), Sanitation, . . 78 STRICKLAND F.), Petrol Motors, 33 .
HEY LIN (H. , Cot. Weavers' Handbk, 83 SUPLEE (H. H.), Mech. Pocket Book, 45
HICKS (J. A.), Mineral Oil Testing, . 61 SYKES (Dr. W. J.), Brewing, . . 75
HO BBS(L.), Engine Design, . . 27 TRAILL (T. W.), Boilers, . 29
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HUGHES (H. W.), Coal Mining, . 55 TURNER (Thos.), Iron, Metallurgy of,
. .
65
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HURST (G. H), Works by, . . . 80 WALTON (T.), Works by, 44
JAMIESON (Prof.), MANUALS,
38,
. .
JOHNSON (J. C. F.), Getting Gold,

. . 34
59
WEBER (Dr. C. O.), India Rubber, . 81
JUDE( A.), Steam Turbine, 7 . .
.
28 WELLS (S. H.), Engineering Drawing, 32

JULIAN SMART
(H F) and (E.),
WIGLEY (T. B.), Jeweller's Art, . 68
Cyanidinsr Gold and Silver Ores, . 59 WILLOUGHBY (Dr. E. F.), Milk, . 73
KASSNER (T.), Gold Seeking, . . 59 WOOD (Francis), Sanitary Engineering, 78
KERR (G. L.), Works by, WORDINGHAM, Electrical Stations, . 48
KNECHT RAWSON,
& Dyeing, . 82 WRIGHT (Dr. A.). Oils and Fats, . 71
LAFAR, Technical Mycology, . '74 ZERR & RUBENKAMP, Col. Manuf., 80
Griffin's Standard Publications
Applied Mechanics, RANKINE, BROWNE, JAMIESON, 35, 46*34
.
Civil Engineering:, . PROP. RANKINE,

. 35
Desigî Of Structures, 8. ANQLIN,. 26 . .
Bridge-Construction, PROF. FIDLER,

. 26 . .
Design of Beams, . W. H. ATHERTON,

. 26 .
Dock and Harbour Eng., B.CUNNINGHAM, 27 .
Engineering Drawing,
Engine Design,
S. H. WELLS,
L. HOBBS,
.
Constructional Steelwork, A. W. FARNSWORTH,

.
.
32
27
26
... . .
Central Electrical Stations, C. H. WORDINGHAM, 48 :
Electricity Control, L. ANDREWS, 48 .
Meters, H. G. SOLOMON, 48 . .
W. H. COLE,
Light Railways,
Sanitary Engineering,
Traverse Tables,
.
F. WOOD,
30
78
R. L. GURDEN,
... .
.
.
. 31
Practical Calculations, C. LARARD & H. GOLDING, 31
Locomotive Engineering, W. F. PETTIGREW, . 30
Locomotive Compounding, J. F. GAIRNS, .
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. . 37
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NAUTICAL WORKS. 39
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NAUTICAL WORKS. 41

SECOND EDITION, Revised and Illustrated. Price 8s. 6d.
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NAUTICAL WORKS. 43

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... 53
53
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of,
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54 .
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Leather, R. S. TROTMAN, . 81
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Painters' Laboratory Guide, 80
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Dyeing, KNECHT AND RAWSON, . 82
Dictionary of Dyes, RAWSON AND GARDNER, 82
The Synthetic Dyestuffs,. CAIN AND THORPE, 82
Spinning, . H. R. CARTER, . 83
Textile Printing, SEYMOUR ROTHWELL, . 83
Textile Fibres of Commerce, W. I. HANNAN, . 83
G. H. HURST, 84
Dyeing and Cleaning, .
84
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CEMENT WORKS CHEMISTS

Their Nature, Preparation

In Crown 8vo. Cloth. With 30 Illustrations, 2.00 net

THE CLAYWORKERS' HANDBOOK

Second Edition, Revised. Illustrated, $4.00 net

CHEMISTRY OF THE MANUFACTURING

PEAT: ITS USE AND MANUFACTURE

Beautifully Illustrated with Plates and other Illustrations. $6.50 net

Treatment and Utilisation

In Medium 8vo. Fully Illustrated. $3.50 net

Being Notes on the Practical Aspect and the Principles

In two volumes, each complete in itself and sold separately.

LONDON : CHARLES GBIFFIN AND Co. LTD. EXETEE ST. STEAND

TO 15E HAD OF J. B. LlPPINCOTT COMPANY. PHILADELPHIA

CEMENT WORKS CHEMISTS

ANDERSON, ESQ., C.E. CHEMIST AT THE XEM

HARTFORD CEMENT WORKS

WITH ILLUSTRA TIO.\S

[AU rights reserved]

ANALYSIS OP RAW MATERIALS

Insoluble Alumina and Iron Oxide Lime ; Volumetric Determination

of CaO Lime as CaS0 4 Magnesia Sulphates Accurate Estimation of

Carbon Dioxide Rapid Estimation of C0 2 Marls, Gault Clay, Calcareous

Shales Clay Estimation of Iron by Means of Standard Permanganate

Mineral Oils Water Analysis Collection of Samples Colour, Odour,

Reaction ; Sediment and Suspended Matter Total Solids Chlorine as

Chlorides Hardness, Temporary and Permanent

Standard Ammonium Chloride, Nessler's Reagent, Alkaline Perman-

tion of Oxygen required to Oxidise Organic Matter Estimation of ;

Nitrates + Nitrites Poisonous Metals ; Water Softening Gas Ana-

lysis Collection of Samples ; Analysis of Gases in the Hempel Appara-

tus Filling the Burette Estimation of Carbon Dioxide, Oxygen, Carbon

Monoxide, Nitrogen, Combustible Gases ; Analysis with the Orsat

INDICES .... ... pp. 137-142

is hoped that it may be found of use in other

carried out. An epitome of most of the processes

and strength in terms of E, this being

molybdate. Manganese carbonate.

CHEMICALS REQUIRED (contimted).

Mercuric chloride. Lead nitrate.

Distilled water. Litmus.

Absorption apparatus. Drying tubes.

Argand burners. Filter paper (Schleicher and

Rough balance. Viscosimeter.

The following works have been consulted in com-

Phillips. Engineering Chemistry.

ANALYSIS OF RAW MATERIALS

sample should be carefully numbered and labelled

experienced, and these are

centage of moisture in sample is required, however,

sample as possible, as well as more accurately in

(1) Chalk or Limestone. If sufficiently dry,

(2) Moisture. If very wet and difficult to

plate, taking care that the temperature does not

(3) If fairly dry and readily powdered, an accu-

Weigh out accurately into a flat porcelain weighed

(4) Loss on Ignition. Into a weighed platinum

from muffle and allow to cool in a desiccator ;

(5) Silica and Insoluble. Brush the ignited