TM 9-2900, Military Explosives

TM 9-2900
W AR DEPARTM ENT
TECHNICAL MANUAL
&
MILITARY EXPLOSIVES
*TM 9-2900
1
LI WAR DEPARTMENT,
W a s h in g t o n , August 29, 191f0.
M ILITA R Y EXPLO SIVES
Prepared under direction of the

Chief of Ordnance
Chapter 1. Propellants. Paragraphs

Section I. General------------------------------------------------------- 1-5
II. Manufacture of smokeless powder__________ 6-17
III. Granulation of smokeless powder------------------ 18-20
IV. Stability and storage of smokeless powder— 21-26
V. Inspection o f smokeless powder_____________ 27-31
VI. Compound propellants______________________32-34
VII. Black potvder______________________________ 35-39
Chapter 2. Military High Explosives.
Section I. General_____________________________________ 40-41
II. Trinitrotoluene (T N T )------------------------------- 42-49
III. Ammonium picrate (Explosive D ) ___________ 50-55
IV. Picric acid__________________________________ 56-61
V. Nitrostarch explosives_______________________ 62-67
VI. Tetryl_____________________________________ 68-73
VII. Mercury fulminate----------------------------------------74-79
V III. A m atol__________________________„ ________ 80-83
IX . Lead azide_________________________________ 84r-88
Chapter 3. Bibliography____________________________________ 89
C h apter 1
PROPELLANTS
S e c t io n I
GENERAL
Paragraph
Definitions______________________________________________________________ 1
Classification-------------------------------------------------------------------------------------------- 2
Action______________________________________________________________________ 3
Use_____________________________________________________________________ 4
Composition_____________________________________________________________ 5
1. D efinitions.— a. Explosive.— An explosive may be defined in

general as being a gaseous, a liquid, or a solid substance, or mixture
♦This manual supersedes W ar Department Document No. 947, August 14, 1919.
249541°— 40------1 1
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1 -2 MILITARY EXPLOSIVES
of substances, which upon application of a blow to a small portion of

its mass, or by a rise in temperature is converted in a small space of
time into other substances more stable which are mainly gases or va
pors but may include solids. The chemical changes thus produced
develop a sudden rise in pressure in the surrounding medium, and the
word “explosive” is applied as a general term to the different types of
phenomena occurring in this sort of reaction. Coincident with this
evolution o f gas a considerable amount o f heat is evolved which pro
duces a flame. A high explosive is one in which this change occurs
within the shortest space of time and the phenomenon accompanying
this decomposition is termed a detonation. Detonation therefore
applies more properly to the chemical reaction incident to the almost
instantaneous decomposil ion o f the high explosive. However, it is not
properly employed when discussing the analogous reaction incident
to combustion of a slower burning explosive as smokeless powder.
The general term explosive which finds universal acceptance applies
alike to high explosives, black powder, and smokeless powder. It
will be seen therefore that the accepted distinction between the d if
ferent classes o f explosives is based primarily upon their relative speed
of decomposition, and only those explosives are classified as high
explosives in which this chemical change is considered practically
instantaneous.
b. Explosion.—Marshall (see par. 89) defines an explosion thus:
“ When gas or vapor is released so suddenly as to cause a loud noise
an explosion is said to take place as, for instance, the explosion o f a
steam boiler or o f a cylinder of compressed gas.” The barrel o f the
gun may be considered at the time of the explosion as being a cylinder
of compressed gas. Walls of the gun constitute walls o f the cylinder,
the breech mechanism one end, and the projectile the other.
2. C lassification.—Berthelot (see par. 89) enumerates and distin
guishes between eight different groups of explosive bodies which owe
their transformation either to application of some external circum
stance such as fire, shock, friction, or else to aid of a secondary reagent
or chemical agent which propagates within itself an explosive wave
and finally accomplishes a general explosion. O f these eight groups
(he greater number of military explosives fall within the third, fourth,
and eighth divisions:
a. Explosive inorganic compound*.—Definite bodies, liquids or
solids, as azides.
b. Explosive organic compounds.—Definite bodies, liquids or solids,
in which classification occurs the nitrated derivatives ol the carbo-
2
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MILITARY EXPLOSIVES 2 -4
hydrates as nitrocellulose, nitrostarch, and the nitrated derivatives of

the aromatic compounds as trinitrotoluene (T N T ).
c. Mixtures.—Mixtures formed by oxidizable and oxidizing bodies,
solid or liquid, neither o f these being explosives separately as, for
instance, black powder, etc.
3. A ctio n .— If an explosive were used which gave instantaneous
detonation the force so generated would either burst the barrel of
the gun or else (in the case o f a reduced charge) would not impart
sufficient velocity to the projectile to develop maximum efficiency.
This particular point illustrates the necessity o f using a relatively
slow burning explosive as the means o f propelling the projectile from
the muzzle o f the gun, an explosive which may be designated as the
propelling charge or propellant. Compression in the powder chamber
o f the gun must be developed slowly at first, gradually increasing in
intensity until the projectile in the case of the ideal gun is forced
to the muzzle, at which place the maximum pressure o f the charge
is exerted. However, in actual practice the maximum compression
in the gun is never developed at the muzzle, a condition which would
cause bursting according to our present design in which maximum
pressure is exerted just after the projectile starts moving from its
original position; usually maximum pressure occurs when the pro
jectile is only 1 foot or so ahead o f its original position. In this
function o f projecting a shot, the high explosive as such finds no
application. However, it may occur as a constituent o f a propellant
as for example, nitroglycerin, a high explosive which is an ingredient
o f certain sporting, pistol, and cordite powders. The field o f useful
ness o f the. high explosive as a class is quite different and advantage
is taken o f its properties o f detonation to use it within the shell or
other bursting projectile so that at the proper time the shell will be
disrupted through detonation o f the high explosive with which it was
filled.
4. U se.—The present tendency is to draw a sharp distinction
between two classes o f explosive bodies in accordance with the use to
which they are put and also in accordance with the speed of reaction
whereby combustion or decomposition takes place.
a. Propellants.— Those substances or mixtures whose rate of com
bustion is such as to permit their use for propelling projectiles from
guns are termed propellants.
b. High explosives.—Those substances whose rate o f decomposition
is so very high as to preclude their use as propellants but which on
the other hand bring about very powerful disruptive action are
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known as detonating explosives, disruptives, or more commonly, as

high explosives.
5. C om p ositio n .— a. The different substances used for high explo
sives are very many, but at the present time one substance with cer
tain modifications and additions is used as the base o f the propelling
charge. This substance is a colloid formed by action o f a solvent
upon a nitrated cellulose with or without addition of nitroglycerin,
and in its final form is called “smokeless powder.”
b. Selection o f these various substances is dependent upon their
cheapness o f manufacture and their safety in handling. In order
that these data may be evaluated properly it is necessary that the
following properties and measurements be determined:
( 1) Chemical equation involved in change o f substance from liquid
or solid to gaseous state.
(2) Thermo-chemical values as given in heats of formation o f the
different components.
(3) Specific heats.
(4) Densities.
(5) Relative pressure which may be developed by comparing equal
parts o f a new explosive with that o f one well known.
( 6) Type and amount o f energy required to initiate reaction.
(7) Rapidity o f reaction.
( 8) Relative power o f the explosive.
S e c t io n II
MANUFACTURE OF SMOKELESS POWDER

Paragraph
Historical sketch--------------------------------------------- 6
Term and form---------------------------------------------------- .-------------------------------------- 7
Manufacturing processes----------------------------------------------------------------------------- 8
Purification of raw cotton-------------------------------------------------------------------------- 9
N itration_________________________________________________________________ 10
Purification of pyrocotton----------------------------- 11
Formation of colloid------------------------------------------------------------------------------------ 111
Graining and cutting----------------------------------------------------------------------------------- 13
Solvent recovery----------------- 11
D ryin g___________________________________________________________________ 15
Blending__________________________________________________________________ 16
FNH and NH powders for cannon------------------------------------------------------------- 17
6. H istorica l sk etch .— The first nitrocotton which was made was

the result o f an experiment performed in 1838, when Pelouze ob
served the action o f nitric acid upon cotton. A few years later in
1845, Schonbein realized the importance o f this material as an explo
4
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MILITARY EXPLOSIVES 6 -7
sive and developed it to such a point that he endeavored to sell the

product to various governments. However, early attempts at the
use o f this new explosive, especially in Austria-Hungary, were
fraught with disaster, for factories were destroyed and guns were
damaged as a result o f unfamiliarity with chemical and physical
properties of this new substance.
However, the unfortunate experiences of the Austrians did not
deter the English chemists from developing the industry. Prominent
among these men at this time was Sir Frederick Abel who started a
small factory for the manufacture of nitrocotton at Waltham Abbey.
The industry received tremendous support, and the important prog
ress which was made during the next few years was in fact respon
sible for the later developments of collodion-photography and for
the artificial silk industry.
During this period use of guncotton as an explosive was restricted
entirely to blasting purposes. In seeking a new material which
might be used in place of black powder and which would not have
the objectionable features of the old propellant such as smoke, resi
due, etc., it occurred to Schultze that guncotton would be a possible
substitute for this purpose. Experiments were made with many
different substances and compounds but the first ones to achieve
any notable success were the Schultze and the E. C. powders. These
won instant recognition as shotgun powders but proved too quick
for use in rifled arms.
About the year 1886, another important step in development of
smokeless powder was made by Vieille, a French chemist. He incor
porated nitrocotton with a mixture of ether and alcohol, and rolled
the resulting paste, a colloid, into thin sheets which were cut into
small squares and dried. Contemporaneous with this work, Nobel
developed ballistite, a powder obtained by gelatinizing a low-nitrated
nitrocotton with nitroglycerin. Shortly after this, a modification
o f ballistite known as cordite was adopted as a smokeless powder.
Ihis propellant consisted of a mixture o f high-nitrated guncotton
gelatinized by means of acetone. In this mixture nitroglycerin and
vaseline were incorporated.
A t the present time all nations use as a propellant either gelatinized
nitrocotton alone or else gelatinized nitrocotton mixed with varying
quantities o f nitroglycerin.
7. Term and fo rm .— a. Application of term.— The term “ smoke-
css powder’ when considered from the exact meaning of the word
is a paradoxical misnomer, for the substance is not entirely smokeless
and it is not a powder.
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b. Form .— Smokeless powder is manufactured in the form o f small

flakes, strips, pellets, sheets, or perforated cylindrical grains. The
last-mentioned form o f grain is the one most commonly used in the
military powders manufactured in the United States. These cylin
drical grains are made with diameters varying from 0.032 inch for
the cal. .30 rifle to 0.947 inch for the 16-inch gun, and in corresponding
lengths varying from 0.085 inch to 2.170 inches. In general, the
smaller caliber weapons are provided with cylindrical powders hav
ing a single perforation running lengthwise through the grain, while
powders having seven perforations are used in the larger caliber
weapons. Triperforated powders have been used experimentally and
a rosette or so-called sliverless grain has been used to some extent;
such forms o f grains are resorted to only when special ballistic
properties are required.
8. M a n u fa ctu rin g p rocesses.— The different processes incident
to manufacture o f pyro smokeless powder may be summarized under
the following heads:
a. Purification and mechanical preparation o f raw cotton. This
includes picking and drying processes.
b. Nitration o f cotton. This is accomplished by treating the cotton
with a mixture o f nitric and sulphuric acid, thus producing a cellu
lose nitrate or “ pyrocotton.”
c. Purification o f pyrocotton from all traces of free acids and
lower nitrates.
d. Mixing o f pyrocotton with ether-alcohol and pressing to form
a colloid.
e. Granulating o f the powder by pressing the colloid through steel
dies.
/. Final processes o f solvent recovery, drying, and blending.
g. Tbe order o f the various steps in the manufacturing processes
for nitrocellulose and for pyro powder are shown in figure 1 and
details o f the various manufacturing procedures are outlined below.
9. P u rifica tion o f raw cotton .— a. (1) Process.— The cotton used
in manufacture of smokeless powder is usually linters, although other
grades o f cotton and wood pulp may be used. The charge o f raw
cotton is cooked in a digester for about 6 hours with a solution o f
approximately 2 percent caustic soda. The digestion is carried out
under a pressure o f about 72 pounds per square inch which cor
responds to a temperature o f 152° C. A fter removing the spent
caustic liquors by washing, the cotton is treated with a solution of
commercial bleaching powder o f about 21/2 percent strength. This
bleaching is carried out at 36° C.. and as short a time as is necessary
6
/ TM 9-2900
MILITARY EXPLOSIVES 9
I' u, uub 1.— Flow sheet for manufacture of smokeless powder.

T M 9 -2 9 0 0
9 MILITARY EXPLOSIVES
to decolorize the fibers is employed. The excess bleach is destroyed

by addition o f a small quantity o f sulphuric acid. The charge is
then washed free o f bleaching agents and dried.
(2) Object.— The object o f boiling with soda and the bleaching
treatment is to reduce the content of vegetable oil, resinous material,
and other extractible substances. It is very important that the alkaline
treatment should not be excessive and that the cotton should not be
overbleached, otherwise the contents of hydrocellulose and oxycellulose
will be undesirably high, as indicated by the test for alkali soluble
described in the specification for cellulose (U. S. Army Specification
No. 50-11-44).
b. Picking.— I f uniform nitration is to be obtained it is essential
that the cotton be o f uniform low moisture content, o f uniform
physical condition, arid that it be free from lumps or any extraneous
material. T o obtain this uniformity the cotton is put through a
picking machine o f which there are various forms. One o f these
machines is provided with a toothed roller which engages the cotton
as it is moving along the feeding table and carries it into such a
position that it is caught’ and torn apart by rows o f sharp hook
shaped teeth set along six evenly spaced elements o f a skeleton cyl
inder revolving at the rate o f 1,000 revolutions per minute. This
operation reduces the cotton to a fluffy state after which it is caught
and blown by an air blast into a large flue leading into the drying
room. A t one portion o f its journey through the flue the cotton
passes through a machine which comprises a system o f W-shaped
flues containing a set o f baffles in the form o f prongs which serve to
fluff out the cotton and separate the fibers from the heavy dust.
This dust settles to the bottom o f bends in the flues whence it is
removed. From this machine the cotton is blown into the dry house-
c. Drying .— (1) Two systems o f drying are in use, one, the con
tinuous drier in which the cotton is conveyed by a. belt through a
long chamber heated to about 100° C., the other by placing the
cotton in a large chamber which is heated by hot air blast. The
former is a continuous operation and the cotton issuing from the
drier is weighed directly into metal containers and transferred to
the nitrating house. Entering cotton usually contains about 8 per
cent moisure. Treatment reduces this to approximately 0.5 percent.
(2) The chamber system is the more expensive of the two and the
least desirable from the standpoint o f time. These chambers are o f
such a size as to hold approximately 2,500 pounds o f cotton. After
the chamber has been filled, it is closed tightly and the heat is grad
ually raised until the temperature reaches 105° C., where it is held
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MILITARY EXPLOSIVES 9 -1 0
for 24 hours. After a laboratory test of the cotton has shown less
than 1 percent of moisure, the dried cotton is weighed in lots of 32
pounds in closed fiber containers which are transferred to the nitrat
ing house by means o f a telpherage system.
10. N itration.—In nitration o f cellulose there are two reactions to
be considered from the manufacturing standpoint. Although these
reactions occur simultaneously, for the sake o f clearness in descrip
tion they are to be considered separately. First, formation of the
nitric acid ester of cellulose, and subsequent removal of water formed
in the reaction by sulphuric acid.
a. Acids.—There are three kinds of acid used in nitrating, namely,
fortifying, fuming sulphuric, and spent acid. The spent acid is that
which is recovered after nitration has been completed. This acid is
built up or fortified by use of a fortifying acid having a strength
o f approximately 50 to 55 percent nitric and 50 to 45 percent sul
phuric. This acid supplies all o f the nitric acid necessary for new
nitration and a portion o f the sulphuric acid. The rest o f the sul
phuric acid is supplied by adding fuming acid of 104 percent H 2S 0 4.
The main function of the sulphuric acid is to combine with water
formed during reaction, and in this manner to prevent dilution o f the
nitric acid. A t the present time mixing of mixed nitrating acids is
generally accomplished by agitation with iron paddles rather than by
use of compressed air.
b. Systems.— Four different systems o f nitration have been used in
this country, the DuPont mechanical-dipper process, the centrifugal
process, the Thompson displacement system, and the pot process. The
mechanical-dipper process has practically displaced the other processes
in this country. The relative proportions of the nitric acid, sulphuric
acid, and water vary not only with the different processes, but also
with change in weather conditions, more particularly o f temperature.
Ihe sulphuric acid content is maintained very nearly constant, and the.
variation in nitric acid is less than 1 percent and is largely accounted
for by the fact that a certain amount o f denitration of nitrocotton
takes place during warm weather. Unless the nitric acid is increased
to take care of this phenomenon, the resulting nitrocellulose will be
below specification requirements for nitrogen content.
(1) DuPont mechanical-dipper process.— (a) The entire cycle of op-
eiation in this process is not more than 35 minutes. Under ordinary
"o ik in g conditions the fumes are negligible, whereas in all the other
ni^ra^ nS systems the fumes are always in evidence so that from the
s anc point of health o f operatives this system is much to be preferred,
pio\ i( ed that, proper care is always exercised in manipulation o f the
machinery.
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TM 9-2900
(Z>) A nitrating unit in this system consists of a battery o f four iron

or stainless-steel nitrators so situated that they can all be handled
from a central point. In each nitrator are two vertical revolving
paddles operated in opposite directions from each other, the motion
being from without inward. These paddles consist o f a series o f hori
zontal arms so placed upon the post that when set in motion the cotton
is quickly drawn beneath the surface o f the acid. A charge o f ap
proximately 1,500 pounds o f acid having a temperature o f 30° C. is
used in each nitrator o f which the following is a fair average com
position: H N ()3, 21 percent; H 2S 0 4, 63 percent; N20 4, 0.5 percent;
HoO, 15.5 percent.
I'lGCRH '1.— Uul’out mecltftnloul-dlpper prongs, nil ration Moor, (.’nrney's Point, N. J.
(c) When the acid has been run in, the paddles are set in motion
and about 32 pounds o f cotton added. The speed o f these paddles is
approximately 60 revolutions per minute. Nitration is continued for
24 minutes, after which the bottom discharge valve is then opened
and the nitrocotton and acid dropped rapidly into a centrifugal
wringer located below the nitrator unit. This centrifugal wringer
rotates slowly at first at about 300 revolutions per minute until the
whole charge is in the centrifuge. The speed o f the wringer is then
increased to about 1.100 revolutions per minute and held at this rate
for 3Yi minutes. The spent acid is run by gravity from the outer
jacket o f the wringer into catch tanks where small amounts o f nitro
cellulose settle out. The spent acid runs from these catch tanks to a
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blow case, and is either blown into mixing tanks or any surplus spent
acid set aside for denitration or other means o f disposal.
(d) The nitrated cotton obtained is forked through a bottom dis
charge o f the centrifuge into an immersion basin below. As fast as
the nitrated cotton falls into the basin it is submerged by a heavy
stream o f water distributed bv fishtail or other form which combines
the greatest dispersion o f water with the maximum force for
submersion.
(e) The pyrocotton, as it is now called, is next transferred by
means of pumps or by gravity to the boiling tub house.
I ' k j u h e 3.— D u P o n t mechuiiirul-Uipper process, wringing centrifugal door. Plcntluny

A rse nti 1. N. J.
(2) Centrifugal process.— In this system the nitrating and the sep
aration o f the spent acid from the nitrated cotton are both carried
on in a large nitrating centrifugal. The latter is filled with a definite
amount o f the mixed acid, usually oO times the weight o f the cotton
charge, at a temperature o f about 32° C., the weighed charge of
cotton (usually 30 pounds) immersed rapidly by means o f an iron
fork and allowed to stand for about 20 minutes, with occasional
turning over by means o f the fork. The drain cock is then opened
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and the spent acid separated by centrifuging, after which the charge
is forked out and drowned as in the mechanical-dipper process.
(3) Pot process.— (a) In the pot process the nitration is best car
ried out in iron pots. These are filled with the mixed acid, the cotton
immersed and allowed to digest for 20 to 30 minutes when the entire
contents are dumped into a centrifugal wringer. The pots are moved
and dumped by means o f a suitable two-wheeled truck conveyer. The;
2X)t process employs considerably less acid than the centrifugal proc-
P iouhb 4.— DuPout mechanical-dipper process, immersing basin and exit flume floor,
Picatiuuy Arsenal, N. J.
ess, about 35 parts o f acid being sufficient to cover the cotton properly.
( b) The charge o f cotton used is generally about 4 pounds. Some
times much smaller pots made o f earthenware are used holding a
charge of only 2 pounds o f cotton, several o f these charges constitut
ing a wringer charge. These small {lots are usually emptied by hand.
(c) The spent acid recovered from the centrifugals is transferred
to storage tanks to be fortified, as has already been mentioned. Its
average composition is approximately H N 0 3, 18 percent; H 2S 0 4, 65
percent; NX).,, 0.5 percent; H jO , 16.5 percent.
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c. Cellulose.-— (1) The exact molecular weight of cellulose is not

known; however, the empirical formula of cellulose is assumed to be
(CeHioOe)*, and it is thus discussed by Marshall as follows:
At first the simplest possible formula was assumed for cellulose, CVHioO«,
und guncotton of high nitrogen content and low solubility In ether-alcohol was
supposed to be formed by the substitution of three NO, groups for hydrogen
atoms, CoHtO»(NO«)s, and was consequently called trinltro-cellulose. The less
nitrated product soluble in ether-alcohol was similarly supposed to be the
dinitro-cellulose C<JInOs(NOj) j. Later workers obtaining evidence of intermedi
ate stages of nitration proposed to increase the formula of cellulose; Eder dou
bled it, Vieille quadrupled it, and Mendeleeff octupled it, giving 48 atoms of car
bon to each molecule, and hydrogen and oxygen in proportion. A nitro-cellulose
having the composition of the above-mentioned trinltro-compound would contain
14.14 percent nitrogen. Quite as much as this has never been found by the
analysis of any product t hat has ever been obtained, but various investigators by
nitrating with mixtures of nitric acid and phosphorous pentoxide, or with con
centrated sulphuric and nitric acids and extracting the product with ether-
alcohol have obtained percentages between 13.9 and 14.4. Lunge and Bebie
found that with mixtures of sulphuric and nitric acids the highest percentage
of nitrogen was attained, not with anhydrous acids, but with mixed acids
containing 11 or 12 percent of water: with a mixture in which the proportions
ILSt).: IINOs: H jO : were 03.35: 25.31:11.34 they produced a nitro-cotton con
taining 13.92 per cent N, but this was not stable. After keeping in the wet state
it was reanalyzed and found to contain then only 13.5 percent N, and other
nltro-cottons nitrated almost as highly were found to decompose rapidly until
the same composition was reached, even though the material was kept under
water. This corresponds very closely with the formula GnHaOjotNOOn, endeka-
nitro-cellulose. Hence the authors conclude that the molecule with 24 atoms of
carbon fits the facts sufficiently well, but point out that this is only the lower
limit of the possible size of the cellulose molecule, as to the real magnitude of
which there is little or no evidence.
(2) The following tabulation shows the percentage of nitrogen and
the volume of NO gas evolved in the nitrometer by the several nitro-
celluloses o f the C2< series (Die ExplosivstofFe mit besondere
berucksichtigung der Neuren Patente Bearbitet von, Dr. Richard
Escales, Leipzig, von Veit, 1914) :
Pnrls C C . No. Percent

Ditrato Designation Formula
per g. N.
12 Dodeka-nitro-cellulose__ __ C 2J I o, O r( N 0 3) i2 . 226. 27 14 14
11 Endeka-nitro-cellulo.se__ 215. 17 13. 47
10 Deka-nitro-cellulose_______ CnHinOintNOllm 203. 35 12. 75
9 Ennea-nitro-cellulo8e______ C j t H s t O n t N O j ) , ’ 190. 75 11. 96
8 Okto-nitro-cellulose. ___ 177. 19 11 11
7 Hepto-nitro-cellulose______ 162. 36 10. 18
6 Hexa-nitro-ccllulose.. ___ 145. 96 9. 15
5 Penta-nitro-cellulose......... .. C^lI-uO.stNO-ib. 127. 91 8. 02
4 Tetra-nitro-cellulose______ C J4H , e 0 IS( N 0 3) 4_______ 107. 81 6. 76
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10-11 MILITARY EXPLOSIVES
(3) A t the present time considerable doubt exists as to the exact

structural formula for cellulose. Some o f the recent investigations
have indicated that the cellulose molecule may consist of extremely
long chains having as many as 3,000 or more o f the ( C J I 10O5) units
in a single molecule. However, it is definitely known that nitro
cellulose is not a true nitro body but is a nitric acid ester, or nitrate
o f cellulose; thus, the term nitrocellulose is a misnomer, but is stand
ard through long usage. The same remarks apply to the terms
“ nitroglycerin” and “ nitrostarch.”
(4) In referring to the several forms o f nitrocellulose, it is custom
ary to speak of nitrocellulose with regard to its nitrogen content
in percentage rather than to refer to it in respect to the number o f
NOa groups present in the molecule as is shown in the tabulation in
(2) above. Paragraph II describes the purification procedure for
pyro nitrocellulose, which when properly prepared contains 12.6
percent nitrogen ± 0.1 percent, and paragraph 12, the manufacture o f
pyro powder from this material. It is important that careful control
o f the manufacturing process be exercised since it is necessary to pro
duce a product uniform in solubility as well as in nitrogen content. I f
this uniformity is not obtained, difficulty is encountered in the subse
quent manufacture o f the pyro powder due to variations existing
in the nitrocellulose. Some control over the viscosity and fineness
o f the pyrocotton is also desirable.
11. P u rifica tion o f p y r o co tto n .— Under the general term o f puri
fication is included the following sequence o f processes: preliminary
boiling, pulping, poaching, screening, and wringing. It is impossible
with the present limited knowledge o f the cellulose molecule and of
intermediate reactions occurring during nitration of the molecule to
control the reaction to such an extent that a nitrocellulose consisting
o f but one nitro body will result from a certain reaction accomplished
under a set o f standard conditions. Products o f the reaction always
include certain nitrocelluloses o f lower nitrogen content and other
impurities. These bodies influence the stability o f the whole mass
and must therefore be removed before the desired stability of the pyro
cotton can be obtained. The object, then, o f the purification treatment
is to insure a uniform stability by eliminating through hydrolysis or
other means these unstable lower nitro bodies and other impurities.
This is accomplished most easily by prolonged boiling in acid water
which in the preliminary treatment has an acidity varying from 0.1
to 0.3 percent calculated as H.SOj.
a. Boiling .—The preliminary boiling process is carried out in
large wooden tubs constructed preferably o f cypress and having a
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MILITARY EXPLOSIVES H
false bottom. In the center of the tub is a square wooden duct rest
ing on the false bottom. This duct serves as a heating chamber for
the water by carrying a centrally located steam pipe. The water
boils in this duct, rises to the top, flows over a false top, and is
distributed through perforations onto the charge o f pyrocotton. The
actual boiling time must be 16 hours. The steam is then turned
off, the excess water decanted, the tub refilled, and boiled again for
8 hours. This is repeated until each tub has had a 40-hour boil with
F kiuke 5. -Roiling tubs for purification of nitrocellulose before pulping, Picatlnny

Arsenal, N. J.
not less than four changes o f water. Careful attention to details

in the boiling tub house insures to the finished pyrocotton a more
satisfactory stability than one in which these details have been
disregarded.
1). Pulping.— The next process, pulping, has for its object reduc
tion o f the pyrocotton fibers to a finer state of division in order
to remove the last traces of acidity occluded by the fibers. The pulp
ing or beating operation is accomplished by machines similar to those
used in the paper industry.
15
T M 9 -2 9 0 0
ll MILITARY EXPLOSIVES
(1) The type o f beater most generally used in manufacture of

nitrocellulose is known as the Jordan engine. This machine consists
o f a series o f broad-bladed knives set in a conical rotor, by means
o f which the nitrocellulose fibers, as they are forced through the
machine along with a large volume o f water, are reduced to the
desired degree o f fineness. The fineness o f the material is indicated
roughly when a handful squeezed free o f excess water shows a clean
break as it is broken in parts. The actual fineness is determined by
laboratory test.
F iuuub (i.— General assembly of apparatus for pulping nitrocellulose showing concentrating
sieve, Jordan engine and feed tank, Picatinny Arsenal, N. J.
(2) Another type o f machine used for this purpose is the Miller
duplex beater. The essential features o f this pulping machine con
sist o f a fixed set o f knives at the bottom o f a tube over which revolves
a roller which is mounted in adjustable bearings and carries a remov
able set o f knives. Pulping is accomplished by the rolls repeatedly
drawing the pyrocotton between the two sets o f knives and thus reduc
ing the material to any desired degree o f fineness. A weak sodium
carbonate solution is used during this process for the purpose o f
neutralizing the acid retained within the fibers o f the cotton and
which is set free mechanically when these fibers are macerated. During
16
TM 9 -290 0
the first stage o f the treatment a washer, consisting o f a large octagonal

box, covered with very fine wire screen, is lowered into the pujp to
remove a part o f the sour water, fresh water being added at the same
time. The water thus removed passes to settling basins, where any
pulp carried off mechanically is recovered. When the desired degree
o f fineness lias been obtained, the material is ready for the next
purifying process.
F igorb 7.— Details of pulping equipment allowing Jordan engine and feed tank, Picatinny
Arsenal, N. J.
c. Poaching .— It has already been pointed out that in the pulping

operation fibers o f the pyrocotton are broken down mechanically so
that the original physical texture o f the cotton is destroyed. Pre
liminary boiling treatment reduced acidity o f the fibers and o f the
interstitial material, but the pulping process by macerating these
240541°— 40------2 17
TM 9-2900
fibers set free an additional amount o f acid. It is therefore necessary

to repurify the pyrocotton by boiling. This operation is carried on in
the poacher house in a manner somewhat similar to that described in
the boiling tub house, but with the notable difference that the first
boiling treatment is carried out in an alkaline solution. For this pur
pose there is dissolved 1 pound of sodium carbonate (soda ash) to a
gallon o f water, and for every 3,000 pounds o f dry nitrocellulose there
may be added 7.5 gallons o f this solution. It is necessary to repeat the
boiling operation five times, but the soda is only added during the first
boiling. All the other treatments are made in a neutral solution.
I'IOUhh 8.— Poaching tubs for purification of pulped nitrocellulose, Picutlnuy Arsenal, N. J.
A fter the boiling treatments the pyrocotton is given at least 10 cold

water washings. During all o f these treatments a thorough agitation
o f the pyrocotton is essential so that it is necessary to employ mechani
cal stirrers driven by gears and shafting. At this stage o f the opera
tion it is necessary for the chemical laboratory to determine—
(1) Stability o f the pyrocotton by K. I. test and heat test at
134.5° C.
(2) Percentage o f nitrogen in the pyrocotton.
(3) Solubility o f the pyrocotton in the ether-alcohol mixture.
(4) Degree of fineness.
(5) Ash.
Details o f perform ing these tests are described in another chapter.
18
TM 9-2900
d. Screening.— A fter purifying the pyrocotton as described above,

it is necessary to separate mechanically any foreign material or any
portions o f the product which may not have been properly macerated
in the beater house. This is accomplished by means o f the Packer
screen. This piece o f machinery consists of a large box, the bottom of
which is fitted with a brass plate having slits 0.025 inch in width. The
pulp is drawn through these slits by suction underneath the screen
and any particles which are too coarse to pass through are returned
to the beater house for additional treatment. From the Packer screen
the pulp is pumped into one o f the large blending tubs where it is
stored until needed in the next operation.
e. Wringing.— (1) Pur pone.—Transference o f the pyrocotton
from the time o f nitration up to this stage o f manufacture is accom
plished by having it suspended in water. It is the function o f the
wringers to remove water from the pulp so that the subsequent opera
tion o f dehydrating by means o f alcohol will be done with minimum
19
T M 9-2900
11-1 2 M ILITARY EXPLOSIVES
amount o f water present. This wringing operation consists merely in

forcing the water out o f the pyrocotton bv means o f centrifugal action.
(2) W ringer.— The wringer consists o f a perforated brass basket
lined with a 24-mesh copper screen. This basket is connected by means
o f a shaft to a motor, which is so geared that the basket revolves at a
speed o f about 950 revolutions per minute. This centrifugal action
forces the water out o f the pyrocotton through the basket and so on
down the drain pipe. The time o f wringing is about 7 minutes. A t
the end o f this operation another sample is sent to the laboratory for
(he purpose o f determining amount o f moisture remaining in the prod
uct. This moisture content averages between 26 and 28 percent.
I f the wringers are operated at a uniform rate o f speed for the
same length o f time moisture content will not vary more than 2 per
cent. This operation concludes the manufacture o f pyrocotton.
12. F o rm a tio n o f c o llo id .— a. Dehydration.— (1) Object .—T he
pyro from the wringers containing approximately 28 percent mois
ture is transferred to storage and placed in warehouses to prevent
freezing in wintertime until it is required for dehydration. The
object o f dehydration is to remove all water from the pyro and to
add in its place the quantity o f alcohol necessary to form the colloid
with the ether which is added later. This amount varies within
relatively small limits and is dependent upon the solubility o f the
pyro being used as shown by laboratory tests, and also to a certain
extent upon size o f granulation o f the final powder. It is customary
to add 114 pounds o f alcohol for every pound dry weight o f
pyrocotton.
(2) Operation.— The dehydrating operation is conducted some
what as follow s: The press consists of a cylinder and movable
piston operated by hydraulic pressure. The press is charged with
pyrocotton and low pressure (about 250 pounds per square inch)
is applied for a few moments, thus squeezing out a portion o f the
excess water. The predetermined amount of alcohol is then forced
into the press by use o f a pump, and the pressure increased to about
3,500 pounds per square inch. The alcohol functions first as an
agent fo r displacing the water in the block and finally as a dehy
drating agent. Its initial entrance into the block forces out
a small portion o f the remaining water; later however, it combines
with the residual water and produces a block o f pyro nearly free
o f water. The first portion o f this alcohol contains relatively large
amounts o f water and is forced out o f the press into the spent
alcohol tank. The remaining amount, however, is about 90 percent
alcohol. The spent alcohol resulting from this process is pumped
20
TM 9-2900
back into the storage tank and eventually rectified with addition
of caustic soda to decompose dissolved or suspended nitrocellulose.
It is then used again either in the dehydrating process or in the
manufacture o f ether.
(3) Solvent required.— The amount o f solvent (ether-alcohol)
necessary to form the colloid is determined from previous experi
ence o f manufacture. The general practice is to vary the amount of
solvent, according to the web thickness o f the powder; thus ap

proximately 105 percent solvent is used in the manufacture o f .30
caliber powder, 100 percent solvent for cannon powder whose web
thickness is approximately 0.025 inch, and about 85 percent for
powder having a web thickness o f 0.185 inch. In the event that 100
percent o f solvent is to be used, or 1 pound of solvent (1 part alcohol
to 2 parts ether) for every pound o f pyrocotton, it is necessary
21
T M 9-290 0
that the usual dehydrating press charge o f 25 pounds dry weight

o f pyrocotton should produce a block weighing 33 pounds 4 ounces
(25 pounds pyrocotton and 8 pounds 4 ounces alcohol).
b. Breaking of blocks.— The dehydrated blocks must be first thor
oughly broken up before the next operation o f mixing is commenced.
For this purpose they are transferred into a rotating drum or block
breaker equipped on the inside with a wire screen and iron prongs.
This barrel upon revolving throws the block against the prongs,
thus breaking it into small lumps which lend themselves more readily
to the mixing operation and which in turn insures a more even colloid.
c. Containers.— From this point up to the time the powder is put
into the solvent recovery (par. 14) the product is kept in closed con
tainers as much as possible between the various steps in the manu
facturing process in order to prevent excessive losses in solvent, which
is an important point not only from the economical but also from
the manufacturing standpoint, since excessive loss o f solvent would
entail difficulty or irregularity in subsequent screening and graining
operations.
d. Mixing .— (1) Operation.— The mixing operation is the next
step in the formation o f the colloid. A s has been pointed out above,
unless care is exercised during the dehydrating process in producing
a block o f uniform dehydration, it will be impossible to secure a
good colloid. It is no less important that the ether be added to the
TM 9-2900
mass in such a manner that the evaporating losses are minimized by

incorporating the ether throughout the mass as quickly as possible.
This is accomplished by use o f a mixing machine. It consists of a
covered water-cooled tank in which two shafts bearing curved agi
tator blades rotate in opposite directions, giving a kneading motion
to the material in the mixer. During this agitation the ether is
poured in rapidly in order to minimize loss o f solvent by evaporation.
(2) Stabiliser.—It is also at this stage o f the process that the so-
called stabilizer is incorporated into the colloid. The material used
for this purpose is diphenylamine, and there is dissolved in the ether
enough o f this substance so that the finished powder will contain
between 0.90 and 1.10 percent diphenylamine. The object o f adding
diphenylamine at this stage is to incorporate it thoroughly through
out the colloid so that on long-continued storage any nitrous fumes
which may be liberated within the powder will be absorbed by this
so-called stabilizer. The many factors entering into the use of this
material are more properly discussed in a later section on surveil
lance and stability.
e. Pressing.— (1) The colloid is next subjected in sequence to ac
tion o f a preliminary blocking press, a macaroni press, and a final
blocking press. Incoi’poration o f ingredients as accomplished in
mixing is really but a preparatory stage for final formation of colloid,
this last step being completed by action o f the presses.
(2) The preliminary blocking press consists merely of a cylinder
and piston similar in action to the dehydrating press. It forms the
colloid into a dense cylindrical mass by subjecting it to a compres
sion of approximately 3,500 pounds per square inch. This so-called
preliminary block is then transferred to the macaroni press. The
operation here consists in straining the solid block o f colloided mat
ter through a heavy brass perforated plate on which are placed one
12-mesh steel plate, two sheets o f 24 and one sheet o f 36-mesh steel
wire screens, at a pressure o f 3,000 to 3,500 pounds per square inch,
in such a manner that the material as it is ejected is similar in ap
pearance and size to macaroni. As it leaves this press it falls by
gravity into the cylinder o f the final blocking press. This is similar
in every respect to the preliminary blocking press and forms the
colloid into final shape before it is taken to the graining press. The
block is here subjected again to heavy pressure (approximately 3,500
pounds per square inch) for 1 to 2 minutes, thus completing the
colloiding o f the pyrocotton. The colloid now is entirely different
in appearance from the material as drawn from the mixers for it
has been changed from a mass resembling light brown sugar to a
23
TM 9-2900
dense, elastic, translucent brown or amber substance. These opera

tions o f pressing insure to the greatest possible degree a uniformly
F igure 12.— Preliminary blocking presses, Carney's Point, N. J.
thorough action o f the solvent upon the pyro, and very nearly elim
inate the possibility o f having uncolloided nitrocotton in the finished
powder.
24
TM 9-2900
13. G raining1 and cutting-.— a. Operation.— The final operation

from the standpoint o f granulation o f the powder occurs in the
graining press room. These presses may be set either horizontally
or vertically. Their action is to force the colloid through a steel
die in such a manner that the. expressed material which takes the
form of a perforated or solid strand will be delivered at a uniform
rate o f speed under control of the operator at the press. The pres
sure which is necessary to force this colloid through the die is very
great and is supplied by means of a hydraulic ram under a pressure
of 2,500 to 3,800 pounds per square inch. The press head may bo
FlGUiitt 13.— Macaroni and final blocking; presses, Picutinny Arsenal, N. J.
equipped with one or more dies depending upon the capacity o f the
graining presses. When small-arms powder is being grained there
may be 36 strands issuing simultaneously from the head. However,
with a large caliber powder such as 16-inch gun it is customary to
use but one die. The powder issues from the press head in the
form of a flexible rope which is led over pulleys to a cutting ma
chine. This cutting machine is capable o f very fine adjustment
and is so manipulated that the length of the grains may be closely
controlled.
b. Size of grain.— Factors affecting size of the grain and its rela
tion to the type o f gun for which it is designed are discussed in
section III.
25
T M 9-2900
14. S olv en t re co v e ry .— a. Pur pone.— The powder as it comes

from the cutter has a definite granular form and contains a consider
able amount o f the ether-alcohol solvent which must be removed.
Hence, the powder is next subjected (o a drying treatment for the pur
pose o f removing the solvent from the powder grains. This drying
process is o f considerable importance in producing a uniform finished
powder, and includes recovery o f a large portion o f the ether and
alcohol solvent remaining in the powder. For this reason the initial
F iu u k u 14. Grain ill); proas room, lMoatliinj' Arsenal, N. J.
process in drying powder is one o f solvent recovery, although recov

ery o f the solvent is only incidental in the powder manufacturing
process.
b. Equipment.— There are three types o f equipment that have been
used successfully in recovery o f solvent and initial drying o f smoke
less powder; first, the chamber type in which the powder is placed
in a metal-lined box provided with a water sealed lid; second, the
car type, which utilizes a solvent recovery car as a drying chamber,
the car being loaded directly from the powder cutters; and third, the
tank type in which the powder is transferred from the cutter room
26
TM 9-2900
MILITARY FA'PLOSIVES 14
to a large metal tank. In all o f these types the operation of removing

the solvent from the powder is the same.
c. Operation.— (1) Warm air is circulated through the powder and
is then forced over cold coils. This change in temperature causes a
precipitation o f the solvent upon the coils and produces in effect a
miniature fog. The saturated air after passing over these cold coils
loses its surplus solvent, is reheated, and then is again forced through
the powder in a continuous cycle, in this manner completing the closed
system o f air circulation. Length of treatment depends upon size of
the powder, the larger calibers requiring a greater length o f time

than the smaller ones. As the solvent is removed from the powder
the grains partially collapse or shrink and it is therefore necessary
to control the rate at which the solvent is removed from the powder
in order to produce a uniform finished product. Furthermore, if the
Solvent is removed too rapidly the surface o f the powder grains
becomes dry and hard, this making more difficult the removal o f the
solvent from the interior o f the grains. Definite rules are laid down
governing the length o f time necessary for powder to remain in the
solvent recovery building, these rules being the result o f experiments
27
T M 9 -2 9 0 0
and combining maximum efficiency with best results from (he stand
point o f drying.
(2) Temperature and times o f heating in solvent recovery proc
esses vary somewhat at different plants. A schedule which has been
followed quite generally is outlined below.
(a) Propellant powders having web thickness up to 0.095 inch—
Raise to 30° and hold fo r 24 hours.
Raise to 38° and hold for 24 hours.
Raise to 45° and hold until total time o f treatment has been 7
days.
F igure 10.— Charging floor, can typo, solvent recovery liouse, Picatinny Arsenal, N. ,1.
( b ) For powder o f heavier web than 0.095 inch—

No heat fo r 48 hours.
Raise to 25° C. and hold for 24 hours.
Raise to 45° C. and hold until total time o f drying o f solvent
recovery treatment has been 8 days.
28
TM 9-2900
T M 9-2 9 0 0
14-15 M ILITARY EXPLOSIVES
It is not practicable from an economic standpoint to reduce the

solvent content o f the powder to the desired degree in the solvent
recovery treatment; hence, the final drying is accomplished as a
separate operation.
d. Ether recovery .—Under normal operating conditions an appre
ciable portion o f the ether in the solvent is lost due to exposure o f
the powder mass to the atmosphere unless means are provided fo r
its recovery. In the more modern powder factories equipment is
installed for recovery o f the solvent vapors from the air.
15. D ry in g ’.—There are two separate types o f drying operations,
the first and most satisfactory, except from the standpoint o f time,
being the air-dry. The second method is known as the water-dry
system and has a great advantage as to time saving.
a. Air-dry treatment.— (1) In this treatment the powder is trans
ferred directly from the solvent recovery house to the dry house
and placed in bulk in narrow bins. The time o f drying varies with
the granulation o f the powder. F or all granulations, however, there
is a heating period o f 30 days at 43° C. The temperature may then
be raised to 55° C. The time required to drive oft' the volatile matter
until the desired total volatile solvent content has been secured varies
from about 30 days fo r the 75-mm powder to 90 or more days fo r
16-inch powder. In the case o f powder having web thickness of
more than 0.095 inch, a period o f at least 2 weeks in the dry house
without heating must precede any heating treatment.
(2) From time to time the laboratory analyzes a sample o f the
powder to determine if the required external moisture and volatile
solvent contents have been reached. The desired external moisture
content for air-dried powders varies inversely as the size o f the
grain from about 0.1 percent to 1.0 percent, while the total volatile
content o f (lie dried powders may vary from approximately 3.5
percent to 7.5 percent, depending upon the web thickness, the heavier
web powders having the greater solvent contents. Control o f mois
ture and volatile content o f finished powders is o f great importance
since rate o f burning and energy content o f powder are reduced as
the amount o f solvent and moisture are increased.
h. Water-dry treatment.— The main difference between the air-dry
process and the water-dry process is the difference in the surround
ing medium. In the first case it is warm air and in the second
warm water, but the object desired is the same in either case. Water
is kept circulating throughout the powder at temperatures which
vary by 10° increments from 25° to 55° C., for approximately 4
days for powders having a web thickness of approximately 0.020
30
TM 9-2900
inch. Later the powder is removed and air-dried for about 48 hours,
this latter treatment requiring much less time to finish than when
the powder has only the air-dry treatment. The external moisture
content o f water-dried powders may vary inversely with the size of
powder from 0.9 percent to 1.4 percent.
c. Continuous drier.— A later development in the powder drying
process is the so-called continuous drier. This differs from the ordi
nary dry house treatment in that drying the powder is accomplished
in between 4 and 5 hours, depending upon size o f granulation. The
powder enters the dry house from the water-dry system, is hoisted
F igure 19.—Interior water-dry house, l ’kiatinny Arsenal, N. J.
to a hopper and then slides by gravity into a shaking screen. This

screen removes foreign material and drops the powder to a bucket
conveyor o f the ordinary type. The powder is then hoisted to the
top o f the building where it is thrown into a drying chute. This
finite is approximately 6 inches in thickness, 5 feet in width, and
about 10. feet in length, and is equipped with baffles running cross
wise in the direction of its smallest dimensions. A series o f screens
on the side wall provides the means for the passage o f warm air
through tile powder; and a temperature o f 50° C. is maintained by
this means at the bottom of the chute. A shaking device near the
floor is capable o f such regulation that the rate o f discharge from
the drier and consequently the volatile content o f the powder is
31
TM 9-290 0
15-16 M ILITARY EXPLOSIVES
controlled by the speed at which this shaker is operated and by the

amount o f clearance between the shaker and the bottom o f the
chute. In one o f the largest, war plants one continuous drier was
capable o f drying to correct moisture and volatile content 100,000
pounds o f 75-mm powder in 24 hours.
16. B le n d in g .— a. Powder Jots.— The next step and an important
one. from the standpoint o f uniformity o f firing is the proper mixing
or blending o f a certain arbitrary amount o f powder. F or the larger
caliber guns it is customary to blend or m ix a complete lot o f 100,000
pounds o f powder, but fo r the smaller caliber powders, particularly
for the small-arms powders, lots ranging from 15,000 to 50,000 pounds
are more usual.
1). Operation and equipment.— (1) The blending operation consists

merely in transference of powder by means o f gravity from one bin
to another, this transference resulting in thorough mixing o f all the
lot. These bins are so constructed that when full o f a lot o f powder
the powder assumes the shape o f a double cone with one apex pointed
down toward the' discharge pipe and the other apex pointed up
toward the top o f the bin. The proper construction o f these bins
from the standpoint o f the correctness o f angles at the sides o f the
bin is very important. I f the sides o f the bin are too steep, the
powder will slide down toward the apex o f the lower cone. I f, on
32
TM 9-2900
the other hand, the sides are built on too gradual a elope the powder
will not flow' freely from the bin and it would be necessary to use a
raking device in order to empty the bin toward the end o f the lot.
It. is essential therefore that a point midway between these two be
found, a point so selected that the powder will not slide down the
side of the bin, yet at the same time will insure a complete emptying
and mixing o f the lot. These angles have been determined and when
the principles are observed no difficulty results from lack of proper
blending. A fter two or three cycles from one bin to the other have
been completed, the powder is weighed and boxed.
(2) Another type o f blender was formerly used at Picatinny
Arsenal. In the place o f two bins set one upon the other as in the
old type— an awkward arrangement which necessitated a building at
least 100 feet high—two separate buildings wrere constructed about
100 feet apart. The bottom of one bin was connected with the top
o f the other by an endless belt. There were then two belts operated
independently o f each other for transference o f the powder from the
bottom of one bin to the top o f the other. The arrangement at the
bottom o f each bin was such that the powder might be boxed in either
building. When it was desired to empty one bin and transfer to the
other for the purpose of blending, it was necessary only to put the
belt in motion and open the chute. The speed of the belt was such
that 100,000 pounds were hoisted in about 75 minutes, a speed not
possible with the older type o f blender. The powder was charged
into a hopper at the base o f one tower from bags if coming from the
dry house, or from boxes if the powder was being reblended, on to
a conveyer belt, carried to the top o f the second tower, and dropped
into the bin until the entire lot had been transferred to this bin.
The conveyer belt at the base o f this second tower was then started,
the powder carried to the top of the first tower, and thence into the
bin, thus completing the cycle. The blending comprised four com
plete cycles.
c. Storage container.— After the blending is completed the lot of
powder is boxed and stored. The powder container used for storage
is merely an airtight zinc box about which is built a wooden box
completely covering and protecting the metal inside. It is o f such a
size as to hold from 110 to 140 pounds o f smokeless powder, depend
ing upon type o f box. These boxes are tested for air leaks to insure
the powder retaining the same moisture and volatile content as when
withdrawn from the dry house. In recent years an all-metal box
lias been used for the larger caliber powders.
l>-»f>!i4T— -40 3 33
T M 9-290 0
17. F N H a n d N H p ow d ers fo r ca n n o n . —a. Development.— At

the outbreak o f the W orld W ar in 1914, the United States Arm y and
Navy employed the same type o f straight nitrocellulose powder, the
manufacture o f which has been described above. A fter the experi
ences in the war certain weaknesses in the standard propellent powder
were recognized:
(1) Hygroseopicity .— The standard nitrocellulose type o f powder if
exposed to the atmosphere is subject to change. The volatile solvent,
F iourk 21. I’owder weighing and packing room, l'lcntinny Arsenal, N. J.
ether-alcohol, used in manufacture is not completely removed, the

powder retaining from 3 to 7.5 percent, depending upon size o f grain.
In a warm, dry atmosphere this residual solvent partially escapes and
the rate o f burning o f the powder is increased. On the other hand, if
the powder is exposed to a humid atmosphere, it absorbs moisture and
the rate o f burning is decreased. Thus, ballistic properties o f the
powder are appreciably affected by changes in atmospheric conditions
to which the powder may be exposed.
(2) Flash.— Another objection to the pyropowder was the fact that
when fired it produces a large, brilliant flash at the muzzle o f the gun.
34
TM 9-2900
This proved to be a serious objection during the W orld War owing

to the great amount o f night firing conducted, since the flash aided
the enemy in locating positions o f the guns.
The need was recognized for a nonvolatile, nonhygroscopic, and
flashless powder which would still retain the property o f being sub
stantially smokeless. Such powder has been developed since the W orld
War, and is designated FNH if flashless, or NH if used in weapons in
which flashlessness is not attained.
Eiuuuu 22.— Piual air testing of powder boxes, l ’ieutinny Arsenal, N. J.
b. FNII powder.— (1) The FN H type of powder has been obtained

by adding to the nitrocellulose inert or partially inert materials for the
purpose o f cooling the products o f combustion and reducing the hy-
groscopicity o f the powder. Such a powder may be flasliless in cer
tain weapons but not flashless in others, since flashlessness is dependent
not only upon composition o f the powder, but upon relationship be
tween quantity o f powder used as a charge and length o f bore o f the
weapon, weight o f projectile, etc. W hile it might appear possible to
obtain flashlessness in any weapon by merely increasing the amount
35
TM 9-2900
o f flash-reducing agent in the powder composition, such a procedure

may be impracticable either because o f increased smoke produced or
reduction in potential o f the powder. While the present type o f FNI-I
powder has a lower potential than the standard pyroeellulose powder,
it has sufficient potential to permit its use in all weapons without
change in ballistic requirements.
(2) Tho manufacture o f the FN H powder can be carried out in
the same equipment and plant used for manufacture o f the standard
pyroeellulose powder. However, details o f the processes fo r the two
types o f powder differ in many respects.
S ection III
G R A N U L A T IO N O F SM O K E LE SS P O W D E R
P aragrap h
Genera!----------------------------- ----------------------------------------- ---------- -------------- 18
Korin and size of grains-- _____________________________ ___ - ________ 19
Control of grain dimensions in powder manufacture_____________________ 20
18. G en eral.— The propellent powder used as a charge for the gun
possesses a certain force or latent power which upon combustion
becomes a kinetic or moving force which drives the projectile from
the muzzle o f the gun. When powder is ignited it undergoes chemical
decomposition and is converted by change o f state, that is, from solid
to gas, into a volume greater than that originally occupied by the
powder. Simultaneously with this change o f state, the heat generated
by the explosion expands the volume o f gas produced and increases
its pressure, and finally sets the projectile in motion.
Rapid development o f gas pressure within the gun should be o f such
a progressive nature that the force exerted does not attain its maxi
mum at time o f ignition (as would be the case if a high explosive
in its usual form were used as a propellant), but rather attains it by
a relatively gradual rise. Control o f this pressure lies in the com
position o f the powder, form or shape o f individual powder grains,
and size or dimension o f any particular form o f grain. Granulation
determines the area o f the burning surface o f (he grain which in turn
controls rate o f combustion, and through that, the pressure.
A brief consideration o f factors influencing and determining proper
granulation o f powder will involve discussion first, o f the best form
o f powder grains and second, factors which determine size o f grains.
19. F o rm a n d size o f g ra in s .— a. Form .— (1) Ballistic require
ments.— The best form o f granulation from a ballistic point o f view
is first, that which with the smallest weight o f charge will impart to the
36
TM 9-2900
projectile the prescribed muzzle velocity within the permitted limit o f

maximum pressure; second, that which will cause minimum erosion to
the bore; and third, that which shows maximum regularity in ballistics.
The grains burn uniformly from the surface and the rate o f burning
varies directly with the pressure; the greater the burning surface, the
Ficuiu: 24.— Cross section ot multiperforated powder grains.
higher the pressure, other things being equal. The shape of the grain
is a direct factor in determining the total amount o f burning surface of
a given weight o f powder.
37
TM 9-290 0
19 M ILITARY EXPLOSIVES
(2) Types .— Smokeless powders are granulated in regular geomet

rical forms o f various sizes and lengths. The principal forms in use
are the solid cord, the flat strip, the single perforated cylinder, and
the multiperforated cylinder shown in Figure 23. The most im
portant dimension o f these grains is the “ web” thickness or minimum
thickness between any two parallel surfaces.
(3) Burning art ion.— (a) Since smokeless powder o f any grain
form burns only on the surface and in parallel layers perpendicular to
the surface, it is readily apparent that the extent o f change o f surface
o f the powder grains as they are consumed varies widely among the d if
ferent grain forms. Thus, grains in form o f cords or strips burn with
a continually decreasing surface until the grains are entirely con
sumed, whereas the multiperforated grain burns with a continually
increasing surface until it is nearly consumed; although the exterior
surface o f the multiperforated grain decreases in area during burning,
the interior surfaces formed by the perforations increase during burn
ing so that the net result is an increase in burning area until the grains
are largely consumed. A ny form o f grain which presents a decreas
ing surface area during combustion is termed a degressive burning
grain, while all form s which present an increasing surface as combus
tion progresses are styled progressive burning grains. Since tubular
or single perforated grains show only slight change o f surface during
combustion, they are usually referred to as neutral grains.
(&) Figure 24 shows that when the inner and outer webs o f the
multiperforated grain have burned through, pieces o f triangular cross
section called slivers remain unburned. When 7 perforations are
present, 12 o f these slivers are produced, these constituting about 15
percent o f the total weight o f the grain. These slivers burn degres-
sivcly and are usually consumed in the bore o f the weapon but if this
is relatively short or if a reduced charge is fired and thus relatively
low pressure is developed, the slivers may be expelled unburned from
the muzzle. The form o f grain known as the Walsh or rosette grain,
(fig. 23) having the usual 7 perforations but with the outer periphery
o f the grain scalloped, has been used in some seacoast mortars. This
type o f grain reduces amount o f slivers and therefore reduces or elim
inates amount o f nnburned powder ejected from the weapon.
(4) Use.— (a) Multiperforated .— The United States Arm y and
Navy have favored the use o f the multiperforated grain form since its
small initial burning surface per unit weight o f powder results in a
slower rise o f pressure during initial stages o f combustion. This
slower rise o f pressure allows maximum pressure to be developed at a
point farther from the breech than is obtained with the degressive
38
T1VE 9-2900
type o f grains. Our guns are designed to withstand a pressure in

creasing to the maximum at a point in the bore just ahead o f the
powder chamber. With the maximum pressure at this point, a higher
pressure is exerted on the projectile throughout its travel to the muzzle
than would be the case if the peak pressure occurred in the powder
chamber.
(b) Mingle 'perforated.— Single perforated powders are used for
United States small arms, minor caliber cannon, and for certain
howitzers largely because o f the difficulty in extruding a multiper-
forated powder when exceptionally thin webs are required to meet
ballistic requirements.
b. Size.— (1) Weapon factore.— In general, for any given grain
form the size o f grain to be produced depends on the type of weapon
in which it is to be used. It. is generally true that the web thickness
o f powder must increase with the caliber or power o f the weapon.
The ratio o f web tliickness to caliber is not the same, however, fo r
the different classes or types o f artillery weapons, namely, guns,
howitzers, and mortars. This is due to the marked difference in the
ratio o f the length o f the tubes to the caliber o f the tubes among the
various weapons.
(a) Length .— In comparing the three types o f weapons as to length,
the gun is the longest, its length ranging from 40 to 60 times the
bore o f the gun (calibers) ; howitzers are medium in length, and
mortars the shortest. Therefore, the mortar type would require a
powder with a larger burning surface and hence smaller granulation
than either a gun or a howitzer o f the same caliber, However, the
gun as a class gives the highest degree o f accuracy, permits the
longest travel of the projectile, and imparts the highest muzzle
velocity. The seac.oast mortars are short guns and in firing them
there is always a large amount o f unburned powder slivers thrown
from the muzzle, except when the sliverless or Walsh grain is used.
This grain, as has been pointed out before, by providing a larger
burning surface burns more quickly and thus practically eliminates
this undesirable feature.
(b) Caliber.—The calibers o f seacoast weapons range from 3 to 16
inches and are permanently mounted in fortifications. Field weapons,
or mobile artillery, are designed to accompany or follow an army
in the field, and are smaller in caliber except in some o f the railroad
mounts. Depending upon the type o f weapon, however, granula
tion o f the powder must be so controlled that the functions o f the d if
ferent weapons are best served. Howitzers arc used only in mobile
39
T M 9 -290 0
artillery. “ For each caliber o f gun there is designed a corresponding

howitzer o f an equal degree o f mobility, and the caliber o f each
howitzer is the same as that o f the gun o f the next lower degree
o f m obility; that is, the howitzer corresponding in mobility to one
o f the guns is o f the same caliber as the next heavier gun and uses
the same projectile.” (Tschappat.) (See par. 89.)
(e) Powder chamber capacity.—Since each type o f gun has its
specified size o f powder chamber, it is necessary to ascertain this
capacity before designing the granulation o f the powder. Other
factors being equal, the greater the capacity o f the powder chamber,
the greater the size o f the powder grains. For instance, the capacity
o f the powder chamber fo r the 12-inch mortar, M1890, is 2,674
cubic inches, and 12-inch mortar, M1912, 3,77n cubic inches, using the
same weight projectile (700 pounds). The “ average web” fo r M1890
is 0.0600 inch and for M1912, 0.0760 inch.
(2) Web.— The term “ web” referred to in (1) (c) above is the
measure o f powder grain size most commonly considered in design
work. It is defined as the least burning thickness from the edge o f
one surface to the edge o f the next surface in the diametric direc
tion. The “ average web” is the mean o f “ inner” and “ outer” webs
(multiperforated grains). Relatively slight adjustments in the
average web o f a powder result in appreciable changes in required
weight o f charge and resultant maximum pressure (velocity remain
ing constant).
(3) Final- dimension factors.— In establishing size o f powder
grains for a particular weapon, the principal features which affect
final dimensions o f the grains are weight o f the projectile, prescribed
velocity, weight o f charge, and percentage o f moisture and volatiles
allowed to remain in the powder.
(a) Effect o f pi'ojectile eight and prescribed velocity.— In gen
eral, the heavier the. projectile or the higher the prescribed velocity,
the larger the powder grains required, holding the maximum pres
sure within the proper limit. “ An increased weight o f projectile will
result in an increased maximum pressure in the gun if the same muz
zle velocity is to be maintained with the same powder, size o f powder
chamber, and length o f travel. The maximum pressure for any
gun being fixed, the use o f a heavier projectile will usually require
the use o f a slower powder, and if the increase in weight is very
great it will require an increase in the size of the powder chamber,
or in the length o f the gun, or in both dimensions.” (Tschappat,
p. 518.)
40
TM 9-2900
(b) Relation between weight of charge and grain dimensions.—

By varying the web thickness o f the powder for any given weapon
and projectile, it is possible to alter appreciably the weight of pro
pelling charge to meet ballistic requirements. For example, pyro
powders have been accepted for use with the 12.7-pound projectile
in the 3-inch antiaircraft gun, with weights o f charge varying from
4.88 to 5.GG pounds. This variation in weight o f charge resulted
from variation in the web thickness o f the lots which ranged from
.0339 inch to .0444 inch. The pressure o f course was higher for the
powder of lower web, being 34,000 pounds per square inch as com
pared to 28.700 pounds per square inch for the heavier web.
From an economic standpoint it is obviously desirable to maintain
the weight of charge as low as practicable, and hence from this
standpoint as thin a web should be used as is compatible with pres
sure requirements.
In the case of zone charges especially, it is desirable to granulate
the powder with as thin a web as practicable, so that higher pressures
will be obtained in firing the inner zones. Better velocity uniform
ity is commonly obtained at the higher pressures.
(c) Effect of moisture and volatiles.—A fter graining, the bulk o f
the solvent is dried out, but 2 percent to 8.5 percent may remain in
pyro powder as moisture and volatiles or total volatiles, the amount
depending upon size of the grain. No better description of the effect
of moisture and volatiles can be given than the following from
Tschappat, page 115 1 1
The alcohol used iu the solvent contains 5 percent water, which generally
remains in the powder after drying. Additional water may be absorbed from
(lie air during the process of manufacturing and handling. Recent lois of
powder also contain approximately 1 percent of a stabilizer, and .30 caliber
rifle powders contain, in addition, a small percentage of graphite.
Smokeless pyro powder may, therefore, be considered to be a mixture of
nitrocellulose, alcohol, water, and sometimes a stabilizer and graphite. Most
of the ether used is evaporated out during (lie drying process.
Prom calculations it is found that the energy per pound of pure nitrocellulose
of 12.60 percent nitrogen is about 1,425,000 foot-pounds per pound. If now, an
inert material, that is, one that takes no part in the reaction at combustion, is
mixed with the nitrocellulose, (he energy per pound of the resulting material
will be less than that of pure nitrocellulose. For instance, if 0.99 pounds of
pure nitrocellulose of 12.60 percent N is mixed with 0.01 pound of inert material,
the inert material will be 1 percent of the total weight and tlie energy per
pound o f the resulting material will evidently be 1,425,000 X 0.99=1,410,750 foot
pounds per pound.
Now, of the materials entering powder as given above, water is considered
as having the same effect as the same percentage of inert matter. Alcohol lias
5 Data slightly revised to bring up to date.
41
TIYE 9-2900
a greater effect; than inert matter for the reason that the carbon contained in
it combines with the C 0 2, resulting from the combustion of the nitrocellulose,
thus forming a larger quantity of CO and a smaller quantity of C 03, than in
the combustion o f pure nitrocellulose. Theoretical considerations and practical
tests indicate that the effect of 1 percent alcohol in reducing the energy per
pound o f nitrocellulose is equal to the effect of 2.5 percent inert matter.
In the same way the effect of 1 percent stabilizer, which is higher in carbon
(.ontent than alcohol, is shown to be equal to the effect of 4 percent inert matter.
Graphite, though entirely carbon, does not readily take part in the reaction and,
therefore, the effect, of 1 percent graphite in reducing the energy per pound of
nitrocellulose is considered equal to that of 2.5 percent inert matter.
Consequently, the granulation of the powder must be so calculated
that it will counteract the reduction o f the energy o f the powder by
the solvent remaining after drying. In order to give more energy,
the burning surface should be increased by diminishing the average
web measurements or the size o f the grain, or by changing the form
o f the grain.
20. C on trol o f g ra in d im e n sio n s in p ow d er m a n u fa ctu re .—
a. Specification requirements.— U. S. Army Specifications for cannon
powder contain the following general requirements regarding dimen
sions of powder grains, such requirements being established to
control bulk density of the powder as well as burning characterictics:
(1) Mvltiperforated grains.— (a) Average grain length (L ) shall
be from 2.10 to 2.50 times average grain diameter (D ).
(&) Average grain diameter (D ) shall be approximately 10 times
average diameter o f perforations (d ).
(c) Difference between average outer web thickness (W o) and
average inner web thickness (W ,) shall not exceed 15 percent o f the
web thickness (W a).
(2) Single perforated grains.— (a) Average grain length (L ) shall
be from 3 to 6 times average diameter (D ).
(&) Average grain diameter (D ) shall be approximately 3 times
average diameter o f perforation (d ).
l>. Dies .— (1) Description.— Figure 25 shows the general design o f
die through which the multiperforated powder is extruded from the
graining presses during manufacture. As the powder comes from
the training press it contains from 10 percent to 50 percent solvent
and is called “ green” because the solvent has not been extracted by
the drying processes. The green powder has about the same dimen
sions as the steel die through which it has just been pressed. The die
body A consists o f a steel block designed to hold the pin plate B, the
water jacket C (having an inlet and outlet for water used for cooling
the die while running the powder) and a closing screw D for the
water jacket. The pin plate consists o f a perforated plate to which are
42
TM 9-2900
attached wires or pins E, which form the perforations in the grain,

and the plug F , which holds the pins in place when the die is not in
use. The dimensions for both the die body and pin plate are called
die dimensions.
(2) Dimension determination.— (a) General factors.—It is neces
sary to calculate the dimensions o f the die very accurately, as there
are many factors which cause the measurements o f the green powder
to differ from those o f the die. Among these factors is the spring
o f the pins (or needle wire) by which action the pins are drawn
together as the powder is being pressed through the die, and which
lias the effect o f decreasing the inner web. Another factor is the
consistency of the powder as it is being grained. The softer the
powder, the more it will contract as it goes through the die, thus
causing the green dimensions to be less than the die dimensions.
DIA. O F G R E E N G R A IN - W ATER J A C K E T - C M ATER IN L E T ,
2 5 ' P IP E T A P
PIN P LA TE PERFORATED
WITH SUITABLE .S IZ E
HOLES. S 3g5555555553S g5S S S 3
'IH S -B
//
PIN PLATE - B
D IE B O D Y -A P lN S - E CLOSING S C R E W -0
W A T E R O U TLE T, . 2 5 " P IP E TA P .
PtyniFi 25.— I'owder die assembly used for cylindrical grains.
(b) Powder shrinkage.— In order to determine the size of die re

quired to manufacture a powder of given dry web, it is necessary to
know the extent to which the powder will contract or shrink after the
solvent has been removed. The shrinkage is expressed as the per
centage reduction o f a given dimension such as the web (W ) from the
green to the dry form. The percentage shrinkage for the various
dimensions varies considerably; for example, the shrinkage in length
o f grain may be as small as 5 percent, while the web shrinkage may
vary from 25 to 35 percent. The shrinkage for the inner web (W ()
for multiperforated powders is usually less than the shrinkage for
the outer web (W 0) ; furthermore, the percent shrinkage will vary
considerably with composition, quantity o f solvent, physical charac
teristics o f the nitrocellulose, and size of grain. The shrinkage which
occurs when the various grain sizes are manufactured according to a
standardized procedure is determined by the actual manufacture o f
small experimental lots o f the approximate grain sizes involved.
TM 9-2900
Once the dry dimensions are decided upon and the percent shrinkage
known for a given composition and manufacturing procedure, the
powder can be made with a reasonable assurance that it will dry closely
to the size expected.
(c ) Method.—The follow ing problem and calculations illustrate
the method used for the determination o f die dimensions to manu-
Wo = Wi + 57. Wi
Ife-i
D ‘ O U T S ID E D IA M E T E R
d = D IA M E T E R O F P E R F O R A T IO N
W o 'O U T E R W E B
W i = IN N E R W ES
CYLINDRICAL GRAIN SINGLE PERFORATION

D RY D IM E N S IO N , 0 ' 3 d
D - O U T S I D E D IA M E T E R
d - D IA M E T E R O F P E R F O R A T IO N
F igure 26.— Grain perforations.
facture a powder o f any given dry dimensions. The symbols used in

these calculations are described in figure 26. When the symbol refers
to a green dimension, it. is followed by the letter “ g” and when it
refers to the dry powder dimension, it is followed by the letter “ d.”
Problem .— A die is desired for the manufacture o f a powder o f the
multiperforated grain form to have an' average dry web (W art) o f
0.0220 inch and a dry perforation diameter (d a) o f 0.0127 inch. The
U
TM 9-2900
shrinkages for this composition are perforation, 21.0 percent; outer

web, 35.0 percent; inner web, 25 percent.
Solution.—Pin size (dg) = 0 .0 1 2 7 (1 0 0 —21) X 100=0.01606 inch.
It is considered desirable to manufacture powders with outer web
(W „d) slightly larger, usually about 5 percent, than the inner web
(W io ); therefore, the outer web will be 2.5 percent greater than the
average web or 0.02255 inch, while the inner web will be 2.5 percent
less than the average web or 0.02155 inch.
Since it is apparent from figure 20 that the bore diameter o f the
die, which is equal to the diameter o f the green grain (D g ), is the
sum o f the thickness o f the green inner and outer webs plus the
diameter o f the green perforations, it is necessary to determine the
green dimensions o f the inner and outer webs. The green outer web
PA M-8524
I
FmuiiB 27.— Die body, i>in plnte, water jncket, mid smokeless powder Strains for 155-nun Kun.
(W ..J is calculated as follows: 0.02255 : (100 —35) X 100= 0.0357 inch.

The green inner web (W iE) then is calculated similarly as 0.0287 inch.
With the above data, the bore diameter (I)K) becomes 3(0.01606) +
2(0.0287)+2(0.0347), or 0.17498 inch.
It is now necessary to calculate the diameter o f the circle on which
the centers o f the pins must be set in the pin plate. This dimension is
referred to as pin circle diameter and is equal to 2 (W ls) + 2 (d g ) which
in this case is 0.0895 inch.
There remains yet the length of grain or the cut to be determined.
Since the shrinkage in length is small and since the ratio o f length
o f grain to diameter may vary from 2.10 to 2.5, the green diameter
(I)K) may be multiplied by 2.5 to obtain the length o f cut. I f a closer
controlled length of cut is desired, the shrinkage in length must be
known and the green length calculated accordingly.
45
TM 9-2900
2 1 -2 2 MILITARY EXPLOSIVES
S e c tio n IV
STABILITY AND STORAGE OF SMOKELESS POWDER

Paragraph
General__________________________________________________________________ 21
Stability tests--------- ---------------- 22
Causes of Instability— ________ 23
Stabilizers___________ 24
Storage--------------------------------------------------------------------------------------------,--------- 25
Shipment-------------------------------------------------------------------------------------------------- 26
21. G eneral.— The subject o f stability o f smokeless powder in

volves both safety in storage and uniformity in ballistics. In the
discussion upon the purification o f nitrocellulose it was pointed out
that the processes o f boiling are made necessary from the fact that
a pure product, or more properly one. definite nitrate, cannot be
prepared. Present knowledge o f the cellulose molecule and o f in
termediate reactions occurring during nitration o f the molecule
limits any attempt at preparation o f a single nitrate, and while
complete hydrolysis o f lower nitrates is sought in the boiling proc
esses, there is no assurance that this reaction is the only one con
cerned, nor is it proven that there are not other factors influencing
speed and completeness o f the reaction. In spite o f the elaborate
process o f purification followed out to insure stability o f the finished
powder, this program is extended by incorporating hi the colloid
1 percent dry weight o f diphenylamine.
22. S ta b ility te sts.— The nitrocellulose for use in making powder
is said to be stable or is said to have good stability when it passes
the K I test and the heat test at 134.5° C., while the stability o f the
finished powder is determined by means o f the heat test at 134.5° C.,
and the test in the surveillance chamber, which is maintained at a
temperature o f 65.5° C.
There is no test, however, o f the stability o f smokeless powder
which is infallible, or which indicates in more, than a general way
the safety o f the powder from thei storage standpoint. The idio
syncrasies and the unreliability o f the KT test are too well known
to require more than passing mention. The heat test at 134.5° C.
serves as a criterion for the incomplete hydrolysis o f the lower
nitrates and for the presence of sulphuric esters (cellulose sulphates).
Such impurities are capable o f giving a low test for “ salmon pink,”
or an early explosion in this test. The surveillance tests o f smoke
less powder are not entirely satisfactory from the standpoint o f
uniformity o f results and also from the standpoint o f elapsed time
necessary to obtain any data.
46
TM 9-2900
MILITARY EXPLOSIVES 22-23
The principal weakness o f the above tests, however, is that they

involve the use o f only small samples which may not he truly repre
sentative o f the large quantity o f powder comprising a lot. Since a
powder lot is commonly a blend o f portions which may not be in
precisely the same condition as regards stability, it is often un
certain whether variations in the results o f stability tests are due
to the test methods or to actual variations in the condition o f the
powder comprising the lot.
23. Causes o f in sta b ility .—All organic compounds can be decom
posed by heat. Explosives in general are. chemical compounds which
undergo decomposition when subjected to only moderately elevated
temperatures, most o f them being unable to withstand prolonged
exposure to a temperature as high as 200° C. The resistance o f
such compounds to decomposition by heat is an inherent property
dependent upon the structure o f the molecule as is color, melting
point, odor, etc.
Nitrocellulose is one o f the least resistant explosives to heat that
is used in military ammunition. Since nitrocellulose is the essential
constituent of smokeless powder, the stability o f the latter is deter
mined largely by the nitrocellulose, and the powder consequently
has relatively low resistance to heat. Decomposition o f smokeless
powder is so rapid above 200°- C. that spontaneous ignition will
occur within a few minutes. The rate o f decomposition is reduced
as the temperature is lowered until at atmospheric temperatures
only very slight decomposition will occur over a period o f many
years, provided the powder is not subjected to influences other than
temperature which tend to promote its decomposition.
Any chemical compound can be decomposed by reaction with cer
tain other compounds. The reactivity o f compounds is also an in
herent property depending upon the structure o f the molecules.
Nitrocellulose, being an organic ester, possesses the characteristics
o f esters in general and can be decomposed by boiling water, such
decomposition being promoted if acids or alkalies are present. The
reactivity o f nitrocellulose with water, acids, and alkalies is o f
special importance because o f the use o f these compounds in the
process o f manufacture. It is essential that they be thoroughly
removed before the nitrocellulose is manufactured into powder; other
wise, the normal rate o f decomposition produced by temperature
effects will be increased by reaction o f the material with the im
purities remaining in the nitrocellulose.
In the nitration o f cellulose, the nitrating mixture o f nitric and
sulphuric acid acts on the impurities contained in the cellulose as
well as on the cellulose itself. Thus, cellulose sulphate and sulphates
47
TM 9-290 0
or nitrates o f oxycellulose, hydrocellulose, and other cellulose com

plexes may be formed as impurities in the nitrocellulose. Such im
purities are also decomposed by heat and some o f them are indicated
to be more readily affected than nitrocellulose. Hence, their presence
tends to reduce the stability o f the nitrocellulose and o f powders
made from it.
From the above discussion it is evident that to obtain nitrocellulose
o f maximum stability, great care must be exercised to eliminate im
purities which are formed in the nitration process and also any acid
or alkali which is present during the purification treatment. In order
that powder made from such nitrocellulose will exhibit the maximum
degree o f stability under any temperature conditions in storage, it is
necessary that the powder be protected from reaction with moisture
or other materials which react with nitrocellulose.
24. S ta b ilize rs.— Prior to 1908 little was done from the manufac
turing standpoint to standardize methods o f purification then in prac
tice. In fact, the importance o f the whole subject o f stability o f
explosives was not recognized to the same extent as at present and
consequently had not received the same consideration. In mixing
the colloid it was the practice to incorporate a small amount o f an
organic dye which served the purpose o f an indicator rather than
a stabilizer.
The indicator which found the widest application was rosaniline,
and its adoption was due to the fact that upon development o f any
marked acidity produced from decomposition o f the smokeless powder,
the red color o f the dye in the powder grains faded to a yellow, which
fact served to indicate instability.
Use o f diphenylamine was not general until the latter part o f
1908, and its function was different from that o f rosaniline, for it.
has the property o f combining with free N 0 2. Upon development o f
the free oxides o f nitrogen in smokeless powder, the diphenylamine
undergoes progressive nitration (Buisson, p. 117‘2) (see par. 89), as
indicated in the follow ing series o f reactions:
(G>KU)2NH (C-HshN.NO a m (NO=).N( NO ).('«&>
diplieiiylamiiie diphenyl-nit rosamine nitro-diphenyl-nilrosaminc
(C «H iX 02) jNH C JL (NO-) .NH.C<Hi (NO j) j
dinitro-diphenylamine trinitro-diphenylamine
These separate substances may be detected by various quantitative

and qualitative reactions, and it was formerly thought that when any
o f the tests applied to the powder were positive, they indicated an
impaired stability. However, more recent work has indicated that
nitrosodiphenylamine itself is an excellent stabilizer so that the p re s-.
48
TM 9-2900
MILITARY EXPLOSIVES 2 4 -2 5
ence o f nitrosodiphenylamine does not necessarily indicate impaired

stability.
25. Storage.— It has already been pointed out that moisture and
volatile content o f smokeless powder are important factors in deter
mining weight o f charge and pressure to be expected for required
muzzle velocity. In order that, this percentage will remain constant
it is necessary that the powder be stored in airtight containers so con
structed that they may be easily Idled, tested, piled, and emptied.
With small-arms powder it is customary to line the inside o f the con
tainer with a muslin bag, the object being to keep the powder entirely
free from dust, chips, or other extraneous material.
a. Containers.— (1) Description.— (a) The powder container con
sists o f a wooden box, zinc-lined, about 26 by 16 by 11 inches. There
are two types, the so-called export type, having a capacity of 140
pounds, and the other, the Picatinny Arsenal type, having a capacity
o f 110 pounds. The cover is provided with an outside ring, locking
ring, and rubber gasket, assembled in such a way that when a lever
is forced down on the top o f the box, tension is put upon the lug in
such a manner that there is no possibility o f air leaks. Each box is
tested before being filled by having a small hole drilled in the cover,
applying compressed air, and noting the reading on the pressure gage
attached to the air line.
( b ) In recent years a steel container has been standardized for
storage o f the larger granulation o f cannon powder. These have the
advantage o f more substantial construction and, hence, less expense
for inspection and repair to guard against air leaks.
(2) Testing.— In order to detect the presence of deteriorated pow
der and remove it from storage before spontaneous combustion can
occur, each box in storage over 5 years old is tested by inserting a
strip o f tenth-normal methyl violet paper above the powder. This
paper is examined and replaced by a fresh strip each year. The con
tents o f any box in which the test strip becomes bleached in 12 months
or less is considered hazardous for continued storage and is removed
and disposed of. Since this test was instituted not one single fire due
to deteriorated powder has occurred.
(3) Piling.— In piling, the boxes are placed on their narrow sides
at an angle o f about 20°, so as to permit removal o f the lids and
insertion o f the methyl violet test, papers without removing consider
able powder from the boxes. They should not be piled closely
together for the reason that such a procedure defeats proper venti
lation. The boxes are commonly piled 6 high, this being about all
the usual magazine space permits.
249541*— 40----- 4 49
TIYE 9-2900
b. Magazines.— (1) Temperature.— Magazines fo r storage o f smoke

less powder should he kept, dry, and should lie so situated that there
is a minimum variation in temperature. This latter point is an im
portant one from the standpoint o f maintaining standard moisture
and volatile content. In those instances where a wide range in tem
perature obtains there is always the added risk o f the powder
containers tending to develop leaks, due to the difference in the
atmospheric pressure inside and outside the zinc boxes. The most
satisfactory storage conditions are those which insure a free circula
tion o f cool, dry air. Therefore, ventilation o f the magazine is a very
important point and should lie so controlled that air will not bo
admitted when conditions on the inside o f the magazine are such
that condensation o f moisture within the magazine would follow.
The zinc-lined containers should be handled the least possible num
ber o f times, and whenever such handling is necessary it should be
done with the greatest care, the object being to obviate any possibility
o f air leaks being produced in the containers.
(2) Cleanliness.— The important preliminary detail o f cleanliness
o f the magazine floor should not be overlooked, for the accumulation
o f dirt, rubbish, and nails, aside from being unsightly, constitutes a
menace. Scrapers should be placed at the door o f the magazine so
that mud, cinders, gravel, or other material will be removed from
the shoes before the powder is stored. Under ordinary conditions
it is not necessary to wear powder shoes in the magazine, except in
the case o f repacking, when it is advisable that this precaution be
observed.
(3) Location.— Magazines must be so located that good drainage
o f the land is possible at all times. This is of special importance
where large quantities o f smokeless powder are being stored. In
spite of the precaution observed for the elimination of leaky powder
cans, the fact remains that there are many instances where the leaks
are not discovered. This results, o f course, in the powder in such
cans absorbing moisture from the damp atmosphere in which it is
stored, a condition very undesirable from the ballistic standpoint.
(4) Fire precautions.—The fire risk is not. o f serious consideration
if the necessary precautions are observed. The danger o f grass fire
is practically nil if brush and undergrowth are removed from a
distance o f 50 feet around the building. Carrying matches or flash-
producing devices o f any kind should be strictly prohibited. This
rule may be enforced by having those employees associated with
50
TM 9-2900
MILITARY EXPLOSIVES 25-26
the storage depot searched for matches in their clothes at irregular

intervals. Smoking, of course, should be absolutely forbidden at all
times where explosives are manufactured, tested, or stored. O il
burning lamps, lanterns, candles, etc., should be prohibited, and in
those cases where artificial light is required special storage-battery
lamps only should be used, or for short inspection the ordinary dry-
battery flashlight.
c. General safety regulations.— (1) When it is necessary to renail
boxes, nonsparking tools should be used. These consist o f copper
hammers, wooden mallets, copper nails, etc. Use o f metal hooks for
moving packages of high explosives or ammunition should not be
permitted.
(2) When circumstances are such that it is impossible to get ex
plosives under cover, a tarpaulin should be thrown over the exposed
material, but in the event that an explosive becomes damp from
inclement weather, it should be piled separately from the other ex
plosives and a special chemical examination should be made of the
wet material.
(3) Each magazine should be provided with a minimum and maxi
mum thermometer, and careful record should be kept at all times
of the variation in temperature.
(4) Except when material is being checked in or out of the maga
zine or during inventory, the building should be kept securely locked.
(5) Under no circumstances should packages of explosives or am
munition be opened within the magazine. I f it is necessary to ex
amine the material, it should be done outside of the building and far
enough away so that in event of accident the building itself would
not be endangered.
(6) Damaged packages should in every case be removed from the
magazine and taken to a special repacking house before any attempt
to salvage the material is made. I f the damage is slight and a re
packing house is not' available, any repair or recoopering may be
done outside at a distance not less than 100 feet from any magazine.
26. S h ipm ent.—The transportation o f explosives should be gov
erned primarily by the rules of the Interstate Commerce Commission.
These provide for the safety in transit o f certain so-called acceptable
explosives, provided that they comply in every way with the rules
for packing and marking. Where shipment is in carload lots, each
tier o f boxes or containers must be carefully cleated and braced to
provide against any possible misplacement through jar or shaking
of the car.
51
TM 9-2900
S e c tio n V
IN S P E C T IO N OF SM O K E L E SS P O W D E R
Paragraph
General------- .------------------------------------------------------------------------------------------------ 27
Testing raw materials______________ - ______________________________________ 28
DuPont nitrometer_________________________________________________________ 29
Testing nitrocellulose---------------------------------------------------------------------------------- 30
Testing smokeless powder----------------------------------------------------------------------------- 31
27. G en eral.—The foregoing consideration o f the manufacture o f

smokeless powder emphasizes the prime importance o f careful chem
ical supervision throughout the factory and demonstrates that stand
ard methods o f analysis are necessary if comparative results from
different factories are to be o f value. The purchase o f the raw ma
terials such as cotton, acids, alcohol, and diphenylamine is governed
by specifications so designed that uniform quality o f material will
be obtained. A s these specifications are necessarily o f a chemical
nature, it is essential that they prescribe in detail methods to be used
in carrying out various tests and determinations. Methods o f testing
described in this manual are in general those prescribed in the latest
U. S. Army specifications for the materials in question. In view,
however, o f the fact that the specifications are revised from time to
time, reference should be made to the last revision of the specifications
in order to obtain exact data as to approved methods.
28. T estin g’ ra w m a te ria ls.— Methods for analysis o f—
a. Cellulose.— (1) Moisture.— Not less than 3 grams (preferably 5
to 6 gr.) are weighed out in a ground glass covered moisture dish o f
suitable size, or an aluminum dish provided with a tight-fitting cover,
and dried to constant weight in an oven at 105° C. (about li/2 hours).
The dish is placed in a desiccator, covered, and when cool, weighed.
The loss in weight is calculated to percent o f moisture. A t the same
time that a sample is taken for moisture, a 2-gram sample is weighed
out for the alkali soluble determination.
(2) Extractive matter.— The dried sample from the above moisture
determination is placed in a W iley or Soxhlet extractor and suf
ficient redistilled ethyl ether for the extraction is added. A fter the
sample has been extracted on the steam bath for 3 hours the ether
is transferred to a weighed beaker or evaporating dish and evaporated
to dryness on a steam bath. The residue is heated for 30 minutes in
an oven at 100° C., cooled in a desiccator, and weighed. From this
the percent o f extractible matter based on the dry cotton is
calculated.
52
TM 9-2900
(3) Ash .—Approximately 2 grams o f the sample are placed in a

crucible and moistened with concentrated nitric acid and digested for
about 1 hour on a steam bath or hot plate, then heated gently at first
over a flame or in a muffle furnace until all combustible material is
consumed. The crucible is then cooled in a desiccator and weighed.
From the increase in weight the percent o f ash is calculated on dry
weight of sample.
(4) Alkali soluble.•—The 2-gram sample o f the cellulose weighed
out with the moisture sample is used for the alkali soluble determina
tion as follow s: The sample is heated in a 250-cc. Erlenmeyer flask
provided with a rubber stopper through which passes a long glass
tube which serves as an air reflux, with 100 cc. of caustic soda solu
tion (7.14 percent±0.1 percent) for 3 hours at 100° C. After heat
ing is completed the cellulose and solution are poured into a heaker
containing a liter o f distilled water. The alkali is neutralized with
a decided excess of acetic acid. The undissolved cellulose is filtered
within 5 minutes on a weighed Gooch crucible having an asbestos mat
and thoroughly washed successively with hot water, alcohol, and
ether. It is then dried rapidly to constant weight at 102° to 105° C.
The loss is then calculated as percent alkali soluble on the dry weight
o f cellulose.
(5) Lime, chlorides, and sulphates.—A 5- to 10-gram sample is
boiled for about y2 hour with approximately 100 co. o f distilled
water. The water is then filtered off, a small portion slightly acidified
with hydrochloric acid and brought to a boil. While hot, about lcc.
o f 5- to 10-percent barium chloride solution is added. I f only a faint
cloudiness is noted the sample is considered as containing but a trace
o f sulphates. Another small portion of the water extract is taken
and acidified slightly with nitric acid. A few drops of silver nitrate
solution are added. I f only a slight cloudiness is noted, the cellulose
may be considered as containing but a trace of chlorides. Another
small portion o f the water extract is made slightly acid with hydro
chloric acid and then faintly ammoniacal with ammonium hydroxide.
A few cubic centimeters of a saturated solution o f ammonium oxalate
solution is added and the solution boiled. I f but a faint cloudiness
is noted without the formation o f a precipitate the material may be
considered as having but a trace o f lime.
(6) Hypochlorites.— Approximately 1 gram of the sample is placed
in a uniform layer on the bottom o f a 150-cc. beaker. Ten cubic centi
meters o f a 10-percent solution o f potassium iodide are poured care
fully on the center o f the moistened cellulose. A slight violet colora
tion indicates the presence o f hypochlorites. The test is sensitive to
about 0.01 percent.
53
TM 9-290 0
(7) Absorbency .— The absorbency o f the cellulose is determined by

taking approximately 1 gram o f the dried sample, rolling it into a
ball in the palm o f the hand, and placing it lightly on the surface o f
approximately 200 cc. o f water in a 250-cc. beaker. The ball will
sink below the surface o f the water within 10 seconds if the sample
has satisfactory absorbent properties.
(8) Viscosity .— I f the viscosity o f the cellulose is specified in the
contract, it is determined by the method given in the Journal o f
Industrial and Engineering Chemistry, Analytical Edition (see
par. 89).
b. Diphenylamine.— (1) Color.— A portion o f the sample o f diphe-
nylamine is ground to pass a 10-mesh screen (opening, 0.065 in.).
The color is determined hy visual examination o f the ground material
and should not be darker than a light brown.
(2) Setting point .— From 80 to 100 grams o f the sample are ground
to pass a 10-mesh screen after which the ground sample is dried for
4 hours at 40° C. In lieu o f drying the molten sample may be mixed
with 20 grams o f anhydrous calcium chloride or sodium sulphate,
and the mixture stirred for 15 minutes at a temperature o f 80° C.,
after which the mineral salts are allowed to settle and the molten
diphenylamine poured off. The dried sample is transferred to the
inner tube o f a solidification point apparatus and melted. This tube
is then placed in the apparatus and a standard thermometer is so
adjusted that the bulb is in the center o f the diphenylamine with a
side thermometer in position fo r the emergent stem correction. The
molten material is vigorously stirred by means o f the hand stirrer
and the point at which the temperature begins to rise is carefully
noted. When solidification begins, the temperature is recorded every
15 seconds until a maximum reading is obtained. The maximum
temperature reading is corrected for the emergent stem by adding
the value calculated from the formula
N (T -t) X 0.000159
where N =D egrees in exposed mercury column.
t = Average temperature o f exposed mercury column deter
mined by means o f a second thermometer suspended
so that its bulb is in the midpoint o f exposed mercury
column.
T=U ncorrected setting point.
0.000159=Coefficient o f expansion o f mercury in glass.
The corrected reading is recorded as the setting point o f the sample
and should fall within a range o f 51.7° C. to 53° C.
54
TM 9-2900
M ILITARY EXPLOSIVES 28
(3) Solubility.— Twenty-five grams of the sample are dissolved in

100 cc. o f ethyl ether of a specific gravity 0.717 to 0.723 at 20°/20° C.
This solution is filtered through a tared Gooch crucible and washed
thoroughly with additional solvent. The crucible is then dried at a
temperature o f 100° C., cooled in a desiccator, and weighed. The
percentage of insoluble matter is then calculated and should not exceed
0.02 percent.
(4) Moisture.—Three to five grams o f the powdered sample are
weighed in a tared weighing bottle o f about 5-cm. diameter. The
weighed sample is heated for 4 horn’s at 40° C. or placed in a sul
phuric acid desiccator at room temperature for 24 hours. The loss
in weight calculated in percent is recorded as the percent moisture
and should not exceed 0.2 percent.
(5) Acid or alkali.— Twenty grams o f the ground sample are
placed in a 250-cc. Erlenmeyer flask and 50 cc. o f nearly boiling dis
tilled water added. The flask is immediately stoppered and shaken
vigorously for about 10 minutes. It is then cooled to 25° C. and the
solution filtered, retaining the diphenylamine in the flask. This ex
traction is repeated with 50 cc. of hot water. A few drops o f phe-
nolphthalein are added to the filtrate, after which it is titrated with
0.1 N alkali if acid, or 0.1 N acid if alkaline. A blank determination
is made on the water and used as a correction in the titration of
diphenylamine for any acidity or alkalinity found. The acidity or
alkalinity is calculated to hydrochloric acid or sodium hydroxide as
the case may be. The sample should not contain more than 0.005
percent o f free and combined acid or alkali. The filtrate on this
determination is reserved for the determination o f aniline.
(6) Aniline and aniline salts.— The filtrate from the acid or alkali
determination is used for the determination o f aniline or aniline salts
present. The bromide-bromate method used for this determination
is as follow s: The filtrate is transferred to a glass-stoppered Erlen
meyer flask and 25 cc. o f 0.1 N bromide-bromate water solution are
added by means o f an accurate 25-cc. pipette. The bromide-bromate
solution contains 2.784 grams o f KBrO$ and 15 grams o f KBr per
liter. The mixture is cooled to 15° C. and 5 cc. o f concentrated hy
drochloric acid are added. After 1 minute, 10 cc. o f 10-percent o f
potassium iodide solution are added. The contents o f the flask are
then titrated with 0.1 N sodium thiosulphate solution using starch as
an indicator. A blank determination is made on 25 cc. o f the bro
mide-bromate solution exactly as described above. In calculating
the results, correction is made for the amount o f diphenylamine dis
solved in 100 cc. o f water at 25° C. by subtracting 0.33 cc. from the
TM 9 -2 9 0 0
28 M IL IT A R Y EXPLOSIVES
number o f cubic centimeters o f normal thiosulphate solution repre

senting the difference between the blank and sample titrations.
Calculation: Percent o f aniline=
((A -B )N -0 .3 3 ) (0.01551) (100)
W
A = c c . o f Na2S 20 3 solution used in blank titration.
B = c c . o f Na2S 20 3 solution used in sample titration.
N = Normality o f Na2S._.03 solution.
W = W e ig h t o f sample taken.
The amount o f free aniline or aniline salts contained in the sample
will not exceed 0.1 percent, calculated as C 0H BN H 2.
c. Mixed acids.— (1 ) Suspended matter.— A portion o f approxi
mately 40 grams o f the sample accurately weighed from an acid
weighing bottle is filtered through a tared Gooch crucible containing
a carefully prepared and dried asbestos mat. The mud or suspended
material held on the asbestos mat is washed with at least five 20-c.c.
portions o f anhydrous alcohol. The anhydrous alcohol used may
be prepared by allowing 95 percent alcohol denatured with 0.5
percent o f benzene to stand over anhydrous copper sulphate, and
filtering the alcohol before use. The crucible is dried fo r 3 hours
at 125° C., cooled in a desiccator, and weighed. The increase in
weight o f the crucible is calculated as percentage o f suspended
matter.
(2) Ash .— The filtrate obtained from the determination o f sus
pended matter is placed in a tared platinum or silica dish, heated
slowly with a Bunsen flame under a hood until the evolution o f
fumes has ceased, and then heated to a dull red for 2 or 3 minutes,
cooled in a desiccator, and weighed. It is heated fo r a further
short period to determine if constant weight has been obtained. The
increase in weight o f the dish is calculated as percentage o f ash.
(3) Total acidity .— B y means o f a Lunge acid-weighing pipette, a
carefully weighed portion o f approximately 1.5 grams o f the sample
is carefully transferred to a 500-cc. Erlenmeyer flask containing
about 50 cc. o f distilled water. Tw o or three drops o f phenol-
phthalein or methyl red indicator are added and the solution titrated
with standardized N /2 or N /3 sodium hydroxide solution. The total
acidity is calculated in terms o f sulphuric acid after subtracting from
the weight o f mixed acid the weights o f suspended matter and ash
calculated to be present.
(4) Total nitric acid.— About 5 cc. o f special nitrogen-free sul
phuric acid (94.5±0.5 percent) are placed in the cup o f the gener-
56
TM 9-2900
M IL IT A R Y EXPLOSIVES 28
ating bulb o f the DuPont nitrometer. There is rapidly introduced

a known weight o f the sample o f mixed acid, estimated to contain
approximately 0.50 to 0.55 gram o f nitric acid into the cup, the
acid being stirred by means o f a small glass rod. As soon as the
mixed acid has been added, the stopcocks o f the acid pipette are
closed and the cap on the pipette quickly replaced and the acid in
the cup drawn into the generating bulb. Four 5-cc. portions of the
sulphuric acid are used to wash thoroughly the sample into the
generating bulb, making a total consumption o f 25 cc. of sulphuric
acid used in the test. It is customary to reweigh the pipette with
as little delay as possible after the first washing with 5 cc. o f sul
phuric- acid to minimize any evaporation losses or absorption of
moisture from the air. When the sample has been completely drawn
into the generating bulb, the upper stopcock is closed, the lower
stopcock allowed to remain open, and the mercury reservoir adjusted
so as to give a slightly reduced pressure in the generating bulb. The
bulb is shaken gently until most o f the gas has been generated. The
mercury reservoir is adjusted so that the mercury in the generating
bulb drops nearly to the lower shoulder, and the lower stopcock
closed. The bulb is shaken vigorously for 3 minutes. The bulb is
replaced on the rack, with the lower stopcock open and the mercury
reservoir adjusted until the mercury in the generating bulb is
approximately the same height as the mercury in the reservoir.
This adjustment is for the purpose o f bringing the pressure inside
o f the generating bulb to approximately one atmosphere, so that
the solubility o f the nitric oxide gas in the sulphuric acid will not
vary too widely. The lower stopcock is closed and the bulb shaken
vigorously for an additional minute. The gas is transferred to the
measuring tube and the levels o f the mercury in the compensating
tube and measuring tube adjusted to approximately the same height.
The gas is allowed to stand for about 20 minutes in order to permit
equalization o f the temperature o f the gas in the two tubes, the mer
cury levels are adjusted closely with a leveling device and the burette
read. The percentage o f total nitric acid is calculated by the
formula
iotal nitric acid = -----g ----
where A = reading on gas burette o f nitrometer.

B = weight o f sample of acid taken minus weights o f sus
pended matter and ash calculated to be present.
(5) Oxides of nitrogen.— A known weight of approximately 10
grams o f mixed acid is transferred to a 300-cc. Erlenmeyer flask
57
TM 9-2900
containing 75 cc. o f distilled water. A standardized 0.1N potassium

permanganate solution is added at intervals with agitation until the
end point is observed, indicated by a permanent delicate pink colora
tion. The percentage o f oxides o f nitrogen is calculated as nitrogen
dioxide by the formula
n •A . .. 4.601AB
Oxides of nitrogen—— ^ —
where A =N um ber o f cc. KM nO, solution used.
B =N orm ality factor o f the KM nO, solution.
C=Weight of sample taken minus weights of suspended mat
ter and ash calculated to be present.
(6) Sulphuric arid.— The sulphuric acid content o f the mixed acid
free from suspended matter and ash is calculated as follow s:
Sulphuric acid= A —0.77816B
where A = Total acidity, expressed as sulphuric acid.
B = Total nitric acid.
(7) Nitric acid.— The nitric acid content o f the mixed acid free
from suspended matter and ash is calculated as follow s:
Nitric acid = A —1.3695B
where A = T o ta l nitric acid.
B = Oxides of nitrogen.
(8) Water.—The water content of the mixed acid free from sus
pended matter and ash is calculated by subtracting from 100 percent
the sum of the percentages of sulphuric acid, nitric acid, and oxides
of nitrogen.
If it is desired, a Gooch crucible with an asbestos mat may be sub
stituted for the filter paper if the mat is thick and compact, and the
operator can check results by this method with those by the method
described above.
d. Ethyl alcohol.— (1) Content.— The specific gravity at 2 0 °/4 ° C.
is determined by means o f a calibrated hydrometer or pycnometer.
The percentage o f alcohol by volume is obtained by reference to the
tables o f the Official and Tentative Methods o f Analyses o f the A s
sociation o f Official Agricultural Chemists. (See par. 89).
(2) Acidity.— 50 cc. of neutral distilled water is placed in a 250-cc.
Erlenmeyer flask and a 50-cc. portion o f the sample added measured
by means o f a graduated cylinder. Six drops o f gallein indicator
(made by dissolving 1 gram o f gallein in 1 liter o f neutral ethyl
alcohol, approximately 95 percent by volume) are added and titrated
with approximately tenth-normal sodium hydroxide or potassium
58
TM 9-2900
hydroxide solution. The percentage of acidity in the sample is

calculated:
„ 0.12 AB
Percentage o f acidity as acetic a c id = ----^ —
where A = cc. o f hydroxide solution.
B=N orm ality of hydroxide solution.
C = Specific gravity o f alcohol.
(3) Residue.—A 100-cc. portion o f the sample, measured by means
of a pipette, is transferred to a tared evaporating dish. The liquid
is evaporated on a steam bath to dryness, then dried for 2 hours at
100° C., cooled in a desiccator, and weighed. The increase in weight
of the dish is calculated to percentage of residue.
Percentage of residue—r>
where A = Weight o f residue.
B = Specific gravity of sample.
(4) Aldehyde.— Silver nitrate and sodium hydroxide solutions are
prepared containing 9 grams o f compound per 100 cc. o f distilled
water. By means o f a pipette 1 cc. o f the silver nitrate solution and
1 cc. o f the sodium hydroxide solution are transferred to a graduated
cylinder (5-10 cc. capacity) and approximately 1 cc. o f ammonium
hydroxide (sp. gr. .90), or an amount sufficient to dissolve the precip
itate formed by addition o f the sodium hydroxide to the silver nitrate
solution is added. By means of a pipette or burette, a 10-cc. portion
o f the sample is transferred to a clean, glass-stoppered bottle or flask
and 1 cc. o f the solution from the graduated cylinder added. The
bottle is shaken well and allowed to remain in a dark place for 1 hour.
The solution is filtered and the clear filtrate tested for unreduced silver
by adding 1 cc. o f a 10-percent solution of sodium chloride. I f any
precipitate is formed as shown by the cloudiness o f the liquid, it is
indicated that the alcohol contains not more than a trace of aldehyde.
When the test is completed the solutions used are destroyed, as a
sensitive silver salt may be formed.
(5) Fusel ails, etc.— Both of the following tests are made:
(« ) By means o f a graduated cylinder, a 10-cc. portion of the
sample is transferred to a clean, clear test tube. One cc. o f a solu
tion made by dissolving 1 gram o f potassium permanganate in 1 liter
of distilled water is added. I f the color o f the mixture turns yellow
in 20 minutes, fusel oils or other oi’ganic impurities are indicated to
be present.
( b ) By means of a graduated cylinder, a 10-cc. portion o f the
sample is transferred to a clean, clear test tube. Ten cc. of C. P.
59
TM 9-2900
sulphuric acid (sp. gr., 1.84) is added. I f a yellow color results, the
presence o f organic impurities is indicated.
(6) Benzene.— By means o f a graduated cylinder, a 100-cc. por
tion o f the sample and 200 cc. o f distilled water are transferred to
a 1-liter side-neck distillation flask fitted with a straight glass con
denser having a water jacket approximately 40 cm. long, 35 mm.
diameter, and a 10-mm. central tube. The mixture is distilled at a
rate o f 1.0 to 1.5 cc. per minute and 20 cc. ±0.10 cc. collected in a
suitable graduated container. I f it is thought because o f a cloudy
appearance o f the mixture after dilution with the water that the
benzene content exceeds 0.75 percent, an additional 10 cc. o f the distil
late is collected in a separate container. The fit's! 20 cc. o f the distil
late collected is transferred to the receiving bulb o f the benzenom-
eter. To this distillate 15.0±0.10 cc. o f a 2.5- to 3.0-percent solu
tion o f potassium dichromate and 3.0 ±0.1 cc. o f hydrochloric acid
(sp. gr. 1.20) are added from a burette. The bulb is closed with a
well-fitting straight-sided rubber stopper, shaken for 2 to 3 minutes,
and allowed to stand for 15 minutes or until an olive-green color
develops, indicating complete oxidation o f the alcohol to acetic acid.
It is important that the oxidation be complete, otherwise values that
are too high may be obtained. The solution is carefully drawn into
the graduated tube and lower bulb by slowly lowering the mercury
reservoir. A fter about. 15 minutes when the drainage o f the liquid
from the walls of the receiving bulb is complete, the exact volume
o f the liquid is read which is approximately 37 cc. The volume o f
the tube and the lower bulb from the mark on the bottom o f tbe
lower bulb to the zero mark on the tube is 37.5 cc. I f the volume o f
the liquid is not within 0.5 cc. o f the zero mark, sufficient dichromate
solution is added to increase the volume to 37.0 cc. The mercury
reservoir is slowly raised until all o f the solution has been transferred
to the receiving bulb and 10 cc. o f petroleum ether is added. The
rubber stopper is inserted in the mouth o f the receiving bulb and
shaken thoroughly fo r 2 or 3 minutes. The mercury reservoir is
slowly lowered until the mercury with glass tube is level with the
mark below the lower bulb. It is allowed to stand for at least %
hour in order to effect complete separation of two layers o f aqueous
solution and petroleum ether, and the decrease in volume o f the aque
ous solution caused by the extraction o f the benzene by the petroleum
ether is noted. I f the 10-cc. additional distillate is collected, it is
treated in exactly the same manner as the 20-cc. portion, and the
values obtained added. A blank determination is made on the same
fit)
TM 9-2900
M ILITAR Y EXPLOSIVES 28-29
amount of absolute alcohol as of distillate used (20 cc. or 30 cc.) and

a correction made, if any is found.
e. Ether.— (1) Color.— Visual comparison is made o f the ether and
water in test tubes of 25-cc. capacity.
(2) Nonvolatile residue.— 100 cc. of the sample is transferred to
a tared beaker or evaporating dish, evaporated to dryness on a steam
bath, and dried at 100° C. for 1 hour. This is cooled in a desiccator
and weighed. The gain in weight is calculated as percentage of non
volatile residue as follows:
Weight residue
Percentage of nonvolatile residue =
Specific gravity
The specific gravity is determined by means of a standardized hy
drometer, Westphal balance, or a specific-gravity bottle, and expressed
as specific gravity at 20° C./200 C.
(3) Acidity .— Fifty cc. o f alcohol are placed in an Erlenmeyer
flask, five drops of phenolphthalein added, and neutralized with
approximately 0.1N sodium-hydroxide solution. One hundred cc. o f
the ether is added, mixed, and titrated with the standard alkali to a
faint pink.
29. D u P ont n itrom eter.— a. Theoretical.— The DuPont nitrome
ter is a modification o f the Lunge nitrometer and is devised to avoid
necessity o f making the usual correction for temperature and baro
metric pressure which must be calculated with every gas measurement.
The principle o f the apparatus is to inclose a known volume o f air
at such a pressure that it takes up exactly the volume which it would
occupy at 20° C. and 760 mm. pressure. I f the same pressure and
temperature are then applied to another volume of gas this will also
take up the volume which it would occupy at 20° C. and 760 mm.
pressure. The volume of air is kept in a “compensating tube” which
isi connected with the reading tube o f the nitrometer. When it is
desired to read the volume o f a given quantity of NO gas at 20° C.
and 760 mm. pressure, the level of the mercury in the compensating
tube is brought to the mark at which the air within the tube occupies
the. space it would occupy at 20° C. and 760 mm. pressure, the level
o f the mercury in the reading tube is brought to the same level as
the mark, and the reading made. The reading tube o f the DuPont
nitrometer is graduated to read directly the percentage o f nitrogen
when a 1-gram sample is used.
b. Assembly.— The various tubes are arranged on the nitrometer
rack in order shown in figure 28; 25 cc. of 94 to 95 percent H>SO< is
then placed in No. 2 and a quantity o f air drawn in through the
61
TM 9-2900
stopcock. The stopcock is then closed and the bulb shaken vigorously
to dry the air. The shaking is repeated several times at intervals
o f from 10 to 15 minutes. When the air is judged to be thoroughly
dry, 2 and 4 are connected and the dry air run into 4 until, with the
stopcock o f 3 open and the mercury in 3, 4, and 5, on the same level,
the reading in 3 is about 12.50. No. 4 is then sealed with a small
blowpipe flame. Another portion o f air is then desiccated in 2 and
transferred to 3 until, with the mercury in 3, 4, and 5 on the same
level, the reading in 3 is about 12.50. It is not necessary that these
gas volumes he exact or equal. The small manometer, A , is then
filled with H 2S 0 4 and attached to 3. The apparatus is then left to
come to constant temperature. The mercury in 3, 4, and 5 is then
adjusted so that the- air in 3 is under atmospheric pressure as shown
by the acid in A. The reading is taken on the graduated scale on 3.
The temperature and barometric pressure are noted at the same time.
From these readings the volume o f air in 3 is calculated at 20° C. and
760 mm. pressure by the gas laws which are expressed by the equation:
V : V '= P ': P
V : V ' = T :T '
in which V = Volume at 20° C. and 760 mm.
V '= V o lu m e at the observed temperature T ' and pressure P '.
From these is derived the equation:
P/ X293 X (1—0.000180
Y v
s
F iolwu 28.— Nitrometer.
62
T M 9—29QI)
M IL IT A R Y EXPLOSIVES 2 9 -3 0
The last term o f the equation represents the correction to be applied

for the coefficient of expansion o f mercury in the barometer where
t' equals temperature o f the barometer. When V has been calculated,
the mercury in 3, 4, and 5 is adjusted so that with the mercury in 3 and
4 on a level the mercury in 3 marks the calculated volume o f air. The
height o f the mercury in 4 is then marked by a strip of paper pasted
on the tube. This is taken as the standard volume with which every
volume o f gas to be measured is compared.
c. Standardization with C. P. K N 0 3.— A sample o f C. P. K N 0 3
which has been recrystallized three times from 95 percent alcohol is
finely ground and dried for 2 to 3 hours at 135° to 150° C. Exactly 1
gram is weighed out into a small weighing bottle and transferred to
the nitrometer (for details see par. 30cZ), dissolving the K N 0 3 in the
nitrometer cup with 20 cc. o f 94.5 percent ± 0.5 percent H ,S 0 4. W ith
the lower stopcock o f the generating bulb open and the mercury bulb
low enough to give a reduced pressure in 2, the generating bulb is
gently shaken until the larger portion o f gas has been generated. The
generating bulb is then raised until the mercury drops nearly to the
lower shoulder, the lower stopcock closed, and the bulb is shaken
vigorously for 3 minutes. After replacing on the rack, the lower
cock is opened and the bulb allowed to stand for several minutes. The
lower stopcock is closed and the shaking is then repeated for an addi
tional 3 minutes, adjusting the mercury as before. Finally the gas is
transferred to 3, the positions o f 3, 4, and 5 so adjusted that the level
of mercury in 3 and 4 is about the same and the apparatus allowed
to stand 20 minutes. The mercury levels are then carefully adjusted
with a leveling device and the reading in 3 taken. This should bo
13.85 percent.
d. Standardization by test blend.— This standardization is run in
a way similar to c above except that a blend o f nitrocellulose which has
been carefully tested on a standardized nitrometer is used. This
method is somewhat more convenient than the method with KNOs
because the nitrocellulose is more easily broken up in the nitrometer
than K N Oa. Whenever a doubt exists, however, the standardization
must be carried out with K N 0 3.
30. T estin g n itrocellu lose.— a. Solvability.— (1) In ether-alco
hol.—The official temperature for this determination is 15.5° C., and in
any case where the material does not comply with the specification
or where greater accuracy is desired, the complete determination is
made at this temperature, the solvents being brought to this tempera
ture before their addition to the sample. Nitrocellulose is more soluble
at 15.5° C. than at a higher temperature. Ether and alcohol used
63
TM 9-2900
should be o f the quality prescribed for use in manufacture o f smoke

less powder.
Volwmetric method.— One gram o f the dry sample is placed in an
Erlenmeyer flask and 75 cubic centimeters o f alcohol added, shaken
thoroughly for about five minutes and allowed to stand for two hours.
One hundred and fifty cubic centimeters o f ether are then added and
the mixture thoroughly shaken and allowed to stand stoppered over
night. It is desirable to start this determination early in the day in
order to give it plenty o f agitation before standing overnight, as agi
tation facilitates solution.
The process used in the remainder o f the determination depends
upon the grade o f nitrocellulose being tested, on account o f the varia
tion in the solubility o f the different grades.
In the case o f pyrocellulose, the mixture in the flask is thoroughly
shaken the next morning and transferred to a special solubility tube
o f the follow ing dimensions: Total length, 21 inches; inside diameter,
1.35 inches; the lower end constricted for a length o f 2 inches to an
inside diameter o f 0.3 inches and graduated in one-tenth cubic centi
meter. The constricted portion should be tapered gradually from
the large part o f the tube. A fter standing in the solubility tube until
the insoluble material has settled completely as indicated by the
volume o f this material remaining constant over a period o f one hour,
the volume occupied by the insoluble and semisoluble matter is read in
cubic centimeters from the scale on the tube. I f the reading is 0.25
cubic centimeter or less, the percentage o f insoluble is considered to
be 1 percent or less. Should the reading exceed 0.25 cubic centimeter,
the gravimetric method will be used as follow s:
Grmimetnc method.— The clear liquid in the solubility tube
obtained as above is siphoned off to about one-fourth inch from the
upper surface o f the settled residue, then alcohol is added to one-
third the capacity o f the tube, shaken vigorously and ether added to
about 3 inches o f the top, shaken and allowed to settle. This process
o f washing by decantation is repeated four times, and after the fourth
decantation the insoluble residue is completely washed into a beaker
with a small quantity o f ether-alcohol solution. The contents o f the
beaker are filtered through a weighed Gooch crucible with ignited
asbestos mat, washed free from soluble nitrocellulose with ether-
alcohol solution, dried at a low temperature until no odor o f ether
can be detected and then at 100° C. to constant weight, cooled, and
weighed. The crucible is then carefully ignited over a free flame,
cooled, and weighed again. The loss o f weight on ignition is consid
ered as the insoluble nitrocellulose.
64
TM 9-2900
M ILITAR Y EXPLOSIVES 30
In the case o f guncotton or blends o f pyrocellulose and guncotton,

100 cubic centimeters of the clear solution is drawn from the solubility
lube (without disturbing the settled layer o f insoluble material) and
run into an aluminum can 50 millimeters in height by 90 millimeters
in diameter, with tightly fitting cover, which has previously been
dried and weighed. The soluble nitrocellulose is now precipitated
from the clear solution in the can by the addition o f distilled water.
A finely divided precipitate o f fibrous appearance is desired, and is
best obtained by first heating the solution on a steam hot plate (the
fared aluminum can should not come in contact with steam or hot
water) to evaporate part o f the ether, then adding about 50 cc. of
distilled water gradually with continued heating and stirring. The
exact procedure for obtaining the best results must be determined by
experience. After the nitrocellulose has been precipitated, heating
is continued until the liquid is evaporated just to dryness. The can
with contents is then dried in an oven at 95° to 100° C. for iy 2 hours,
cooled in a desiccator, and weighed. A check weight should be
obtained after additional drying for y2 hour. The increase in weight
o f the can is the weight o f soluble nitrocellulose. The percentage of
the latter is calculated as follow s:
Percent soluble nitrocellulose=g 100
Where A = Weight o f soluble nitrocellulose in 100 cc. of clear

solution.
B = % o f weight o f original sample.
(2) In acetone.—This is determined by the same method as the
solubility in ether-alcohol, except that acetone is used as solvent. I f
the volumetric reading is greater than 0.2, the determination is made
gravimetrically.
b. K. / . starch test.—The sample is pressed in a clean cloth or
wrung out in a wringer if it contains a large excess o f water. The
cake is rubbed up in the cloth until fine, taking care that it does not
come in contact with the hands, spread out on clean paper trays, and
dried in the air bath at 35° to 40° O. until the proper moisture con
tent has been obtained. The desired moisture content is that which
will give condensation of moisture in diminishing amounts in the five
test tubes used, ranging from an appreciable amount in the first tube
to none in the fifth as the test progresses. The proper condition o f
nitrocellulose for the first sample is indicated when the nitrocellulose
clings, after rubbing, to a spatula or tissue paper which has been
wrapped about the fingers. A sample of 1.3 grams is weighed out on
240511°— 40---- 5 65
TM 9-2900
a dispensing balance and transferred to a tube. More tubes are filled

approximately at 4- to 5-minute intervals until five tubes have been
prepared. The tubes used should be 5y2 inches long, i/2 inch internal
diameter, and % inch external diameter. During the test the tubes
are closed by a clean, tight-fitting cork stopper through which passes
a tight-fitting glass rod equipped with a platinum holder for the
paper. Corks are discarded after one test. The nitrocellulose is
pressed or shaken down in the tube until it occupies a space o f 1%
inches. The test paper, about 1 inch in length and % inch wide, is
hung on the platinum holder, and moistened on its upper half with
a 50-percent solution o f pure glycerin in water. The heating bath
is carefully regulated at Go.5° C .± l°, and is placed so that a bright
reflected light is obtained. The time is taken when the tubes enter
the bath. As the test continues, the line of demarcation between wet
and dry test paper is kept abreast the lower edge o f the moisture film.
The first appearance o f discoloration o f the damp portion o f the test
paper marks the end o f the test for each separate tube, the minimum
test o f any one o f the five tubes being the heat test o f the nitrocellu
lose. This discoloration is to be greater than that obtained at the
same time by a blank test. Standard test paper is used in this test
and is furnished by the Government. The standard water bath holds
10 tubes and is made long and narrow to reduce to a minimum the
heating o f the upper portions o f the tubes. The tubes are immersed
in the bath to a standard depth o f 2.25 inches.
c. Heat test at 134.5° C .— A sample o f nitrocellulose is laid out in
paper trays and dried for 4 or 5 hours at about 40° C., or is dried
over night at room temperature and then further dried y2 hour at
about 40° C., after which 2.5 grams are pressed into the lower 2 inches
in each o f two tubes of heavy glass about 290 mm. long, 18 mm. out
side diameter, and 15 mm. inside diameter, closed with a cork stopper
through which a hole or notch 4 mm. in diameter has been bored or
cut. A piece o f standard normal methyl violet paper, 70 mm. long
and 20 mm. wide, is placed in each tube, its lower edge 25 mm. above
the sample. When the constant temperature bath has been carefully
regulated at 134.5° C.± 0.5° C., these tubes are placed in the bath so
that no more than G or 7 mm. o f length project from bath. Exam
ination o f the tube is made by withdrawing about one-half its length
and replacing quickly each 5 minutes after 20 minutes have elapsed.
The minimum time, which will be a multiple o f 5, in which the violet
color o f the test paper in either tube has completely turned to salmon
pink will be reported as the time o f test. F or example, if the violet
GG
TIVT 9-2900
color is not completely changed in 25 minutes but is completely

changed in 30 minutes, the time o f the test is recorded as 30 minutes,
phe bath must be placed in a good light, with a suitable background.
The standard normal methyl violet paper is furnished by the Gov
ernment.
d. Determination o f nitrogen.— A sample o f approximately 1 gram
of nitrocellulose air-driecl at a temperature not above 46° C. is placed
in a ground glass stoppered weighing bottle (dimensions, approxi
mately 50 mm. high by 25 mm. diameter) and dried for iy> hours at
a temperature ranging from 98° to 102° C., cooled in a desiccator,
and weighed. The standard DuPont 5-part form o f Lunge’s ni
trometer with properly standardized compensating and reading tubes
is used for determination of nitrogen. For standard operation room
temperature must be between 15° and 32° C. The cup o f the gener
ating bulb is washed free from any nitrogenous impurities and the
nitrocellulose transferred to the cup; 20 cc. of nitrogen-free sulphuric
acid, strength 94.5 ± 0.5 percent is measured out into a graduate or
small beaker. Small portions of the acid are run into the weighing
bottle and transferred to the generating bulb until a sufficient quan
tity has been used to make an emulsion with the nitrocellulose. The
mercury reservoir is lowered sufficiently to cause reduced pressure in
the generating bulb. The upper stopcock is opened wide and the
lower opened sufficiently to draw the nitrocellulose into the generat
ing bulb. Successive rinsings with sulphuric acid are made until all
of the nitrocellulose has been drawn in with the 20 cc. o f acid. The
upper stopcock is generally manipulated after the first time. Any
air drawn into the bulb should be forced out, after which the upper
stopcock is closed, the lower one remaining open, and the mercury
reservoir adjusted just low enough to give a slightly reduced pressure
in the generating bulb. The generating bulb is shaken gently, keep
ing the lower end in a fixed position until most o f the gas has been
generated. The mercury reservoir is adjusted so that the mercury
in the generating bulb drops nearly to the lower shoulder, whereupon
the lower stopcock is closed and the bulb shaken vigorously for 3
minutes. The bulb is replaced on the rack with the lower stopcock
open and the mercury reservoir adjusted until the mercury in the
generating bulb is approximately the same height as the mercury in
the reservoir. This adjustment is for the purpose o f bringing the
pressure inside o f the generating bulb to approximately one atmos
phere so that the solubility o f the nitric oxide gas in the sulphuric
acid will not vary too widely. The lower stopcock is closed and the
67
TM 9-2900
30-3 1 M IL IT A R Y EXPLOSIVES
bulb shaken vigorously for an additional 3 minutes. The gas is now

transferred to the measuring tube and the levels o f the mercury in
the compensating tube and the measuring tube are adjusted to ap
proximately the same height. The gas is allowed to stand for about
20 minutes in order to permit equalization o f temperature o f the gas
in the two tubes, and the mercury levels closely adjusted with a level
ing device. The reading o f the measuring tube is divided by the
weight of the sample o f nitrocellulose, giving the percent nitrogen
in the nitrocellulose. The tare weight o f the weighing bottle may be
obtained before or after the test.
e. Ash .— Two grams o f dried nitrocellulose are placed in a recently
ignited and tared crucible and treated with sufficient acetone contain
ing 5 percent castor oil (by volume) to gelatinize thoroughly the
nitrocellulose. It is then ignited and allowed to burn without apply
ing heat until a charred residue remains, and finally it is thoroughly
ignited, cooled, weighed, and the percentage o f ash calculated. I f
preferred, the nitrocellulose may be digested with nitric acid, ignited
carefully, and the ash determined.
31. T e s tin g S m ok eless P ow d er.— a. 'Samples.— (1) Ballistic.—
The number o f containers required to make up the ballistic sample
and the chemical and stability sample as prescribed in the specifica
tion should be selected so as to be representative o f the lot. I f the
weight o f the samples required is less than 10 containers, a portion
equal to y10 the weight o f the required ballistic sample should be
removed from each o f 10 boxes and those 10 portions should be packed
in individual airtight containers. It is desirable that the ballistic
sample be taken not sooner than 2 weeks after the original packing.
(2) Chemical and stability.— From each o f the containers sampled
for the ballistic tests, there should be removed equal portions o f the
powder so as to have a sample for the chemical and stability tests
o f approximately the weight prescribed in the specification. Not
less than 5 pounds o f this sample should be set aside fo r 65.5° C.
surveillance tests. The greatest cleanliness should be observed in
handling the chemical and stability sample and handling it with
damp or soiled hands should be avoided. The sample should be
mixed thoroughly.
b. External moistVA'e.— (1) Air-dried.— A sample o f about 20
grams o f the powder (or 2 whole grains, if 1 grain weighs more than
10 grams) is weighed accurately in a tared glass weighing bottle.
It. is dried in a vacuum oven (vacuum o f at least 25 inches o f
mercury) at 5 5 ± 2 ° C. for 6 hours, cooled in a desiccator, and
68
TM 9-2900
weighed. The loss in weight is calculated to percentage of moisture

in the sample as received.
(2) Water-dried.—A sample o f about 20 grams o f the powder (or
2 whole grains if 1 grain weighs more than 10 grams) is weighed
accurately in a tared glass weighing bottle. It is dried for 6 hours
at 100±2° C. at atmospheric pressure, cooled in a desiccator, and
weighed. The loss in weight is calculated to percentage of moisture
in the sample as received.
c. Diphenylamine.— A sample o f 5 grams of the powder is weighed
accurately into a 250-cc. lipped beaker. The sample may be in whole
grains if small enough to give a fair sample or in slices of
medium or larger grains. Ten cc. o f glacial acetic acid and 20 ce. of
nitric acid (sp. gr. 1.42) are mixed and poured on the powder. The
beaker is covered with a watch glass and placed on a steam bath at
about 95° C. for V/2 hours. It is necessary that the above quantities
o f acid be strictly adhered to by using either a pipette or graduate
for the measurement. The powder dissolves completely with copious
evolution o f red fumes. The time and temperature given allows all
red fumes to be dissipated without too much reduction o f volume,
and this is the end to be attained as the nitro compounds have a
tendency to crystallize out if the solution is evaporated too much or
is allowed to stand too long after removal from the steam bath.
Whenever such crystallization occurs results are slightly low.
Immediately after heating on the steam bath is completed, the
solution is cooled, being careful not. to agitate, and poured into 75 cc.
o f distilled water which has been cooled to 15° C. in a 250-cc. glass-
stoppered Erlenmeyer flask. The beaker is washed with water so
that the solution including washings will be approximately 120 cc.
The flask is shaken well fo r about 2 minutes and allowed to stand
overnight.
The nitro compound is filtered on a Gooch crucible prepared by
washing with 10 percent nitric acid and igniting. The nitro com
pound is washed six or seven times with water containing 1 percent
o f nitric acid, dried at 100° to 105° C. for 1 hour, cooled in a desic
cator, and weighed. The crucible is placed in a small beaker, 10 cc.
of acetone added, and allowed to soak for 15 minutes. The crucible
is placed on a suction flask and washed with small quantities o f ace
tone until nitro compounds are completely removed. The crucible
is dried at 100° to 105° C. for 1 hour, cooled in a desiccator, and
weighed. The loss in weight is calculated as nitro compounds.
TM 9 -290 0
The factor for conversion o f nitro compound to diphenylamine,

using the quantities o f acid stated above, is 0.4259.
W eight o f nit ro compound X 0.4259 X 100
Percent diphenylamine=
W eight o f powder
d. Graphite.— The crucible used for the determination o f diphenyl
amine is placed in a muffle furnace or in an inclined position over a
gas burner and heated strongly until all carbonaceous material has
disappeared. The crucible is cooled in a desiccator and weighed.
The loss in weight is calculated as percentage o f graphite in the
sample as received.
e. Total volatiles.— The volatile determination is started as soon
after receipt o f the sample as possible. Any grains which have been
handled should not be returned to the sample, except in special cases
where the sample available is very small. The sample container is
kept tightly closed. About 20 grains o f all powders are used regard
less o f caliber. A total o f at least 2 grams is cut, taking approxi
mately the same number o f slices from each grain, after first cutting
off and discarding about 14 ° f the grain so that the slices used come
from approximately midway between end and center o f the grain.
Each slice is cut so as to have as nearly as possible the same thick
ness at all parts o f its area. The slices are cut either clear across
the grain giving a circular area, or just half across giving a semi
circular area. A sample o f about 1 gram is weighed accurately into
a tared aluminum can, approximately 50 mm. high and 90 mm. in
diameter, provided with a tight fitting lid and an aluminum stirring
rod, the weight o f which is included in the weight o f the can. This
is treated with 50 cc. o f alcohol com plying with U. S. Arm y Specifi
cation No. 4-1018, and 100 cc. o f ether com plying with U. S. A rm y
Specification No. 50-11-45. This should be stirred frequently if it
is desired to hasten solution, or covered and the can left under a bell
jar overnight. When solution is complete the ether that has evap
orated is replaced. The can is placed on a steam box or on a closed
steam bath and a portion o f the ether evaporated. The aluminum
can should not be permitted to come in contact with steam or hot
water. The amount o f ether evaporated before the precipitation o f
the nitrocellulose determines the character o f the precipitate; if too
much ether is evaporated the precipitate will be gummy and difficult
to d ry ; if too little ether is evaporated the precipitate will be sandy
and cause bumping. The amount o f ether to evaporate in order to
obtain the desired fine, flaky precipitate depends upon the amount o f
nitrocellulose present and can be learned only by practice. When it
is considered that the correct amount o f ether has been evaporated,
70
TM 9-2900
M ILITA R Y EXPLOSIVES 31
10 cc. o f distilled water is added. I f the solution becomes opaque

indicating that the precipitation has started, water is added slowly
with constant stirring to make a total o f 50 cc. I f the 10-cc. portion
of water does not start the precipitation, a little more ether is evap
orated and again 10 cc. o f water is added. This process is repeated
until a 10-cc. portion of water starts the precipitation and the pre
cipitation is finished by adding sufficient water to make a total of
50 cc. I f the precipitate seems too heavy, 5 cc. portions of ether are
added and stirred until the precipitate becomes light and flaky. The
ether is evaporated with constant stirring until there is no further
danger of bumping and then just to dryness. The can is trans
ferred to an oven at 95° to 100° C. and dried for 1]■/%hours, cooled
in a desiccator, and weighed. The can is returned to the oven for
1/2 hour, cooled in a desiccator, and weighed. I f the latter weigh
ing does not check the former within 0.0005 gram, the i/^-hour dry
ings in the oven are repeated until the results check within this limit.
A nonvolatile residue at 95° to 100° C. is run on the quantities of
water, alcohol, and ether used and the percentage o f total volatiles
is calculated as follows:
( A —B + C —D X 1 0 0 )
Percentage o f total volatiles=
E
where A = Original weight of can and sample.
B = F in a l weight o f can and sample.
C = Weight o f water, ether, and alcohol residues.
D=Correction in grams for volatilization of diphenylamine
during the determination. 25 percent o f diphenylamine
content o f powder is allowed.
E = Original weight of sample.
The percentage of total volatiles, graphite, and diphenylamine is
subtracted from 100 and reported as percentage o f nitrocellulose in
the sample.
/. A s h .— From the remainder o f the slices or grains a sample o f
about 1 gram is weighed accurately in a fared porcelain crucible.
The sample is moistened with a small quantity o f concentrated nitric
acid and digested for 2 to 3 hours on a steam bath. The crucible
is removed from steam bath and heated over a Bunsen burner
cautiously at first to avoid loss. The crucible is finally placed in
a muffle furnace, or in an inclined position partially covered with a
lid over a gas burner, and heated strongly until all carbonaceous
matter has disappeared, cooled in a desiccator, and weighed. From
this weight the original weight o f the crucible is subtracted and the
result calculated as percent of ash in the sample as received.
71
T3VE 9 -2 9 0 0
g. Compressibility.— In this test grains which are abnormal in

shape or contain obvious flaws are not used. The ends of 10 normal
grains o f powder are cut so that new surfaces perpendicular to the
length are exposed, and the length is equal to the diameter. The
average length o f these pieces is determined with a micrometer.
Each grain is compressed between parallel surfaces, increasing the
load slowly until the first crack appears. The load is removed and
the grain measured. The average reduction in length is calculated
in percentage o f the average original length. I f these 10 grains
fail to pass this test, 20 more grains are subjected to the test. The
average reduction in length is calculated in percentage o f the aver
age original length o f the total 30 grains tested.
h. Heat test at 134.6° C .— Tests are made on five samples thus:
2.5 grams o f sample are weighed out and each sample placed in a
test tube made o f heavy glass, preferably pyrex, approximately 15
mm. inside diameter, 18 mm. outside diameter, and 290 mm. long.
Each sample should consist o f as nearly whole grains as consistent
with a weight o f 2.5 grams of sample. In sectioning grains to ob
tain the required weight, the grains are split longitudinally. A
piece o f standard normal methyl violet paper, 70 mm. long and
20 mm. wide is placed vertically in each tube, its lower edge 25 mm.
above the powder. The tubes are stoppered with corks through
which holes 4 mm. in diameter have been bored. The tubes are
placed in a constant temperature bath at 134.5 ± 0 .5 ° C. so that no
more than 6 or 7 mm. o f length project. Each tube is examined by
withdrawing about one-half o f its length and replacing quickly at
5-minute intervals after 55 minutes have elapsed. The time o f the
observation which reveals the test paper in any tube to be com
pletely changed to a salmon pink color is recorded as the time o f
completion o f the test. Heating is continued and report is made
w'hether any sample o f powder explodes in less than 5 hours.
(Standard normal methyl violet papers and standards fo r salmon
pink are secured from the Ordnance Department.)
i. Dimensions.— The form o f grain is determined by visual exami
nation.
(1) Length .— Thirty normal grains o f powder are selected at ran
dom and the length measured with a micrometer. When the ends are
irregular, the average length is determined as closely as possible.
(2) Grain and perforation diameter, and web thickness.— Ninety
normal grains are selected o f either single or multiperforated powder.
By means o f a razor blade or hacksaw each grain is cut partly through
from opposite sides at about the middle, and broken under strain so
that a narrow ridge o f powder which includes the desired line of
72
TM 9-2900
measurement is left along the line o f breakage. This desired line o f

measurement is a straight line forming a diameter of the grain which
passes through the center o f the perforation of a single perforated
powder and through the centers of three perforations o f a multi-
perforated powder.
A number o f the grains are placed vertically on a glass slide so
that the broken ends are uppermost and the individual desired lines
of measurement are in alinement. A film o f vaseline is used on the
glass slide to hold the grains in position if necessary. The slide is
placed on the stage o f a measuring microscope having a magnification
of approximately 25 diameters, equipped with cross hairs, and having
a horizontal scale and vernier screw scale capable o f giving measure
ments accurate to 0.001 inch.
In case o f multiperforated grains, the diameter o f the grain, the
two outer web thicknesses and two inner web thicknesses, and the
diameters o f three perforations of each of the 90 grains are measured
by means o f a continuous series o f readings taken along the desired
line o f measurement o f each grain. In the case of single perforated
grains, the diameter of the grain, the two web thicknesses, and the
diameter of the perforation o f each o f the 90 grains are measured by
means o f a continuous series of readings taken along the desired line
o f measurement o f each grain.
(3) Length-diameter ratio.—From the measurements o f length and
grain diameter taken as described above, the ratio between the average
length (L ) and the average diameter (D ) is calculated.
(4) Length and diameter uniformity.—From the measurement o f
length and grain diameter taken as described above, the mean varia
tion of individual dimensions from the mean dimensions, expressed
as percentage of the mean dimensions is calculated.
(5) Grain diameter-perforation diameter ratio.—From the meas
urements taken as described above, the ratio between the average
grain diameter (D ) and the average perforation diameter (d ) is
calculated.
j. 1Veb measurements.— (1) Type I.—From the measurement made
as described above, the average outer web thickness (W o) and the
average inner web thickness (W i) for the 90 grains measured are
calculated. The average web thickness (W „) is calculated by taking
the average of W 0 and Wi. The diffei’ence between the average outer
web thickness (W 0) and the average inner web thickness (W i) in
terms o f percentage o f the average web thickness (W tt) is calculated.
( W o - W , ) X100 ( W i- W o) XI OO _
or percentage difference
W. \Ya
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TM 9-290 0
3 1 -3 2 M IL IT A R Y EXPLOSIVES
(2) Type II. — From the measurements made as described above,

the average o f the 90 web thicknesses above the median and the aver
age of the 90 web thicknesses below the median are calculated. The
percentage is calculated by which each o f the (wo averages differs
from the average o f all the web measurements (W ,).
Ic. Ballistic tests.— (1) Service velocity.— The number o f rounds
prescribed in the specification are fired in the proper weapon with
the prescribed projectiles with charges calculated to give the required
service velocity. Powder from a different container is used fo r each
round. In case the amount o f powder required fo r a charge exceeds
the contents o f one box the charge is made up from as few containers
as possible. The velocities and pressures developed are measured.
(2) Velocity uniformity.— The maximum variation and mean vari
ation in the uniformity series are calculated.
(3) Pressure.— The mean pressure for the series is calculated. I f
the mean velocity obtained in the uniform ity series is not equal to
the prescribed service velocity, the charge that would be required to
give the prescribed service velocity is estimated and the observed
mean pressure corrected to the pressure that would have been obtained
if the correct charge for obtaining the prescribed service velocity had
been used.
(4) Excess charge.—"With the prescribed projectile in the weapon
for which the powder is intended, the number of excess charge rounds
prescribed in the specification is fired, using a weight o f charge 105
percent o f the charge calculated to give the prescribed velocity. The
maximum pressure developed fo r each is measured. In any case
where the 105-percent charge exceeds the chamber capacity o f the
weapon, the excess charge should be as near 105 percent o f the service
charge as practicable.
S ectio n V I
COM PO UND P R O P E L L A N T S
Piirngrapli
General____________________________________________________________________ 32
Double base powders------------------------------- 33
E. C. powder------------------------------------------------------------------------------------------------ 34
32. G eneral.— Discussion in preceding sections has been concerned

largely with straight nitrocellulose powder, commonly referred to as
pyro powder. There are some military weapons which require the use
o f propellants which have a greater potential than pyro powder, or
which for special reasons are commonly provided with powders hav
ing compositions different from pyro powder. Various types o f
powder used for special purposes will be discussed briefly in this sec-
74
TM 9-2900
M IL IT A R Y EXPLOSIVES 3 3 -3 3
lion. Other small-arms compound propellants used for military pur

poses will not be discussed in this manual as their composition and
methods of manufacture cannot be described without disclosing infor
mation regarded by manufacturers as confidential.
33. D ouble base pow ders.— a. Composition.— The term “ double
base” powder has been applied to powders containing nitrocellulose
and nitroglycerin as the principal constituents. These powders as
used by various military services usually contain from 60 to 80 per
cent o f nitrocellulose and from 40 to 20 percent nitroglycerin. Cer
tain commercial powders used in sporting ammunition are of similar
composition. The nitrocellulose used in double base powders may
be o f the pyrocellulose type containing about 12.6 percent nitrogen
or the more highly nitrated type containing above 13.0 percent nitro
gen, commonly referred to as guncotton. Small percentages o f inor
ganic salts such as potassium or barium nitrate are often used in dou
ble base powders, these salts serving the purpose o f reducing flash or
rendering the powder more ignitible. When the percentage of nitro
glycerin in the powder composition is small or when the powder is to
be extruded, it is customary to use a volatile solvent to colloid the
powder. With compositions containing a high percentage o f nitro
glycerin and which are granulated in thin sheets or discs by rolling,
the volatile solvent may be omitted since nitroglycerin is in itself a
solvent for nitrocellulose, and the rolling operation colloids the
powder to the desired degree.
b. Characteristics and m e .—The energy content o f nitroglycerin is
considerably higher than that for nitrocellulose and, therefore, pow
ders containing nitroglycerin have higher potential than straight
nitrocellulose powders, the difference increasing with the percent of
nitroglycerin present. The double base powders are also more read
ily ignitible and have a higher rate o f burning. These characteris
tics have led to the use o f such powders in trench mortars where
especially rapid burning is required. They are also used in certain
high velocity weapons where the high potential of the double base
powders is favorable.
c. Inspection tests.— (1) General.— In the inspection o f the double
base powders, the usual chemical stability, and ballistic tests are con
ducted. Since the chemical and ballistic test requirements vary with
the various types o f powder but the stability requirements are com
mon to all, the latter requirements only are given in (2) below.
(2) Heat test at 120° C .—The heat test at 120° C. is used to deter
mine stability. All powders are required to withstand this test for
at least 40 minutes without changing the color o f the test paper, and
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TM 9-2900
3 3 -3 4 M IL IT A R Y KXPLOSIVES
to show no evidence o f mines in 60 minutes. The procedure for this

test is as follow s: 2.5 grams o f the sample are placed in each o f two
tubes of heavy glass having the following approximate dimensions:
length, 290 mm., outside diameter, 18 mm.; inside diameter, 15 mm.
Each o f the tubes is closed with a cork stopper through which has
been cut a. hole or groove of about 2-nnn. diameter. A piece of
standard normal methyl violet paper 70 mm. long and 20 mm. wide
is placed in each tube so that its lower edge is 25 mm. above the
powder. These tubes are placed in a hath at a temperature o f 120.0
±0.5° C. so that no more than G or 7 mm. o f each tube project out
side the bath. The tubes are examined by withdrawing about one-
lnilf their length outside the bath and replacing immediately. The
tubes are examined every 5 minutes after the first 20 minutes have
elapsed. The time in which the methyl violet paper has turned
completely to standard salmon pink in either tube is reported. A fter
60 minutes the tubes are examined against a white background for
evidence o f fumes.
34. E. C. P ow d er.— a. Composition and vac.— This propellant is
generally used for loading blank cartridges and hand grenades. It
consists o f semieolloided nitrocellulose granulated with inorganic
nitrates.
b. Manufacture.— The main point observed in manufacture is
proper incorporation and mixing o f all ingredients. This process is
usually conducted by means o f a wheel mill in a manner somewhat
similar to that used fo r black powder. Nitrocellulose o f approxi
mately 13.15 percent nitrogen is mixed with about 16 percent o f a
mixture o f equal parts of potassium nitrate and barium nitrate, to
gether with a small amount o f diphenylamine and a pink or yellow col
oring matter. The powder mixture is granulated by adding a mixture
o f water and a suitable solvent to the material in a revolving drum
in such a manner that it forms small rounded grains. The nitro
cellulose in these grains is only partially colloided, acting as a bind
ing material and hardening the surface o f the grains as the solvent
is removed.
c. Granulation.— The granulation o f E. C. powder is such that the
powder will pass a 12-mesh and remain on a 50-mesh screen. A tol
erance o f 3 percent is permitted, that is, 3 percent o f the powder may
.remain on the 12-mesh screen, but the material remaining on the
screen must pass a 10-mesh screen, and 3 percent may pass a 50-mesh
screen.
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M ILITAR Y EXPLOSIVES 3 4 -3 5
d. Heat test at 13.\.5° C.—The powder must not turn normal

methyl violet paper to a salmon pink color in less than 30 minutes
and must not explode in less than 4 hours in this test.
S e c t io n V II
B L A C K POW DER
Paragraph
General____________ 35
Manufacture________________________ 30
Packing------------------------------------------------------------------------------------------------- 37
Inspection______________________________________________________________ 3S
Storage________________________________________________________________ 30
35. General.— a. Historical sketch.— European history contains

references to black powder as early as A. D. 1250. Roger Bacon in
12(>4 performed the first recorded experiments with this material, and
shortly after this time it was introduced as a propelling charge for the
fourteenth century bombard. Authorities differ upon the subject o f
the origin o f black powder. It lias been attributed severally to the
Chinese, Arabs, and Hindus. It is certain that the alchemists of medi
eval days were familiar to a certain extent with the properties o f the
mixture o f saltpeter, sulphur, and charcoal. Certain authorities re
gard Berchtold Schwarz as the inventor. To him at any rate belongs
the credit o f being the first (A. I). 1313) recorded user of this material
in the propelling of stones from a gun. Powder was first used in a
meal state. Later camphor was added to prevent crumbling. Grain
ing or granulating is first recorded in 1425, resulting in a stronger and
more uniform powder. Classification of the grains by screening is
reported by the French in 1525.
h. Use.— (1) Black powder gradually replaced all other devices as
a propellant, until 1870 it was practically the only propellant used.
Its present military use is practically confined to—
(a) Ignition charges.
(b) Base charge or expelling charge for shrapnel shell.
(c) Manufacture o f primers and fuses.
( d) Saluting and blank-fire charges.
( e) Time-train rings and combination fuses.
(2) It is thus seen that in its former function as a propellant, black
powder has been superseded almost entirely, having been replaced by
smokeless powder. Among some o f the factors which may be men
tioned as responsible for effecting this change are—
(a) Large quantity o f solid residue after ignition o f charge.
( b ) Volume o f smoke caused by presence o f a large quantity o f
noncombustible material.
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T M 9-290 0
(c ) Relatively great speed o f erosion o f the gun barrel due to high

temperature o f combustion.
( d) Rapid deterioration when exposed to atmospheric conditions
due to its hygroscopic nature.
36. M a n u fa ctu r e .— a. General.— (1) Precautions.— The manu
facture o f black powder is not technically complicated, but owing to
its sensitivity unusual precautions must be observed in its manufacture.
(2) Composition.— Black powder is a mechanical or physical m ix
ture o f potassium nitrate or sodium nitrate, charcoal, and sulphur in
the approximate proportions o f 75, 15, and 10, varying percentages
being used with varying effects. Potassium nitrate is used in manu
facture o f the powder for all military uses except charges for saluting
ammunition. The commercial blasting powder made with sodium
nitrate is now used fo r saluting charges. The saltpeter and sulphur
is o f a very high grade commercial quality and is practically free from
chlorides and chlorates. Purification o f saltpeter is obtained by
means o f repeated recrystallization, the formation o f large crystals
being prevented by continuous agitation o f the saltpeter liquor.
Charcoal is obtained from burning o f peeled willow, alder, or suit
able hardwood. Depending upon the use to which the particular
grade is to be put, the percentage composition o f the finished ma
terial is altered as necessity demands. It has been found, fo r instance,
that by increasing the percentage o f saltpeter the rate o f burning is
increased; by increasing the percentage o f charcoal the rate o f burning
is decreased. Extensive incorporation improves the quality and
uniformity.
l>. Process.— (1) The sulphur and charcoal in the proportions speci
fied are pulverized in a ball mill which consists o f a revolving steel
cylinder in which iron or steel balls do the crushing or grinding. This
pulverized material is mixed either with pulverized saltpeter or stirred
into a saturated solution o f saltpeter, depending on the plant equip
ment. The three methods o f m ixing are—
(a) French, which is rarely used in this country. The pulverized
saltpeter, charcoal, and sulphur are mixed and incorporated in a
ball mill in which the revolving cylinder is o f hardwood and part of
the balls are lead composition and part lignumvitae.
(&) D ry mixing, in which the ingredients are blended by hand or
by mechanical devices. In each o f the above methods a small quantity
o f water is added.
(c) W et mixing, in which the pulverized sulphur and charcoal
are stirred into a saturated solution o f saltpeter at a temperature o f
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TM 9-2900
M ILITA R Y EXPLOSIVES 3 6 -3 7
about 130° C. (265° F .). The mass is then spread on a floor to

cool, after -which it is ready for incorporation. The lumps formed
in the cooling are easily broken.
(2) After mixing by either o f the above methods, the material is
spread on the bed o f the wheel mills in quantities of 300 pounds per
wheel mill. The wheels, weighing 8 tons each, rotate on the material
for 3 hours at 10 rotations per minute. Edge runners keep the material
worked toward the center o f the tread o f the wheels. Wheel cake
or clinker formed during this operation is crashed or broken before
pressing.
(3) In order to obtain uniform ballistic results, it is necessary
that the powder be of uniform density before granulation. The hori
zontal hydraulic press has been found to be the best type for this
operation. The press plates, usually o f aluminum, are so placed as
to give press cake approximating <% inch in thickness and about 24
inches square. The effective pressure on the press cake is about
1,200 pounds per square inch.
(4) The press cake is cracked or granulated in the corning mill
by feeding the cake between crusher rolls. Mechanically operated
shaking screens separate the dust and coarse grains from the finished
grain, the coarser lumps passing through successive crushing rolls,
four sets o f crushing rolls being the usual number per mill. The
operation is considered as the most hazardous o f the various opera
tions in the manufacture o f black powder. Many devices have been
employed to reduce the loss of property and life in the corning mill
to a minimum.
c. Finishing.— Rounding or polishing the grain is accomplished by
tumbling in a revolving wooden cylinder. Drying may be done in
the same cylinder by forcing a current o f warm air through the
cylinder while the powder is being polished, or the powder may be
removed from the cylinder and dried in stationary wooden trays.
T o glaze the grains a small quantity o f pulverized graphite is added
to the powder while the powder is hot from the tumbling process and
the process continued for about half an hour. The drying and glazing
process, when carried out on the single operation plan, requires
approximately 8 hours.
37. P a ck in g .— Before packing, the powder is rescreened and sepa
rated into grades according to specification requirements. Containers
for black powder are made o f soft steel and average about 9 inches
in diameter by 11 inches high, capacity 25 pounds, painted black, sten
ciled to show grades, lot number, maker, and contract number.
79
TM 9-2900
38 M ILITA R Y EXPLOSIVES
38. In sp ectio n .— a. Grades.— (1) The various grades o f black

powder specified by U. S. Army specifications are as follows for
potassium nitrate powder, using U. S. standard sieves:
Wire screen
Designation
Passer Duster
Army black powder: O pin in g, O pening,

Grade A: ■Series number inc/tes S er in number incites
No. 1 4 0. 187 8 0. 0937
No. 3 _________________ 12 . 0661 10 . 0469
No. 4 _____ 16 . 0469 40 . 0165
No. 5 ________ ______ 40 . 0165 100 . 0059
No. 6 ______ _____ ____ 100 . 0059 140 . 0041
Fuze powder 140 . 0041
(2) Sodium nitrate powders have the following granulations:

(а) Class A :
Through a No. 12 sieve, 100 percent.
Through a No. 16 sieve, not less than 45 percent.
On a No. 40 sieve, not less than 99 percent.
(б) Class B:
Through a No. 4 sieve, 100 percent-.
On a No. 16 sieve, not less than 99 percent.
(3) In addition, Class A powder is used in pellet form, one or
two pellets constituting a saluting charge. The above powders are
intended for use as follow s:
Designation Uses
Army black powder:

Grade A:
No. 1_____ All igniting charges and the M l, M1B1, M21, and
M22 primers; it may be used for saluting charges.
No. 3........ . Special uses.
No. 4_____ Base charges for shrapnel; base charges for fuzes;
friction primers, M1914, obturating friction
primers; M23 and M25 primers; smoke-puff
charges; bursting charges for practice bombs;
practice loaded projectiles; and certain subcaliber
shell.
No. 5 ____________ Pellets for primers and fuzes.
No. 6_____ _____ Do.
Fuze powder________ Loading time-train rings.
Sodium nitrate pow
der:
Class A ................ Saluting charges.
Class B _________ Practice bombs.
80
TM 9-2900
b. Tests.— Methods prescribed for testing are as follows:

(1) Samples.— About 50 grams o f the original sample are crushed
in small portions in a porcelain mortar and passed through a 60-
mesh sieve. All precautions are taken to avoid unnecessary exposure
of the sample to air during this treatment. I f each portion is placed
in a stoppered bottle as soon as sifted, there is no appreciable change
in hygroscopic moisture content. The powdered sample is well mixed
before its analysis is begun.
(2) Moisture.— About 2 to 3 grams of the ground sample to pass
at least 60-mesh fineness are spread in a thin layer on a tared 3-inch
watch glass, carefully weighed, and dried over sulphuric acid in a
desiccator for 3 days or in a drying oven at a temperature of 60°
to 70° C. to constant weight (about 2 hours). Cooled in desiccator
and weighed. Loss of weight is calculated as percent moisture.
(3) Potassium nitrate.— Into a tared Gooch crucible provided
with an asbestos mat a known weight, approximately 10 grams, of
sample is weighed. By means of suction about 200 cc. of hot water
in successive portions of 10 to 15 cc. each are drawn through the
crucible. The final portions of water passing through the crucible
are tested with an excess of strong sulphuric acid containing a few
crystals of diphenylamine until there is no blue color reaction in
dicating the presence of nitrates. The crucible is dried for 1 hour
at 70° C. and weighed. The percentage loss in weight minus the
moisture content is considered as the potassium nitrate content. (It
is recognized that this includes any water-soluble portion o f the char
coal or sulphur.) To test purity of the nitrate, 1 cc. of nitric acid
(1.42 sp. gr.) is added to the water extract and evaporated to dryness
and dried at 150° C. The residue is mixed and 1 gram tested for
nitrogen content in a nitrometer. The nitrogen content o f the residue
should be 13.84 percent ±0.03 percent.
(4) Sulphur.—The dried and weighed material left from the ex
traction with water consists of the sulphur and charcoal. The sul
phur is determined by loss of weight on extraction with carbon di
sulphide in the Wiley extractor or other suitable extraction apparatus,
drying the insoluble residue to constant weight at about 100° C.
Before drying this residue in a hot oven, the carbon disulphide
should first be allowed to evaporate by placing the crucibles in a
warm place away from any flame or other source o f high temperature,
as the vapors of carbon disulphide are very inflammable.
(5) Charcoal.—The residue left from extraction of the sulphur
is the charcoal which is weighed direct as already noted.
(6) Ash .—The ash o f the charcoal is determined by ignition o f
the insoluble residue over a Bunsen burner until all of the carbon
240541 81
TM 9-2900
38 M ILITA R Y EXPLOSIVES
lias been burned off, and weighing. The. ash usually amounts to
about 0.5 to 1 percent o f the total powder. An unusually high value
for ash may indicate incomplete extraction with water.
(7) Specific gravity .— A known weight o f approximately 10 grams
is placed in a strong 50-cc. specific gravity bottle with a perforated
glass stopper. The bottle is filled y2 to % full with clean mercury,
placed under vacuum, and the remaining space filled with mercury.
The bottle containing the powder and mercury is weighed at 19° to
21° C. Actual weight o f the bottle plus mercury plus powder sub
tracted from the gross weight o f bottle full o f mercury, plus the
powder taken at 19° to 21° C. represents the weight o f mercury dis
placed. This weight divided by the specific gravity o f mercury at
19° to 21° C. (13.59) gives the weight o f an equal volume o f water.
The weight o f the powder used divided by this weight o f water repre
sents the specific gravity of the powder.
N o t e . —To displace the air from the specific gravity hottle, a piece of heavy
rubber tubing about 2 feet long is attached to the bottle. The other end of the
rubber tubing is attached to one leg of a Y-tube. The other leg of the tube is
extended by means of a small piece of glass tubing and rubber tubing to dip into
a vessel containing mercury. The stem of the Y Is connected with the suction
line. The rubber tube leading to the mercury vessel is closed by means of a
pinch cock. The suction is applied, the specific gravity bottle evacuated, and
the suction line closed by means o f a pinch cock placed close to the specific
gravity bottle. The pinch cock on the tubing leading to the mercury vessel is
opened to allow the mercury to flow into the specific gravity bottle. This op
eration is repeated until the bottle is filled with mercury.
(8) Granulation determination.—A sample o f about 100 grams of
the powder is weighed out accurately, emptied into the passer screen,
and shaken vigorously over a sheet o f brown paper for exactly 1
minute. Tbe powder which has passed through the screen is set
aside. The material remaining in the sieve is emptied onto the sheet
o f brown paper, striking the screen sharply with the fingers to remove
any adhering powder grains. The material so obtained is sifted
again for exactly 1 minute, the sieve emptied, and any grains ad
hering to the mesh removed, after which the material is submitted to
a third sifting. The material which lias now failed to pass through
the screen is collected, weighed to the nearest tenth o f a gram, and
the percentage o f powder which failed to pass through the passer
screen is calculated. All the material which has been used in the
passer screen test is now emptied onto the duster screen and sifted
three times as described above, collecting each time the material
which passed through the screen. This material is collected, weighed,
and the percentage o f powder which passed through the duster screen
calculated.
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TM 9-2900
(9) Moisture- and ash-free.—Percentages on a moisture- and ash

free bases are calculated by dividing the percentages o f potassium
nitrate, sulphur, and carbon, respectively, by the remainder obtained
by subtracting the sum of the percentages of moisture and ash from
the sum total o f the percentages obtained for potassium nitrate, sul
phur, carbon, moisture, and ash.
39. S torage.— a. Safety precautions.— (1) In consideration of
storage o f low explosives, o f which black powder is an example, it
must be remembered that these materials are particularly sensitive
to flame or spark. The restrictions relative to carrying matches,
cleanliness o f magazine floors, smoking, and use of nonsparking tools
in general should be rigidly enforced and carefully supervised.
(2) When working in magazines where black powder is stored it
is advisable to wear safety shoes, the so-called ‘'powder shoes” .
(3) When it becomes necessary to open a box or container of black
powder it should always be done with a wooden wedge and mallet, at
least 100 feet from the nearest magazine, and in a place which is
protected from dampness or direct sunlight. No metal tools o f any
description will be used.
(4) I f it becomes necessary to repair a magazine, all explosives
should be removed to a safe distance and the building washed before
work is started.
1). Magazines.— Black powder should be stored preferably in a
bullet-proof magazine. It should not be stored in the same building
with dry picric acid, dynamite, or other high explosive. The kegs
may be placed in the magazine either on their ends with bung down,
or sides with seam down. In view o f the fact that black powder has
a tendency to absorb moisture which causes deterioration and seriously
affects properties o f the powder, it is important that the storage
magazines are dry and well ventilated.
83
C hapter 2
M IL IT A R Y H IG H E X P L O S IV E S
S e c t io n I
G E N E RA L
Paragraph
Requirements______________________________________________________________ 40
Manufacture----------------------------------------------------------------------------------------------- 41
40. R e q u irem e n ts.—When the entire field of high explosives is
considered, the term “ military high explosive” has a restricted appli
cation to a relatively small number o f substances. In determining
suitability o f a high explosive for military use, careful consideration
must be given to its various properties including—
a. Strength.
b. Sensitivity to shock or friction such as may occur in loading.
c. Ability to withstand shock o f set-back in the gun.
d. Ability to withstand penetration by bullets in the case o f drop
bomb explosives.
e. Stability.
/. Hygroscopicity.
g. Action on metals, etc.
These various requirements, together with questions o f availability o f
raw materials, have excluded many high explosives which may be
used successfully for commercial purposes.
41. M a n u fa ctu re.— In the case o f some o f the explosives discussed
in this manual, details o f manufacture are not described as such data
are regarded by manufacturers as confidential,
S e c t io n II
T R IN IT R O T O L U E N E (T N T )
Paragraph
G eneral_________________________________________________________________ 42
Properties_______________________________________________________________ 43
Manufacture_____________________________________________________________ 44
Nitration________________________________________________________________ 45
Purification_____________________________________________________________ 46
U se_____________________________________________________________________ 47
Inspection_______________________________________________________________ 48
Storage__________________________________________________________________ 49
42. G eneral.— a. Uses.— Although trinitrotoluene was known as
early as 1863, it was not suggested as an explosive until about 1890,
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TM 9-2900
and its importance from a military standpoint dates from 1904.

Since that time it has appeared as the principal constituent, of many
explosives, and has been used by itself under such various names as
triton, trotyl, tolite, trilite, trinol, tritolo, etc. It is commonly known
in this country by the abbreviation TNT. The term trinitrotoluol,
which is more generally used than trinitrotoluene, is less correct from
the chemical point of view than the latter.
b. Characteristics.— The importance of this explosive is based upon
its relative safety in manufacture, loading, transportation, and stor
age, on the fact that it is not hygroscopic, on the lack o f any tendency
to form unstable compounds with metals, and upon its powerful,
brisant, explosive properties.
43. P roperties.— a. Color and solubility.— TN T usually resembles
in appearance light brown sugar, although in different grades o f
refinement or purity its color and appearance vary. When pure it is
a crystalline powder o f very pale straw color. It dissolves readily in
ether, acetone, alcohol, and various other solvents, but it is practically
insoluble in water.
b. Classification.— TN T is classified in U. S. Army Specifications
into two grades designated as grade I, with a setting point of 80.2° C.
minimum, and grade II, with a setting point of 76.0° C. minimum.
Grade II is obtained directly by the nitrating process as described
below, while grade I must be prepared by recrystallization or by spe
cial chemical treatment of grade II material.
c. Safety 'precaution.— Both grades o f TN T are slightly toxic, and
it is necessary that proper precaution be taken by those engaged in
its manufacture or handling to avoid inhaling the vapors or dust from
the molten or crystalline material. Good ventilation in manufactur
ing or shell loading plants is highly essential, and personal cleanli
ness should be enforced. All clothing should be changed upon the
beginning and completion o f work.
d. Stability.— TNT is one o f the most stable of high explosives,
and when properly purified may be stored over long periods of time
without alteration. It is quite insensitive to blows or friction but
can be detonated by severe impact between metal surfaces. When
ignited by flame it burns rapidly without explosion. Burning or
rapid heating o f large quantities especially in closed vessels may, how
ever, cause violent detonation. It should therefore be melted in
equipment so arranged that the maximum temperature o f the melting
unit cannot exceed 105° C.
e. Chemical action,—While TN T has no tendency to form com
pounds with metals thereby producing sensitive salts, it will react
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TM 9 -290 0
with alkalies such as sodium hydroxide or sodium carbonate to form

unstable sodium salts which are quite sensitive. For this reason the
use o f alkalies in purification o f T N T is not permissible.
/. Detonation-.— (1) Detonator.— T N T in crystalline form deto
nates readily under the influence o f a No. G detonator (containing
1 gram o f mercury fulminate). When compressed to a high density
it requires a No. 8 detonator (containing 2 grams o f mercury fulm i
nate), and when cast it is necessary to employ a booster charge o f
pressed tetryl, or an explosive o f similar high brisance, to insure com
plete detonation.
(2 ) Rate.— T N T may be classed as a “ quick acting’' explosive. It
detonates at a rate varying from about 5.200 meters per second for
loosely compressed material to nearly 7,000 meters per second for
material cast, or compressed to its maximum density.
g. Decomposition.— (1) Formulas.— The decomposition o f T N T
on explosion may be regarded as occurring according to one or both
o f the follow ing reactions:
2C«H2(C H ,) ( N 0 2) s= 1 2 CO + 2CH 4+ H 2+ 3 N 2
or
20011,(0110 ( N 0 3) ,= 1 2 C O + 5 H 2+ 3 N 2+ 2C .
(2) Oxygen compensation mixtures.— The deficiency in oxygen as
indicated by both o f these reactions is always apparent from the
black smoke produced by the explosion o f TN T. This deficiency o f
oxygen may be compensated for by addition o f such substances as
ammonium nitrate or sodium nitrate in various proportions, the re
sulting mixtures being designated as amatol and sodatol, respectively.
44. M a n u fa ctu r e .— Manufacture o f T N T involves the follow ing
processes:
a. Nitration o f—
(1) Toluene to mononitrotoluene.
(2) Mononitrotoluene to dinitrotoluene.
(3) Dinitrotoluene to trinitrotoluene.
b. Washing finished product until free o f acid.
c. Purification by remelting and chemical treatment or recrystalli
zation.
d. Granulation, screening, and drying.
45. N itra tio n .— a. Processes.— The process for ritration o f tolu
ene with a mixture o f nitric and sulphuric acids may be carried out
in various ways, for example by the—
(1) One-stage process, where a large excess o f a strong mixed acid
is used and the temperature gradually raised, with the result that
86
TM 9-2900
trinitrotoluene is produced in the one process without transfer or

separation of spent acid from intermediate products.
(2) Two-stage process, where either mono- or dinitrotoluene is
produced in the first stage and trinitrotoluene in the second.
(3) Three-stage process, where by use o f three different acid
mixtures and different conditions o f temperature, etc., there are
successively produced mono-, di-, and trinitrotoluene.
b. Three-stage 'process*— The one-stage and two-stage processes
have been superseded by the more practical and more economical
three-stage process. A general description o f the three-stage process
follow s:
(1) First.— The normal charge used in the manufacture is
1,300 pounds o f toluene. The first step in the nitration is accom
plished by running into the nitrator approximately 1,200 pounds
o f mono spent acid. The purpose o f adding the spent acid is to
provide a very weak charge as a bottom layer so as to prevent
stripping the nitrating acid o f nitric acid and also to raise the
toluene level so that it will come in contact with the cooling coils.
I f this spent acid is not added, stripping o f the nitrating acid is
likely to occur which results in a charred mononitrotoluene. The
amount o f acid used in the mononitration is based on a nitric ratio of
1 part o f toluene to .9 parts o f nitric. The composition o f the mixed
acid is 76 percent sulphuric, 23 percent nitric, approximately. The
agitation used during this nitration should be slow enough to prevent
mixing o f the toluene and the acid; that is, a separating line between
these two components should be maintained throughout the nitration.
The acid is added through a spider distributor and the temperature
maintained at 50° C. for the first 2,000 pounds, between 50 and 55° C.
for the next 4,000 pounds, and at 55° C. for the balance o f the
charges. The nitration is accomplished by the acid dropping
through the toluene. A fter all the acid has been added, the charge
is cooked fo r 10 minutes, cooled to 45° C., allowed to settle for 15
minutes, and the acid charge run off. The acid used in this nitration
where a plant is in continuous operation is made up by fortifying
the spent acid from the dinitration.
(2) Second.— This stage consists in nitrating the mononitrotoluene
to dinitrotoluene. The mononitrotoluene obtained in the first stage
is blown from the mononitrating house to the di-tri-nitrating house
and placed in the di-tri-nitrator. The charge is first cooled to
45° C. The mixed acid used in this nitration is usually a fortified
acid made by adding nitric to a spent acid from a previous trinitra-
87
TIVT 9-290 0
tion. The strength o f the acid approximates that used in the mono
nitration, the nitric ratio being the same as for the mononitration.
The acid is added to the mononitrotoluene and the temperature
allowed to increase by 3-degree steps until it has reached a tempera
ture o f 80° to 83° C. It is held at this point for the completion o f
the nitration. A fter all acid has been added, the charge is cooked
for 30 minutes and cooled to 60° C., settled fo r 30 minutes, and the
spent acid discharged. This spent acid is forwarded to the forti
fying house fo r the addition o f nitric acid so that it may be used
in the next mononitration.
(3) Third.— In this stage, the dinitrotoluene is nitrated to trinitro
toluene. It is this stage o f manufacture that offers the most difficulty
and extremely strong acids are required to obtain a complete nitra
tion. T o do this it is necessary to employ an anhydrous acid.
Approximately 3,500 pounds o f fuming sulphuric acid is added to
the di-oil. This acid is added gradually, the temperature being
allowed to rise in 3-degree steps until a temperature o f 80° C. has
been reached. A s soon as the fuming sulphuric has been added the
mixed acid is started. The mixed acid has a composition o f 57
percent nitric and 41 percent sulphuric, approximately. The nitrat
ing temperature in this stage is 85° C. at the start with a gradual
rise in 3-degree steps until it reaches 104° C. From this point the
nitration is continued until a test o f the oil shows it has a freezing
point o f 72° C. or higher. Normally it requires 3 hours o f nitration
after all the acid is in to obtain this setting point. A fter this, the
charge is cooled to 100° C. and allowed to Settle for 30 minutes,
after which the spent acid is sent to the fortifiers and the tri-oil to
the neutralizing house.
c. Yield .— (1) Humphrey (see par. 89) states that contrary to
usual belief, yield o f T N T from the di or second nitration at a given
temperature is not the function o f the water content o f the mixture
(except that too strong an acid tends to oxidize the material and in
this manner lowers the percentage o f yield), but is rather dependent
upon the proper low temperature during nitration.
(2) The mononitration yields a product containing a mixture of
about 4 percent o f the meta nitrotoluene in addition to the ortho and
para isomers. The subsequent nitration changes the meta mononi
trotoluene chiefly into the beta and gamma trinitrotoluenes, which
differ from the alpha form in chemical properties and are regarded
as impurities. Small amounts o f other isomers o f trinitrotoluene
have also been identified in the product o f the complete nitration of
toluene. Depending upon the completeness with which the last nitra-
88
TM 9-2900
M ILITARY EXPLOSIVES 45—46
tion is performed tliere may be either a large amount of dinitro-

toluene present if improperly carried out, or, if correctly done, a
relatively small amount.
(3) In addition to these impurities, there may also be such bodies
as tetranitromethane which possesses the undesirable property o f
lowering the solidification point o f the pure alpha TNT. I f the
nitration has been properly carried to completion, there should not
be present more than 4 percent beta and gamma TNT. This condi
tion is not usually attained under manufacturing conditions and it
is therefore necessary to recrystallize the TN T or purify it by other
means in order that the impurities may be eliminated, and a product
of the required solidification point for grade I, TNT (80.2° C .),
obtained.
46. P urification.— a. Process and equipment.— The crude trini
trotoluene, which, due to the temperature of nitration, is in the form
of an oil, is run from the nitrator into neutralizing tubs which have
the shape o f a cone at the bottom. At the apex of the cone a gate
way valve for regular discharge from the tub is provided. Steam
coils for heating and air coils for agitation are both provided. Wash
water is drawn off by means of suction through a suitable pipe which
reaches the tub near the top and extends along the side wall to about
2 feet from the bottom. A small quantity of sodium sulphite can
be used to assist in the purification at this point, although it is not
necessary to do so. Washing is carried on until no test for acidity
is shown by the use o f litmus paper. The neutral TNT in the form
o f oil is now pelleted by running into cold water for transportation
to the graining house, or can be transported in the molten condition
to suitable storage tanks through heated pipe lines. I f pelleted,
these pellets are transported to storage tanks as above mentioned,
and again melted before running into the crystallizing kettles. The
storage tanks are kept at an approximate temperature of 95° C., and
are provided with a gateway screw valve from which the molten
charge is drawn off into the graining kettles. These kettles are made
of cast iron in one piece, and the junction o f the bottom and the
side walls is rounded so that plows can scrape the TNT loose from
the sides. The lower part of the kettle is fitted with a jacket into
which steam or cold water may be discharged. As the plows are
started, the charge cools down and the crystals begin to form on the
sides which increase until the whole mass becomes plastic. During
the operation all moisture is driven off and the TNT produced is in
a fine crystalline condition. The TN T produced is usually better
than grade I I ; that is, it has a melting point above 76° C. I f it is
89
TM 9-2900
desirable to obtain T N T o f grade I, recrystallization from either

sulphuric acid or other suitable solvent, or a treatment with sodium
sulphite may be made. A brief description o f each is given below.
b. Crystallization, from sulphuric acid.— The fine crystals pro
duced in the graining kettles are dissolved in hot sulphuric acid,
usually weight for weight, and cooled. The purified crystals thus
settling out are washed free from acid and regrained to such de
gree o f fineness as to pass U. S. Army specifications. The crude
material held in sulphuric acid is accumulated until such time as
the amount warrants separate purification.
c. Sulphite treatment.— The sodium sulphite treatment may be
applied by taking the fine crystals from the graining kettles, and
placing them in bins or cars which are equipped with a Filtros
bottom. These bins or cars are given one hot-water washing, then
four washings with the 5-percent solution o f sodium sulphite, then
one warm-water washing followed by sufficient cold-water washings
to remove the last traces of the red color which is formed in the
treatment. The purified crystals thus obtained can be dried, sieved,
and packed, or regrained, as may be necessary to meet specifications.
47. U se.— a. Bursting charge.— (1) Grade I T N T is slightly more
expensive than grade II because it requires the additional purifica
tion. Grade I is used as the bursting charge for high-explosive
shell, either alone or mixed with an equal weight of ammonium
nitrate to form 50/50 amatol (the T N T in either case being melted
so that the shell is filled by a casting or pouring process). Grade
I I is used only in 80/20 amatol, where it is mixed in the molten state
with four times its weight o f ammonium nitrate and filled into high-
explosive shell by hand stemming or by means o f a screw filling
machine.
(2) A charge of about iy± pounds of cast T N T .in a 75-mm high-
explosive shell weighing about 10 pounds breaks up the shell into
approximately 400 fragments retained on a 4-mesh screen.
(3) Other military uses for T N T are as a bursting charge for
rifle grenades, airplane drop bombs, naval submarine mines, depth
bombs, and as a constituent o f propellent powder. In airplane
bombs it has the disadvantage that penetration o f the bomb by a
rifle bullet may cause an explosion o f the charge. This is also true
o f amatol, which is used extensively in drop bombs.
b. Demolitions.— TN T is also used for military purposes in demo
lition work on bridges, railroads, etc., and for land mines placed
under enemy trenches or fortifications. For demolition work car
ried on by the Corps o f Engineers, the T N T is made up in the form
90
TM 9-2900
M ILITARY EXPLOSIVES 4 7 -4 8
of small, highly compressed blocks inclosed in a fiber container which,

protects them from crumbling in handling and renders them water
proof.
c. Blasting work.—TNT has been demonstrated to be suitable for
all kinds o f blasting work where 40 percent dynamite is used and to
give practically equal effects. It is well adapted for “ adobe” shoot
ing or “ mud capping,” terms applied to breaking up large rocks
or bowlders by means o f a charge o f high explosive placed on the
rock and confined only by means o f a shovelful of mud or wet earth
thrown over it. Only quick-acting explosives can be successfully
used for such work. Even in drill holes containing water, TNT
gives excellent results because of the fact that it is insoluble in water.
However, its use for blasting has been negligible because of the
fact that it is expensive as compared with commercial dynamites.
d. Detonating fuse.—“ Cordeau Bickford,” a trade designation for
detonating fuse, consists o f a flexible lead tube, smaller in diameter
than a lead pencil, filled with TNT. It is quite entensively used
in certain blasting operations, especially for insuring complete deto
nation of large charges o f dynamite. The detonating fuse, being
passed through the entire length of the charge and detonated at its
external end by means o f an ordinary blasting cap, transmits its
high rate of detonation to the entire charge o f dynamite.
48. In sp ection .— a. Specifications.— Chemical and physical re
quirements prescribed by U. S. Army specifications for the different
grades of TNT are as follows:
Grade I Ornde II
Solidification point, not less 80.2° C. 76.0° C.

than.
Insoluble matter, not more 0.10. 0.10.
than (percent).
Moisture, not more than 0.1. 0.1.
(percent).
Acidity as HaSO,, not more 0.01. 0.01.
than (percent).
Color______________ ________ Light vellow. Light vellow.
Granulation, not less than No. 14 U. S. standard No. 14 U. S. standard
95 percent shall pass sieve, opening 0.055 sieve, opening 0.055
through. inch. inch.
It will be noted that the specifications for the two grades vary only
in solidification point.
b. Tests.—The most important test in connection with the inspec
tion o f TN T is the determination o f its solidification point or “setting
91
TM 9-290 0
point.” This temperature serves as an indication o f (lie purity o f the

explosive inasmuch as the presence o f moisture, lower nitrated prod
ucts, objectionable amounts o f isomers, and other impurities all tend
to lower the solidification point. However, in order to insure proper
degree o f purity, additional determinations of insoluble matter,
moisture, and acidity are required by U. S. Army specifications.
Prescribed methods o f conducting these tests are as follows:
(1) Solidification point.— (a) Apparatus.—The apparatus used
consists o f the follow ing parts: A test tube 1 inch in diameter and 6
inches long is fitted through a cork into a second test tube V/2 inches
in diameter and 7 inches long, which in turn is set into a large-mouthed
liter bottle. Into the inner tube is fitted a cork stopper through which
are three openings. One is in the center for the standard thermometer,
which should be graduated in Vio0 c. One is immediately at the side
o f the center hole and is for a small thermometer which is passed
just through the stopper and which reading is taken as the average
temperature o f the exposed stem o f the standard thermometer in
making the stem correction. The third hole in the stopper is a small
V-shaped opening at the side, through which passes a wire whose
lower end is bent in a loop at right angles to the axis of the tube
and which is used as a stirrer.
(b) Method.— A 50-gram sample o f T N T is placed in the inner
tube and melted in an oven, maintained at 95 to 100° C, the inner tube
being separated from the rest o f the apparatus for this purpose.
When the TN T has completely liquefied, the tube is replaced in the
apparatus, the standard thermometer placed so that (he bulb is ap
proximately in the center o f the molten TNT, and the small side
thermometer put in place. The stirrer should already be in (he
molten TN T. Stirring is continued vigorously as the temperature
falls, and the thermometer must be watched very carefully. When a
point is reached where the temperature begins to rise owing to the
heat o f crystallization, readings should be recorded about every 15
seconds until the maximum temperature is noted. This temperature
usually remains constant for several minutes until crystallization is
complete, and observation should be continued until it is certain that
the maximum temperature has been reached. This takes from 5 to
10 minutes after beginning o f crystallization. This maximum tem
perature with the correction for emergent thread is taken as the
solidification point o f the sample.
(2) Insoluble matter.— A known weight, approximately 10 grams,
is boiled with 150 cc. of 95-percent ethyl alcohol or benzene, filtered
92
TM 9-2900
M ILITARY EXPLOSIVES 48-49
while hot through a tarccl Gooch and washed with hot additional
solvent. After drying to constant weight at 100 cc., the crucible is
cooled and weighed.
(3) Moisture.— A known weight, approximately 5 grams, is ex
posed in a desiccator over sulphuric acid in a watch glass for 48
hours.
(4) Acidity.—A known weight, approximately 10 grains of the
sample, is melted and shaken with 100 cc. of neutral boiling water
and allowed to cool. The sample is then remelted and again ex
tracted with 50 cc. o f neutral boiling water. The total water ex
tract is cooled and titrated with N/10 sodium or potassium hydroxide,
using phenolphthalein as an indicator. The results are calculated
as percent sulphuric acid in the original sample.
(5) Granulation,—A weighed portion of approximately 100 grams
and a small crucible lid, a 25-cent piece, or a similar object are placed
on the specified sieve and shaken for 3 minutes. The portion re
tained on the sieve is weighed and the percentage passing through the
sieve calculated.
49. Storage.— a. Magazines.— (1) Construction.—The type of
magazine best designed for storage of TNT is approximately 2G feet
wide and 42 feet long and when grouped together in a magazine area
they are usually spaced 400 or 800 feet apart. They are constructed
with concrete foundation walls or piers, hollow tile or brick walls,
and wood floors. The flat roof supported on wooden roof trusses
is o f gypsum blocks or slabs covered with a fire-resistant built-up
roofing. There are ventilators on the roof and in the foundation
walls below the floor. The openings in the foundation walls are
always well-screened or baffled to prevent entrance of sparks. The
limiting floor load is 300 pounds per square foot. The bulletproof ex
plosives magazine is similar in construction to the magazine described
above except that the hollow tile walls are filled with sand or are
made of materials which will stop rifle bullets.
(2) Capacity.—These magazines were originally designed for stor
age o f 250,000 pounds of explosives, but with ample aisle space for
inspection and shipping, and piles o f convenient height, the amount
is usually limited to approximately 100,000 pounds.
(3) Fire.—I f a fire occurs in a magazine in which TNT is stored
in wooden boxes, the explosive will usually burn quietly, but may
possibly detonate. I f the fire has gained considerable, headway be
fore it is discovered, no attempt should be made to fight the fire.
b. Safety precautions.— (1) It is desirable but not required that
safety shoes be worn when handling, storing, and shipping TNT in
93
TM 9-290 0
boxes. Safety shoes should he worn in repacking rooms or buildings,

or whenever loose T N T is being handled.
(2) Boxes should be opened and repaired with nonsparking tools.
(3) A container should never be opened in a magazine in which
explosives or ammunition are stored.
S ectio n I I I
A M M O N IU M P IC R A T E (E X P L O S IV E D)
Parn graph
G en era l____ r>o
Properties __ 51
Manufacture. 52
U se________ 53
Inspection_ 54
Storage------- __ 55
50. G en eral.— a. Historical sketch.— The use o f ammonium picrate

as an explosive was patented by Nobel in 1888 (Mosenthal, Jour. Soc.
Chem. Ind., V ol. 18, p. 44T, May, 1899), although even prior to that
time Brugere made use o f a mixture o f ammonium picrate and sodium
nitrate as a propellant explosive.
b. Characteristics.— The importance o f ammonium picrate as a
military explosive is due entirely to its marked insensitiveness to
shock and friction, which makes it well suited fo r use as a bursting
charge in armor-piercing projectiles. From the standpoint o f explo
sive strength, however, this explosive is inferior to TNT.
51. P rop ertie s.— a. Color and solubility .— Ammonium picrate is
soluble in water, crystallizing from its solution in orange-yellow
needles darker in color than picric acid. It resembles picric acid in
its bitter taste and property o f dyeing the skin, clothing, etc., o f those
engaged in its manufacture or handling.
b. Ilygroscopicity .— It has a much greater tendency to absorb mois
ture than has picric acid, samples having been found to absorb over
5 percent by weight o f water during storage fo r 1 month in an
atmosphere saturated with moisture.
c. Chemical action.— Like picric acid, ammonium picrate can react
with metals to form metallic picrates, but it reacts with much less
readiness than picric acid; in fact, when dry its action is almost
negligible. W et ammonium picrate reacts slowly, especially with
copper or lead, to form picrates which are particularly sensitive and
dangerous.
94
TM 9-2900
d. Heat action.—Ammonium picrate does not melt on heating, but

explodes when heated to a temperature of about 300° C. Small
traces of metallic picrates may however lower this ignition tempera
ture appreciably.
e. Sensitiveness.—Ammonium picrate is the least sensitive of all
military explosives used as the bursting charge for shell. Its insensi
tiveness to shock accounts for it being given preference over TNT or
amatol as the bursting charge for armor-piercing, base-fuzed shell.
It is also more insensitive to detonation by means o f mercury ful
minate than is TNT. A t a pressure of about 12,000 pounds per
square inch the two explosives have the same densities, about 1.48.
/. Toxicity.—Like TN T and picric acid, ammonium picrate liber
ates free carbon on explosion, giving a black smoke. The products of
explosion, although more disagreeable in odor, are less poisonous than
those from TNT and picric acid in that they contain less carbon
monoxide.
52. M anufacture.— a. Process.—The manufacture of ammonium
picrate consists in the main of a simple neutralization o f picric acid
by means of ammonia either alone or in combination with ammonium
carbonate. This process is not attended with any serious manufac
turing difficulties or dangers, provided one excludes the possibility
o f leaking ammonia pipes.
1). Method.—Details o f manufacture are as follows: Approxi
mately 300 pounds of picric acid are mixed with 500 gallons of
water at room temperature and then slowly heated by direct steam.
As the mixture warms, aqua ammonia is added at the bottom of the
tank until neutralization is completed. In some factories it was the
practice to add a faint excess, thus insuring complete neutralization
of all the picric acid, this condition being evidenced by the forma
tion o f a reddish colored crystalline mass o f ammonium picrate.
U. S. Army Specifications permit a maximum of .025 acidity or
alkalinity. When this stage has been reached the resulting material
is dropped into tanks for crystallization. These tanks are so
equipped that a continual agitation of their contents can be main
tained by air with the object of accelerating the crystallizing of the
ammonium picrate during the cooling. When the mass has cooled to
about 25° C. the crystals are separated from the mother liquor by
filtering or draining. From the crystallizing tank the ammonium
picrate is taken to the dry house where it is subjected to a tempera
ture o f about 45° C. for 8 hours in drying bins which are so con
structed that warm air circulates constantly through the mass.
Finally the dried material is screened by means of a rotating screen
TM 9-2900
and sent directly to the packing room. The finished product is then
packed in 50-pound boxes lined with waterproof paper and sent
to storage.
c. Reworking ammonium picrate.— This operation consists in re
dissolving impure or waste ammonium picrate in water, removing
the impurities by filtration, then heating the solution by steam coils
until it has been evaporated sufficiently to produce crystallization.
From here on the reworking operations are exactly the same as those
followed out in the manufacture o f the new material.
53. U se.— As has been mentioned, ammonium picrate is used as
the bursting charge for armor-piercing shell on account o f its in
sensitiveness to shock which permits the shell to pass through the
armor without exploding. Owing to the fact that it cannot be
melted without decomposing, it must be loaded into the shell by
pressing. The interior o f the shell is covered with a suitable non-
metallic paint or varnish. It has no commercial use as an explosive,
although it enters into the composition o f numerous patented blasting
explosives which have not been used to any great extent.
54. I n s p e ctio n .— a. Specification*.— U. S. A rm y Specifications
prescribe the following requirements for ammonium picrate:
(1) Ammoniacal nitrogen, not less than 5.64 percent.
(2) Moisture, not more than 0.2 percent.
(3) Solubility, not more than 0.2 percent insoluble.
(4) Ash, not more than 0.2 percent.
(5) Acidity or alkalinity, not more than 0.025 percent.
(6) Color, yellow to red.
(7) Granulation:
(a) Through No. 14 U. S. standard sieve, 99.5 percent minimum.
(?>) Through No. 100 U. S. standard sieve, 20 percent maximum.
b. Test*.— The following tests and determinations are made on
ammonium picrate to determine its suitability for military use:
(1) Ammoniac at nitrogen .— A known weight, approximately 1 gram
o f the ammonium picrate to be analyzed, is placed in a 500-cc.
Kjeldahl flask. The flask is equipped with a two-hole rubber stop
per which carries an exit tube leading away to a bottle containing N/10
sulphuric acid, and an ingress tube reaching to its bottom, through
which air that has already been dried and freed from ammonia by
passage through concentrated sulphuric acid may be bubbled. Twenty
cc. o f water is introduced into the flask, 12 cc. o f 5-percent sodium car
bonate solution added, the flask set in a boiling water bath and
ammonia-free air bubbled through until contents o f the flask have
96
TM 9 -2 9 0 0
been evaporated to dryness. The ammonia is absorbed by bubbling

the air through 50 cc. of N/10 sulphuric acid, a bulb full of very
small holes such as may be made conveniently with a hot. platinum
wire being used for the purpose. To deal with the possibility of
splashing of the sulphuric acid, the exit tube from the bottle is
equipped with a trap. The excess sulphuric acid is titrated with
N/10 sodium hydroxide, using methyl red or sodium alizarin sul-
phonate as an indicator, the amount which has been consumed is
noted, and the ammoniacal nitrogen in the sample is calculated as
follows:
_ , 1.401 (A B — CD)
Percentage of ammoniacal nitrogen =
where A —number of cc. of sulphuric acid solution in bottle.

B = normality of sulphuric acid solution.
C==number of cc. o f sodium hydroxide solution used.
D=norm ality of sodium hydroxide solution.
E = weight of sample.
(2) Moisture.— A sample of about 5 grams of the ammonium
picrate is accurately weighed in a previously tared wide-mouthed
weighing bottle at least 1y2 inches in diameter and dried for 2 hours
or to constant weight in a drying oven at 100° C. The loss of weight
is calculated as percentage of moisture in the original sample.
(3) Insoluble material.—A known weight, approximately 10
grains, is dissolved in 150 cc. o f hot distilled water by boiling for 10
minutes. The solution is filtered through a tared Gooch filter, the
insoluble residue washed thoroughly with hot water, and dried for
1 hour at 100° C.
(4) Mineral matter (ash).—A known weight, approximately 2
grams, is wetted with molten paraffin in a tared crucible and care
fully burned until all carbonaceous residue has been eliminated. It
is cooled in a desiccator and weighed.
(5) Acidity or alkalinity.— A representative sample o f 5 grains of
the ammonium picrate is ground in a porcelain mortar with 50 cc.
o f water at room temperature, and the supernatant liquid poured
through a folded filter, the filtrate being caught in a 500-cc. Erlen-
meyer flask. This process is repeated until all of the ammonium
picrate is brought into solution and the total volume o f the filtrate
is 250 cc. Three drops o f sodium alizarin sulphonate or a 1-percent
alcohol solution of methyl red indicator are added. The solution is
acid as shown by either o f the indicators assuming a yellow color. I f
the solution is acid, it is titrated with approximately 0.1 N sodium
21!) 541°— 40- 97

TM 9-2900
54-55 M IL IT A R Y EXPLOSIVES
hydroxide solution and the percentage o f picric acid in Ihe sample

calculated as follow s:
Percentage o f picric acid = 22.905 AB
where A = number o f cc. o f sodium hydroxide solution used.

B== normality o f sodium hydroxide solution.
C =w eight o f sample.
I f the solution is alkaline as shown by the indicator assuming a
purple or red color, it is titrated with approximately 0.1 N sulphuric
or hydrochloric acid. The percentage o f free ammonia in the sample
is calculated as follow s:
„ , , , . 1.7034 AB
Percentage ot tree ammonia n
0
where A = number o f cc. of acid solution used.
B =norm ality o f acid solution.
C = weight o f sample.
(6) Granulation.—A No. 14 U. S. standard sieve is fitted on a No.
100 U. S. standard sieve and a receiving pan attached to the bottom
sieve. A weighed portion o f 100 grams o f the sample and two metal
washers are placed on the upper sieve, covered, and shaken 3 minutes.
The material retained on the No. 14 sieve and that passing through
the No. 100 sieve are weighed and calculated each in terms of
percentage.
55. S torage.— a. Regulation*.— Storage o f ammonium picrate is
governed by the same regulations as are applicable fo r the storage
o f TN T both as to type of magazine and rules for handling, and
special regulations governing this particular explosive are not
necessary.
b. Special precautions.— (1) Ammonium picrate which has been
pressed at a shell-loading plant and removed from a shell is very much
more sensitive to shock or blow than new material, and there are
cases on record where serious accidents have happened in the
loading o f shell with ammonium picrate so treated. I f it becomes
necessary to store this material, special precautions should be ob
served to protect it against shock or fire, and it preferably should
be stored in a building by itself.
(2) Although less sensitive than T N T ammonium picrate can be
exploded by severe shock or friction, is highly inflammable, and
when heated to a high temperature may detonate. It is therefore
necessary that it be treated with proper care as a high explosive.
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TM 9-2900
c. Magazines.— Since it absorbs moisture it should be stored ill dry

magazines and protected from dampness. Moisture, however, has
no effect on ammonium picrate except to reduce its explosive strength
and its sensitiveness to detonation.
<1. Containers.— Ammonium picrate is always stored in wooden
containers because of the possibility o f its forming metallic picrates
in contact with metals, especially when moist.
S ection TV
PICRIC A CID
Paragraph
General----------------------- 56
Properties----- ------------------------------------------------------------------------------------ 57
Manufacture------------------------------------------------------------------------------------------ 58
Use------------ 50
Inspection____________________________________ 60
Storage________________________________________________________________ 61
56. General.— Picric acid or trinitrophenol was first adopted as a

military high explosive by the French Government in 1886 under
the. name of melinite, and has since been used to a greater or less
extent by almost all countries with or without addition of various
materials intended to reduce its melting point. The British ex
plosive designated as lyddite and the. Japanese explosive schimose
are both cast picric acid, and various names are given to other shell
explosives the chief component o f which is picric acid.
57. P roperties.— a. Color and solubility.— Picric acid is a lemon -
yellow, crystalline solid, only slightly soluble in cold water but
soluble in alcohol, benzene, and other organic solvents. A very small
amount is, however, sufficient to color a large volume of water a
distinct yellow color. It likewise stains the skin o f workmen, colors
clothing, hair, and everything else with which it comes in contact,
and lias an exceedingly persistent, disagreeable, bitter taste. Its
property of coloring is utilized in the dye industry, and in fact, picric
acid was long known as a dyestuff before its explosive nature was
discovered. It lias no tendency to absorb moisture from the air.
b. Heat action.— Picric acid melts at a temperature of about
122° C. when pure, and is usually required for explosive use to have
a melting (or solidifying) point o f at least 120° C.
c. Chemical action.— Being an acid, it. has the property o f combin
ing with ammonia and alkalies and with many of the metals, form
ing salts which are called picrates. Some o f the picrates are much
more sensitive than picric acid itself, and it is therefore necessary
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that formation of tlie.se pierates be avoided by keeping picric acid

from direct contact with those metals with which it readily reacts.
<1. Precautions.—Picric acid is not as toxic as T N T and the chief
danger in connection with its use is probably the fumes given off
from the molten explosive in loading shell. While practically no
trouble from poisoning results in manufacture or handling o f picric
acid, care must be taken, however, to avoid breathing the large
amounts o f picric acid dust that may arise in screening or packing
the dry material.
e. Stability*— Picric acid is entirely stable, Tl has no tendency to
decompose at any temperatures which it might meet in storage. On
sudden heating at temperatures much above its melting point
(122° C.) it may explode, although many cases are noted where con
siderable quantities o f picric acid have burned without explosion.
Presence o f any trace o f explosive that will detonate more readily
such as metallic pierates may cause sudden detonation o f burning
picric acid.
/. Detonation.— It has about the same sensitivity to shock or fric
tion as T N T and is somewhat more readily detonated by means o f a-
detonator. Picric acid is one o f the most powerful of military explo
sives. Its high strength or concussive effect is due to its high rate
o f detonation which, for the. cast or highly compressed explosive, is
about 7,000 meters per second, slightly greater than that o f TN T
under the most favorable conditions. By both the Trauzl lead block
test and the ballistic pendulum test, picric acid shows appreciably
greater strength than TNT, being exceeded only by tetryl and TNA.
The results o f these methods o f testing are confirmed by actual frag
mentation tests o f high-explosive shell where it is found that a larger
number o f shell fragments are produced from picric acid than from
TN T at equal loading densities.
58. M a n u fa ctu re.— a. Material.— The raw material from which
picric acid is derived is benzene (often called benzol). This sub
stance must not be confused with benzine which is essentially gasoline
obtained by distillation o f petroleum. Benzene is an inflammable-
liquid obtained as a byproduct in manufacture o f coke, by recovery
from illuminating gas, or by “cracking” oils at high temperatures.
b. Processes.—Picric acid may be manufactured from benzene by
two distinct processes designated respectively as the phenol and the
chlorbenzene process.
(1) Phenol.— (a) Benzene conversion.— Practically all o f the
picric acid produced in this country during the W orld W ar was made
from phenol (carbolic acid). Phenol is prepared from benzene as a
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TM 9-2900
raw material by first treating pure benzene with strong sulphuric

acid and heating the mixture in jacketed iron kettles provided with
agitation at a temperature of about 90° C. for several hours. The
resulting benzene sulphouate is usually treated with lime which con
verts it to calcium benzene sulphouate, which in turn is converted to
sodium benzene sulphouate by means o f sodium carbonate (soda
ash). The sodium benzene sulphouate is dried and heated in fusion
kettles with caustic soda which converts it into sodium phenate. The
fusion mixture is dissolved in water and treated with either carbon
dioxide or sulphuric acid which causes the phenol to separate out as
a distinct layer. This layer is drawn oft' and distilled in order to
separate the pure phenol from water and other impurities. Pure
phenol is a. white crystalline solid which melts at about 40° C.
(b) Phenol conversion.—For conversion to picric acid the phenol
is melted into large jacketed iron kettles and treated with sulphuric
acid o f about 93 percent strength, the mixture heated with stirring
at a temperature o f about 95° C. from 4 to 6 hours. The resulting
phenol sulphonic acid is diluted with water and treated in a large
acidproof, brick-lined nitrator with 42° Baume nitric acid (about
70 percent), The reaction generates heat and the mixing is therefore
carried on very slowly, the maximum temperature being about 110° C.
After cooling the mixture, the crystallized picric acid is separated
from the spent, acid on a vacuum filter, washed with water, and dried.
(2) Chlorbenzene.—Although this process has been quite extensively
used abroad, its use in this country until recently has been rather
limited. Briefly, the process involves first, treatment o f benzene with
gaseous chlorine whereby monochlorbenzene results. This product is
purified by distillation and then nitrated with a mixture o f nitric acid
and sulphuric acids to give dinitrochlorbenzene. The latter on treat
ment with lime or soda loses its chlorine and becomes calcium or
sodium dinitrophenolate, which on acidifying is converted to dini-
trophenol. The dinitrophenol is readily nitrated to picric acid (tri-
nitrophenol) by means of nitric and sulphuric acids.
59. U se.— a. General.— The fact already noted that picric acid
combines readily with some metals to form pierates which are unduly
sensitive to friction, shock, or heat has been detrimental to the use of
picric acid for military purposes in spite of the fact that it is a
stronger explosive than TNT. When a nonmetallic lining is used for
the shell cavity as for instance, certain lacquers, varnishes, or paints,
danger o f formation o f these salts is obviated to a great degree.
Introduction of TNT as a military explosive has resulted in gradual
abandonment of picric acid by practically every country except France
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TM 9-2900
where it was largely used during the W orld War. In the. United
States it is used for conversion into “ Explosive D ” or ammonium
picrate which is used in base-fuzed shell fo r seacoast cannon. Picric
acid has also found use as a booster explosive, and even as a substitute
for part o f the mercury fulminate charge in detonators.
b. Mixture*.—Picric acid has been used extensively in the form of
mixtures with other nitrocompounds. Such mixtures having a lower
melting point than picric acid can be melted and cast at temperatures
below 100° C. The mixtures are more generally practicable because
o f the hazard involved in melting picric acid at the relatively high
temperature required. Some o f the compounds which have been used
with picric acid are trinitrotoluene, trinitrocresol, trinitrobenzene,
and the di and mono nitro derivatives o f phenol, cresol, and naph
thalene. Little, if any, change in brisance results from the addition
o f the trinitro compounds, but the addition o f the mono and dinitro
compounds causes a reduction in brisance in proportion to the amount
added.
60. In sp e ctio n .— a. Specifications.—Chemical requirements pre
scribed for picric acid by II. S. Arm y Specifications are as follow s:
(1) It must have a solidification point o f not less than 120° C.
(2) It must contain—
(a) Moisture, not more than 0.2 percent if purchased dry, and not
more than 22 percent if purchased wet.
(&) Sulphuric acid, not more than 0.1 percent, both free and com
bined.
(c) Nitric acid, no free.
(d) Ash, not more than 0.2 percent.
(c) Material insoluble in water, not more than 0.2 percent.
( / ) Lead, not more than 0.0004 percent.
(3) It must be o f a white to yellow color.
(4) Not less than 99.5 percent shall pass a No. 14 IT. S. standard
sieve.
(1) Solidification, point.— A sample o f the picric acid to be used
for this test must be dried to constant weight at a temperature not
exceeding 50° C. The apparatus used consists o f the following parts:
A test tube 1 inch in diameter and 6 inches long is fitted through a
cork into a second test tube iy2 inches in diameter and 7 inches long,
which in turn is set into a large-mouthed liter bottle. Into the inner
tube is fitted a cork stopper through which are three openings. One
is in the center for the standard thermometer which should be grad
uated in i/10° C. One is immediately at the side o f the center hole
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T M 9 -2 9 0 0
and is for a small thermometer which is passed just through the

stopper and which reading is taken as the average temperature o f
the exposed stem o f the standard thermometer in making the stem
correction. The third hole in the stopper is a small V-shaped open
ing at the side through which passes a w'ire whose lower end is bent
in a loop at right angles to the axis of the tube and which is used as
a stirrer. The inner test tube is removed and charged with approxi
mately 50 grams o f the sample. It is than placed in an oven at a
temperature of 130° C. until the picric acid has attained the tempera
ture o f the bath throughout. The tube is then assembled in the
apparatus for cooling, the standard thermometer graduated in Vio°
immersed in the picric acid with its bulb in the center o f the molten
mass, and stirring continued vigorously as the temperature falls.
The temperatures o f both thermometers should be recorded every 15
seconds in order to note the maximum temperature reached on the
slight rise o f temperature which results during crystallization. This
maximum temperature corrected for emergent mercury column is
taken as the solidification point.
(2) Moisture.■—A sample o f about 5 grams of the picric acid is
accurately weighed in a previously fared wide-mouthed weighing
bottle at least 1i/2 inches in diameter, and dried for 5 hours or to
constant weight in a drying oven at 70° C. The loss o f weight is
calculated as percentage o f moisture in the original sample.
(3) Sulphuric acid.— A known weight of picric acid, approximately
10 grams, is dissolved in 250 cc. boiling distilled water, filtered and
washed with 25 cc. o f hot distilled water, acidulated with hydrochloric
acid, and the solution heated. A slight excess o f hot solution o f barium
chloride is then added with constant stirring, the precipitate allowed
to settle, and filtered while hot on a fared Gooch crucible. The latter is
washed thoroughly with hot water, dried for 3 hours at 100° C., and
the weight of BaSCh calculated as H 2SO* in the original sample.
(4) Nitric acid.—A water solution o f picric acid is tested with a
solution o f diphenylamine in concentrated sulphuric acid. No colora
tion should result.
(5) Ash,— A known weight, approximately 5 grains, is moistened
with strong sulphuric acid in a fared crucible and carefully burned
until all carbonaceous residue has been eliminated. To compensate
for reduction o f metallic salts, a few drops o f nitric acid and sulphuric
acid are added, carefully evaporated, the crucible again ignited, cooled
in a desiccatoi-, and weighed.
(6) Insoluble material,— 10 grams o f the sample is dissolved in 150
cc. o f boiling water, boiling continued for 10 minutes. The solution is
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TM 9-290 0
filtered while hot through a fared Gooch crucible which is washed

thoroughly with hot water, and dried fo r 2 hours at 100° C.
(7) Lead.— A known weight, approximately 300 grams o f the picric
acid, is placed in a 2-liter flask and allowed to soak in 100 cc. o f a hoi
saturated solution o f barium hydroxide in 65 percent alcohol. The
flask is well shaken, 1,400 cc. o f 95 percent alcohol added, and the whole
allowed to digest at a temperature below the boiling point o f alcohol
until all the picric acid has been dissolved with the exception o f small
particles o f insoluble matter. The solution is shaken thoroughly and
allowed to stand in the cold until most o f the picric acid has crystal
lized out, then filtered. It is not necessary to disturb the crystalline
picric acid at the bottom o f the flask as only 500 cc. o f the solution is
used for completion o f the tests and this amount can be decanted. To
500 cc. o f this filtered solution which represents 100 grams o f picric
acid, four or five drops o f nitric acid and 10 cc. o f a 1 percent mercuric
chloride solution are added and a slow stream o f hydrogen sulphide
passed through this solution for 15 minutes. A fter allowing to settle
20 minutes, the solution is filtered and the precipitate washed with
alcohol saturated with hydrogen sulphide, the filter paper dried and
ignited in a porcelain crucible; 9 cc. o f nitric acid, sp. gr. o f 1.42, is
added and the solution warmed on a hot plate. Enough warm water
is then added to make up the volume to 50 cc. The solution is electro-
lized with a current o f 0.4 ampere and 2^ volts, temperature 65° C.
using a tared platinum anode. A fter 1 hour, the electrode is washed
by replacing the beaker with another one full o f distilled water with
out interrupting the current. The tared anode is dried and weighed.
The weight o f lead peroxide found by difference multiplied by 0.8661
gives the percent o f lead.
(8) Granulation,.— A weighed portion o f 50 grains o f the sample
is placed on a No. 14 U. S. standard sieve to which a bottom pan has
been attached. Two metal washers are placed on the sieve and shaken
for a maximum o f 3 minutes or until no more material passes through
the sieve. A ny material remaining on the sieve is weighed and the
percentage passing through the sieve calculated.
61. S tora g e.— Rules governing storage o f dry picric acid are the
same as for TN T. Dimension o f magazines should not exceed 42 by
26 feet. It is necessary that all dust accumulating from dry picric
acid should be carefully removed from any point in or around the
buildings, conveyors, or cars. Although dust originating from this
source is not as dangerous as that from black powder, it is nevertheless
a matter o f record that serious explosions have been caused from this
source. Safety shoes must be worn in every instance where picric
acid is being handled.
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S ection V
NITKOSTARCH E X P L O SIV E S
Paragraph
General------------------------------------------------------------------------------------------------ 02
Manufacture----------------------------------------------------------------------------------------- 63
Properties__________________ 04
Use------------------------------ ------------------------------ — _____________________ __ 65
Storage------------------------------------------------------------------------------------------------ 60
Inspection________ 67
62. General.— a. During the World War certain explosives having

nitrostarch as a base were used under the designations “Trojan grenade
explosive,” “ Trojan trench mortar shelL explosive,” and “ Grenite.”
These explosives were, frequently referred to as “nitrostarch,” hut it
should be noted that pure nitrostarch was not used alone as a military
explosive, the nearest approach to it for military purposes being
grenite, which was about 95 percent nitrostarch, the balance being a
binding material added for the purpose o f granulating. The two
Trojan explosives which were practically identical in composition
contained approximately 25 percent nitrostarch with ammonium ni
trate, sodium nitrate, and small amounts of materials added for the
purpose o f stabilizing, reducing sensitiveness and hygroscopicity, and
neutralizing any possible acidity of other ingredients.
h. These nitrostarch explosives were used for the reason that at the
time the United States entered the war a decided shortage o f T X T was
indicated and investigation showed nitrostarch explosives to be en
tirely suitable for trench warfare purposes and to offer the advan
tages o f low7cost and ample supply of raw materials, etc.
63. M anu facture.— a. Process.— (1) /Starch conversion.— Nilro-
slurcli is prepared by treating starch with a mixture of nitric and sul
phuric acids. It can be prepared from any variety o f starch, but it is
claimed that a cassava or tapioca starch gives a slightly more stable
product than cornstarch. The starch is first freed from impurities
such as fats, oils, and water-soluble matter, then carefully dried at
low temperatures, and screened. It is fed slowly into the acid mix
ture in a nitrator provided with suitable agitation and cooling sur
face. This treatment converts the starch into starch nitrate (com
monly but incorrectly referred to as nitrostarch), without any change
in appearance, but with a decided change in chemical properties.
(2) Starch nitrate treatment.—The nitrated product is separated
from the excess of spent nitrating acid, drowned in water, washed
thoroughly to remove all traces of free acid, then separated from the
water in filters or centrifugal wringers, and finally spread on trays to
TM 9-2900
6 3 -6 4 M IL IT A R Y E X P L O SIV E S
dry in suitable dry houses heated with air at a temperature of 35°

to 40° C.
b. Drying .—The drying operation, especially handling the warm,
dry product, is the only really dangerous operation connected with
manufacture, the dry nitrostarch being highly inflammable, capable
o f being ignited by the slightest spark such as might result from a
static charge and when once ignited, burning with explosive violence.
c. Mixing .—Mixing dry nitrostarch with the “ dope” materials,
as the inert ingredients o f such explosive mixtures are frequently
called, is a simple operation carried out in large revolving mixing
barrels. All o f the dope materials must first be ground to the proper
degree o f fineness and dried to the proper moisture content so that
the moisture content o f the finished explosive will not be in excess
o f the prescribed amount. Granular nitrostarch explosives such as
Grenite are usually prepared by spraying the dry material with a
solution o f the binding material while the mixture is being agitated
in a revolving mixer. The resulting granules are dried and screened
to proper size.
64. P rop erties.— a. Color and solubility.— (1) Nitrostarch.— Ni
trostarch is a white, finely divided material similar in appearance
to ordinary powdered starch. When observed under the microscope
there is no appreciable difference between nitrated and unnitrated
starch until the granules are treated with iodine which colors the
unnitrated starch blue but does not affect the nitrated product.
Nitrostarch is insoluble in water and does not gelatinize or form a
paste when heated with water, thereby differing from starch. The
grade o f nitrostarch ordinarily employed contains from 12.50 to
12.75 percent nitrogen; that prescribed for military purposes con
tains at least 12.80 percent. All nitrostarch is readily soluble in
acetone, solubility in ether-alcohol in general increasing as the nitro
gen content decreases. It has no great tendency to absorb moisture
from the atmosphere beyond the amount of 1 to 2 percent.
(2) Trojan explosive.—Trojan grenade or trench mortar shell ex
plosive differed greatly in appearance and in certain o f its properties
from straight nitrostarch, being o f grayish-black color and o f about
the consistency o f ordinary brown sugar, having a slightly damp
feel and tendency to pack under compression due to the small amount
o f mineral oil contained as an ingredient. This oil, besides decreas
ing the sensitiveness o f the explosive to ignition and to shock or
friction, helped to reduce its attraction for moisture, the mixture o f
ammonium nitrate and sodium nitrate which it contained being very
hygroscopic. In spite of this coating of oil the Trojan explosive
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TM 9 -2 9 0 0
when spread out in a thin layer in a damp atmosphere rapidly ab

sorbed moisture to such extent that it became decidedly wet. Under
ordinary working conditions therefore great care was taken in loading
this explosive to avoid absorption of an undesirable amount of
moisture.
(3) Granite.—Grenite, which was almost entirely pure nitrostarch
with addition of a small amount o f oil and a binding material, differed
greatly in appearance from Trojan explosive, being in the form o f
small, white, hard granules which flowed freely without sticking to
gether. Since it contained no ammonium nitrate or other hygroscopic
materials, Grenite had no particular tendency to absorb moisture
even in damp atmospheres.
h. Sensitivity.— (1) Pure dry nitrostarch is more sensitive to impact
than TN T but less sensitive than dry guncotton or nitroglycerin.
As mentioned above, it is highly inflammable and readily ignited by
the slightest spark Such as may result from friction, and like black
powder bums with explosive violence. It is readily detonated by
by a mercury fulminate detonator.
(2) Trojan explosive and Grenite were both much less sensitive than
straight nitrostarch, being required to pass the pendulum friction
test o f the United States Bureau o f Mines and the rifle bullet test
when packed in pasteboard containers. In heavy metal containers
these explosives frequently ignited and burned when penetrated by a
rifle bullet, and in rare instances exploded under this test. Trojan
explosive was especially insensitive to ignition, being rather difficult to
ignite with the flame o f a match when spread out imcontined. When
once ignited, however, especially in any quantity, it burned freely with
a light-colored smoke.
c. Detonation.— Nitrostarch explosives were readily detonated by
mercury fulminate detonators, a No. 6 detonator containing 1 gram
of fulminate composition, producing complete detonation unless the
explosive had been rendered unduly insensitive by absorption of ex
cessive moisture or by other cause.
d. Stability.—Early attempts to manufacture nitrostarch resulted
in production o f material which was unstable, and numerous state
ments found in literature of explosives refer to nitrostarch as
being unsatisfactory for use as an explosive because o f sensitivity
and instability. However, manufacturers in this country succeeded
in placing on the market nitrostarch explosives which proved highly
satisfactory in thesei respects and found considerable application
as blasting explosives. Developments led to a product which met
requirements prescribed for military explosives. However, the Tro-
TM 9-2900
jan explosive if allowed to absorb undue quantities o f moisture, es

pecially in a warm atmosphere, tended to deteriorate, being quite
similar to nitrocellulose in this respect.
65. U se.— a. Trojan explosive.-—The Trojan nitrostarch explosive
was used as the bursting charge for hand grenades, rifle grenades, and
trench mortar shell. It was well adapted to such purposes but was not
considered for use as a bursting charge for high-explosive gun shell.
Its physical consistency was such that it was loaded into grenades
through the small filling hole by means o f vibrating machines, the
explosive being “ jarred” into the grenade through small funnel open
ings. Trench mortar shell were loaded by hand-stemming.
b. Grenite.—Grenite was used only fo r grenades and was considered
too sensitive for use as a trench mortar shell explosive. Being granu
lar and “ free-running” it was readily loaded into the grenades through
funnel openings, no attempt being made to pack it to a high density.
c. Nitrostarch.— (1) Nitrostarch has been considered for the manu
facture o f smokeless propellent powder and numerous attempts have
been made to develop a satisfactory powder o f this type, but the
problem cannot as yet be considered solved.
(2) Nitrostarch explosives similar to Trojan grenade explosive
have been used for a considerable number o f years as blasting explo
sives for use in mining, quarrying, and other engineering operations,
and have met with considerable success as substitutes for the more
expensive nitroglycerin explosives.
(3) There has recently been adopted, after thorough investigation,
a nitrostarch demolition explosive as a substitute for TN T. This
explosive is somewhat similar to that used during the W orld W ar
but the formula has been modified by raising the nitrostarch content
and the replacement o f the ammonium nitrate with barium nitrate.
It can be consolidated into blocks in the same manner as T N T , and
in comparison tests it has been found that the T N T formula for
computing small charges are directly applicable to the nitrostarch
demolition explosive.
66. Storage.— Storage o f nitrostarch explosives in general is
mainly a fire risk, that is, the danger accompanying storage is more
one o f fire than o f explosion. However, burning may proceed at
such rate as to be almost explosive in nature, and the fact that nitro
starch can be exploded by impact should not be overlooked.
a. Magazines.— Magazines should be kept at as low temperatures
as possible in order to avoid as much as possible the tendency o f
nitrostarch to undergo decomposition on heating. A reasonably dry
atmosphere in magazines is also essential for the Trojan explosive.
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TM 9-2900
This explosive was not suitable for storage in bulk in wooden con
tainers because o f its hygroscopicity. Even when loaded into gren
ades it- tended to absorb moisture. Long contact of the explosive
with the metal parts of the grenade, either iron, brass, or copper,
resulted in corrosion.
b. Handling.—There is no danger of poisoning of any kind con
nected with the handling o f nitrostarch explosives.
67. In sp ection .— a. Specifications.— (1) The chemical composi
tion o f Trojan explosive as used was as follows:
No', loss than— Not more than—
P ercent P ercent
Nitrostarch___ ___ ____ __ _____ _ 23. 0 27. 0
Ammonium nitrate.____ 31. 0 35. 0
Sodium nitrate___ __ ____________________________ 36. 0 40. 0
Charcoal ... __ 1. 5 2. 5
Heavy hydrocarlxms----- --------------- . . — .5 1. 5
Antiacid . ______ . . . . _________ ___ .5 1. 5
Diphenvlamine . ______ ________ __________ . .2 .4
Moisture . . __ ____ _________ ___________ . . 1. 2
(2) T h e ch e m ica l c o m p o s itio n o f g ren ite is p rescrib ed as follow s:
Not I<‘s-<than— Not mure than—
P ercen t P ercen t
Nitrostarch.. ___________- _____________________ 95. 5 98. 25
Petroleum oil________ ____ ____ . . ---- ------- . 75 2. 00
Gum arabic. __ — ------------- -------- . 75 2. 00
Moisture ___ __ ________________ 1. 00
b. Tests.— (1) Trojan explosive— The following methods for an

alysis o f Trojan explosive were prescribed:
(a) Moisture.— Approximately 5 grains of the sample, accurately
weighed out, are spread evenly on a 90-mm. watch glass ( 3 ^ -inch
diameter) and placed in a desiccator over concentrated sulphuric acid.
Loss in weight after 48 hours is taken as moisture. As an alternative
method, a vacuum desiccator may be used with sulphuric acid (sp.
gr. 1.84) as a desiccating agent and employing a vacuum of at least
700 mm. o f mercury. A fter 24 hours the vacuum is slowly relieved
and the loss in weight taken as moisture.
(b) Ether extract.—Approximately 10 grams o f the sample are
accurately weighed out and placed in a porous crucible (Gooch cru
cible. with thin asbestos mat, or an alundum filtering crucible) and
extracted with pure petroleum ether o f 0.040 to 0.000 specific gravity.
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T M 9 -2 9 0 0
After complete extraction the crucible and contents are dried by

means o f a stream o f dry air until complete removal o f the petroleum
ether, after which the crucible is placed in a steam oven and dried to
constant weight at approximately 70° C. The difference in weight
between the original weight o f the sample after deducting weight of
moisture and the weight after extraction is taken as the heavy hy
drocarbon oil present, together with the diphenylamine. The di-
phenylamine in this mixture may be determined by means o f the
Dumas method for determining nitrogen.
( a) Water extract.— The material in the crucible after removal o f
the heavy oil consists o f nitrostarch, ammonium nitrate, sodium ni
trate, charcoal, and sodium bicarbonate. By treatment with warm
distilled water the ammonium nitrate, sodium nitrate, and sodium
bicarbonate are removed, and the material in the crucible after dry
ing at 80° C. for several hours consists o f nitrostarch and charcoal.
The loss in weight in the water extraction is determined and also the
weight o f the crucible plus nitrostarch and charcoal. These two fac
tors are then used in the subsequent calculations.
(d) Sodium bicarbonate.— The water extract is made up to a fixed
volume. One portion is taken for the determination o f the sodium
bicarbonate present. This is determined by titration with N /10 sul
phuric acid, using methyl orange as an indicator and the alkalinity so
found is calculated to sodium bicarbonate.
( e ) Ammonium nitrate.— A t the option o f the inspector, the per
centage o f ammonium nitrate is determined by taking an aliquot por
tion o f the water extract, adding caustic soda until the solution is
strongly alkaline, and then distilling in an apparatus as used for
ammonia determinations and collecting the distillate in a known vol
ume o f standard sulphuric acid. The excess acid is titrated with
standard alkali, methyl orange being used as an indicator, and the
result, is then calculated to ammonium nitrate.
( / ) Sodium nitrate.— An aliquot part o f the water extract, is acidi
fied with nitric acid and the solution evaporated to dryness in a
platinum dish. It is then ignited at a low red heat over a suitable
flame, using care to avoid loss o f the contents. The weight is then
taken and a correction made for the amount o f sodium bicarbonate
present and the results regarded as sodium nitrate present. Follow
ing this procedure, the ammonium nitrate would be taken by differ
ence in order to avoid the determination o f ammonia.
(g) Charcoal.— The residue in the crucible after the water extrac
tion consists o f nitrostarch and charcoal. This material is best
extracted in a. W iley extractor with warm acetone until no further
T M 9 -2 90 0
soluble material is obtained. The crucible is then dried in a stream

o f dry air and further dried for several hours at 100° C. The weight
of the charcoal is taken as the increase in weight of the crucible over
its original weight empty.
(k) Nitrostarch.—The difference between the sum o f nitrostarch
and charcoal content as determined in ( c) above and the percentage of
charcoal as found by (</) above represents the nitrostarch present.
(2) Grenite.— Analysis o f Grenite is carried out in a similar man
ner, the ether extraction removing the oil, the water extraction dis
solving the gum arabic and leaving the nitrostarch.
S ection VI
TETKYL
PiirnKrnph
General------------------- _____ 6S
Manufacture____ __ 6 9
Proper! ics---------------- ______ 70
U se__________________ ______ 71
Storage and handling ______ 72
Inspection___________ ---------- 73
68. General.— The high explosive commonly known as tetryl is

trinitrophenylmethylnitramine. It is a derivative o f benzene and
is therefore in the same class of aromatic uitro compounds as TNT.
Tetryl was first synthesized by Mertens in 1877. It did not acquire
prominence as a military explosive until the W orld War when it
was used as a booster explosive.
69. M a n u factu re.— a. Although the explosive manufacturer
starts with dimethylaniline as bis raw material, the entire process
beginning with benzene is as follows: Benzene is nitrated to nitro
benzene by means of a mixture o f nitric and sulphuric acids and the
resulting nitrobenzene reduced with iron filings and hydrochloric
(muriatic) acid to aniline. Aniline is then combined with methyl
alcohol (wood alcohol) bv heating these ingredients under pressure
in the presence o f sulphuric acid or iodine, yielding dimethylaniline.
b. The dimethylaniline is an oily liquid o f slightly lower specific
gravity than water. Prior to nitrating it is dissolved in a large ex
cess o f approximately 96 percent sulphuric acid because if treated
direct with mixed acid a very violent reaction results. This solu
tion in sulphuric acid is now added to nitric acid or a mixture of
nitric and sulphuric acids in a nitrator provided with means for
cooling and agitation. The temperature o f nitration is approxi
mately 68° to 72° C.
I ll
TM 9-2900
69-71 M IL IT A R Y EXPLOSIVES
c. The. tetryl is separated from the acid mixture by filtration or

by drowning in water and decanting the sour water. The tetryl is
given short boiling treatments to reduce the total acidity to 0.5 per
cent or less. The excess water is removed by filtration and the crude
tetryl thus obtained is purified by recrystallization from benzene,
acetone, or nitric acid. In recrystallization conditions are so con
trolled that granulation o f the finished product makes it free-flowing.
This free-flowing property is required so as to allow the manufacture
o f tetryl pellets in automatic pelleting presses.
70. P rop erties.— a. Chemical and physical.—Tetryl is a fine crys
talline powder o f a yellow color, practically insoluble in water but
soluble in acetone, benzene, and other solvents. It is readily re
crystallized and can therefore be obtained in very pure condition
if desired. It melts when pure between 129° and 130° C. Tetryl
is poisonous when taken internally and precaution is necessary in its
manufacture, especially regarding the dust encountered in handling
and packing the dry material. It has a higher nitrogen content
(24.4 percent) than any other military explosive. Tetryl is prac
tically nonhygroscopic, absorbing less than 0.1 percent moisture
when stored for several days in a saturated atmosphere.
b. Stability and sensit/oiiy.—Tetryl is stable at all temperatures
which may be encountered in storage. When heated above its melt
ing point it undergoes gradual decomposition and explodes when
exposed to a temperature o f 260° C. for 5 seconds. It is more sensi
tive to shock or friction than TN T, being o f about the same order
of sensitivity as picric acid. It is slightly more sensitive to detona
tion by means o f mercury fulminate than TNT, and is readily
exploded by penetration of a rifle bullet.
c. Detonation.— Tetryl has been found to have a rate of detonation
somewhat higher than the maximum rate obtained with TN T (7,000
meters per second). Strength tests such as the Trauzl lead block
test show tetryl to be stronger than any other military high explo
sive, the average expansion produced in the lead block for the more
common military high explosives being as follows:
Tetryl, 320 cubic centimeters.
Picric acid, 300 cubic centimeters.
TN T, 260 cubic centimeters.
71. U se.— a. Charges.— (1) The high explosive strength and bri-
sance o f tetryl would seem to adapt it for use as a bursting charge,
but its sensitivity to mechanical shock is such that if used as a shell
filler it would not withstand shock o f discharge o f the gun. It is,
however, sufficiently insensitive that when compressed into a booster
112
TM 9-2900
it is perfectly safe. In this condition it is readily detonated by (he

detonator in the fuze of the shell, and the violence of its detonation
insures a high order of detonation o f the bursting charge.
(2) Tclryl has been adopted as a booster explosive. Formerly it.
was combined with TNT (grade 1), the two explosives being usually
loaded separately into the booster casing in the form of highly
compressed pellets.
b. Detonator.—It is also used in detonators for both military and
commercial purposes as a base charge, the tetryl being pressed into
the bottom of the detonator shell and then covered with a small
priming charge o f mercury fulminate, lead azide, or other initiator.
72. Storage and h a n d lin g .— The same precautions should be
observed in storage and handling o f tetryl as in the case o f other
sensitive high explosives. It. should be kept dry because moisture
interferes with its effectiveness. It must be properly protected from
bullet fire in brick or hollow tile magazines with iron door’s and
window shutters. Detonators, blasting caps, fuzes, dynamite, etc.,
must not be stored with tetryl. Rubber-soled shoes should be worn
in magazines and every precaution taken to prevent ignition or
explosion from friction or blows due to rough handling.
73. In sp ection .— a. Specifications.—U. S. Army Specifications
require that tetryl will have—
(1) Melting point, not less than 128.5° C.
(2) Acidity, not more than 0.05 percent.
(3) Insoluble in benzene, not more than 0.20 percent.
(4) Moisture, not more than 0.10 percent.
(5) Color, light yellow' or buff.
(6) Granulation:
(a) Through No. 12 U. S. standard sieve, 100 percent minimum.
( b) Through No. 16 U. S. standard sieve, 95 percent minimum.
(c) Through No. 100 U. S. standard sieve, 20 percent maximum.
(7) Sand test: 0.4 gram o f tetryl primed with 0.24 gram mercury
fulminate will crush not less than 45 grams standard Ottawa sand to
pass a 30-mesh sieve on each of five trials.
b. Tests.— Prescribed methods of testing tetryl for acceptance are
as follow s:
(1) Melting point.—A portion o f about 5 grams of the tetryl is
ground in a mortar to pass a 100-mesh screen and this finely ground
material used for the test after drying for 2 hours at 100° C. or in a
sulphuric acid desiccator for 48 hours. The capillary tubes used must
be of 'uniform external diameter o f about 0.30 mm. to 0.80 mm. with
light walls, and long enough to extend out of the bath of liquid used
240541° 113
T M 9 -2 9 0 0
for heating. The thermometer must lie accurately standardized and

the mercury column completely immersed at the temperature o f the
observed melting point, or accurate corrections for emergent stem
applied. The capillary tube is filled to a depth o f 3-4 mm. with the
sample, compacted by tapping, and fastened to the thermometer with
its bottom end in contact with the bulb o f the thermometer. The
thermometer is then suspended in the bath with its bulb at least V/2
inches from the bottom of the bath. The bath being provided with
efficient agitation, its temperature is raised rapidly to about 120° C.
and then very gradually so that the rise in temperature is about 1°
in 5 minutes. The point taken as the melting point is the temperature
which is observed at the instant that the first meniscus o f melted ma
terial appears across the capillary tube.
(2) Insoluble matter.— A known weight, approximately 5 grams,
o f the sample is dissolved in 75 cc. of benzene by heating to about
75° C. and filtered through a tared Gooch crucible, The residue in
the crucible is washed with 25 cc. o f benzene, dried to constant weight
at 100° C., and weighed.
(3) Acidity .— A weighed portion of approximately 5 grams of the
sample is dissolved in 150 cc. o f benzene. The solution is transferred
to a separatory funnel and shaken with 100 cc. o f cold, recently boiled,
distilled water. The liquids are allowed to separate, the water drawn
off, and the benzene solution washed with another 50 cc. o f cold boiled
water. The combined water washes are titrated with approximately
0.1N sodium hydroxide solution, using phenolphthalein as indicator.
The acidity is calculated as percentage o f sulphuric acid.
(4) Moisture.—A sample o f about 5 grams o f the tetryl is ac
curately weighed in a previously tared wide-mouthed weighing bottle
at least l 1/? inches in diameter, and dried for 2 hours in a drying oven
at 100° C. or in a desiccator over sulphuric acid for 48 horn's. The
loss of weight is calculated as percentage o f moisture in the original
sample.
(5) tim id test.— (a) Loading the five caps.— 0.4 gram of tetryl
weighed to the nearest milligram is placed in the empty shell of a
commercial No. 6 blasting cap (composed o f copper or gilding metal,
and 1.46 inches long by 0.217-inch inside diameter) which is held
in a loading block. A plunger 0.20 inch in diameter is inserted in the
shell and a pressure o f approximately 3,000 pounds per square inch
applied to the tetryl for 3 minutes. 0.24 gram o f mercury fulminate
weighed to the nearest milligram is placed in the shell and covered
with a reinforcing cap (having a diameter o f approximately 0.217
inch at the lower end and a hole o f 0.11 ±0.03-inch diameter in the
114
TM 9-2900
top). The same pressure o f approximately 3,000 pounds per square

inch is applied for 1 minute.
The powder train in one end o f a piece o f miner’s fuse 8 or 9
inches long is pricked with a pin, and a loaded cap crimped on to
this pricked end of the fuse. Care should he taken to crimp near
the mouth o f the cap in order to avoid the danger of squeezing the
fulminate. The cap should he held away from the body when the
crimp is being made.
(b) Method.— 80 grams±0.1 gram of standard Ottawa sand
which have been previously sieved through a No. 20 U. S. standard
screen and retained on a No. 30 U. S. standard screen are poured into
the cavity o f the sand test bomb and leveled by striking the bomb
two or three times. The fuse is inserted through the hole in tire
cover o f the bomb, and the cap lowered into the bomb cavity until
the bottom touches the sand. One hundred and twenty grams±0.1
gram more o f the sand (making a total o f 200 grams) are then
poured around the cap and the bomb tapped as before.
To avoid possible loss o f sand caused by the explosion blowing
the burned fuse out of the hole in the cover, a piece of rubber tubing
about % inch long and o f such inner diameter that it fits the fuse
snugly is slipped over the fuse and adjusted at a point on the fuse in
such a manner that when the detonator is in position the rubber will
be against the inner side o f the bomb cover. The cover is then se
curely fastened to the bomb, taking care not to displace the cap in
the sand. The fuse is lighted and after the explosion has taken
place the sand is emptied onto a smooth (glazed) piece of paper, care
being taken to remove completely any sand adhering to the sides
of the bomb or to pieces o f the detonator, shell, or burnt fuse. All
of the sand is emptied onto the No. 30 U. S. standard sieve, and the
amount which passes through after shaking for 3 minutes is weighed.
S ection V II
M ERCU RY FU LM IN ATE
P u raK raph
General__________________________________________________________________ 74
Manufacture_______________________________________________________________75
Properties_______________________________________________________________ 76
Use------------------------------------------------ 77
Storage----------------------------- 78
Inspection_______________________________________________________________ 79
74. General.— Mercury fulminate is one of the explosives used for

bringing about detonation o f high explosives. It detonates com-
115
TM 9-2900
pletely and with great violence on ignition by means of a flame such

as the spit from a fuse or by means o f an electrically heated wire.
This fact, together with its property o f initiating detonation o f other
explosives, makes it a most suitable detonator material.
75. M a n u fa ctu re .— a. Materials.— Mercury fulminate is pre
pared, generally on a relatively small scale by the action o f alcohol
on mercury nitrate in nitric acid solution. The raw materials re
quired are metallic mercury, nitric acid, and ethyl alcohol (common
grain alcohol o f 95 percent strength). All of these materials must
be o f high purity in order to produce a satisfactory product.
b. Process.— Process o f manufacture is quite simple and may be
carried out as follow s:
(1) About 1 pound o f pure mercury is weighed carefully, added to a
weighed charge o f from 8 to 10 pounds of strong nitric acid in a
suitable bottle or acid pitcher, and allowed to stand until completely
dissolved, giving a solution o f mercury nitrate in the excess o f nitric
acid. A large number o f such charges are usually prepared and
allowed to stand over night until dissolved.
(2) The acid solution o f mercury is then poured into about 8 to
10 pounds o f 95 percent alcohol which has previously been measured
into a large thin glass flask or balloon o f about 10-gallon capacity
supported in a suitable rack under an open shed or in the open air.
A violent reaction results, usually within 2 or 8 minutes, the mixture
in the balloons appearing to be boiling violently as a result o f the
evolution o f great quantities o f vapors and fumes. These vapors,
at first white, become brownish red hi color toward the end o f the
reaction as the heat generated drives off nitric acid. A t this point
a small amount o f dilute alcohol is usually added to prevent exces
sive heating which would decompose the mercury fulminate pro
duced. The reaction usually lasts about 1 hour. When fuming
ceases, the liquid remaining in the balloon is found to contain the
crystalline fulminate. In most plants the balloons are placed in
troughs o f water in order to control the temperature, and the necks
o f the balloons are connected with a suitable condenser system where
the alcohol driven off in the fumes is recovered.
(3) A fter cooling, the charge in the balloons is dumped onto a
cloth screen and washed with cold running water until all free acid
is removed and the fine impurities in the form o f “ fulminate mud”
washed away. The washed fulminate is then drained and packed
in cloth bags which are usually stored in crocks o f water in vaults,
or in underground concrete tanks o f water until required for use.
For shipment the bags are packed in barrels of wet sawdust. 'When
required for use, the fulminate is removed from the bags, the water
116
TM 9-2900
drained, off, and the wet fulminate spread on cloth to dry in dry-
houses carefully regulated at a temperature of about 43° C. (110° F.).
1 pound of mercury produces approximately ld/j pounds of dry
mercury fulminate.
76. Properties.— a. Color and solubility.—Mercury fulminate is a
heavy, crystalline solid, white when pure, but ordinarily of a faint
brownish yellow or grayish tint. It has practically no tendency to
absorb moisture from the atmosphere. It is only slightly soluble in
water, 100 parts of water at 15.5° C. (60° F.) dissolving less than
0.01 part of fulminate, and may be kept in contact with water for
long periods o f time without undergoing change.
b. Size of crystals.—Size o f the crystals o f mercury fulminate is
an important factor, since it has been determined that very finely
divided fulminate consisting mostly of fragments o f crystals and
usually containing an excessive amount o f impurities is less ofiicient
in detonating value and strength than larger crystals. In specify
ing the size o f crystals desired, however, consideration has been given
to the possibilities of controlling this feature in manufacture and
also to the fact that there is some reason to believe that very large
crystals o f fulminate are more sensitive to friction or shock than
smaller ones. As indicated below, U. S. Army specifications for
mercury fulminate prescribe definite limits for the size of the crystals.
c. Impurities.—Mercury fulminate is required by U. S. Army
specifications to be at least 98 percent pure and the amounts of
impurities which it may contain are strictly limited. The most
objectionable impurities are—•
(1) Free metallic mercury, for the reason that it readily attacks
copper or brass with which it may be in contact when loaded into
fuzes, detonators, or primers, causing the metal to become brittle.
(2) Acidity, which would cause deterioration of the explosive
composition and corrosion of metal parts.
(3) Insoluble material such as sand and grit, which might cause
explosion of the dry fulminate in loading operations.
I f improperly manufactured or incompletely washed, the fulminate
may also contain various compounds of mercury which might pro
duce decomposition and would certainly diminish explosive efficiency.
d. Stability.— (1) Mercury fulminate has been kept for long pe
riods both dry and wet, and is believed to undergo practically no
change when properly manufactured and stored. However, when
stored either wet or dry at tropical temperature gradual deteriora
tion takes place. It has been found that when stored at 35° C.
(95° F.) mercury fulminate deteriorated to the point o f malfunc-
T M 9 -2 9 0 0
tioning in about 3 years and at 50° C. (122° F .) it deteriorated

to practically the same degree in 10 months. It is never stored in
quantity in dry condition except when loaded into detonators, fuzes,
or primers fo r the reason that when dry it is readily detonated by
friction or shock. Whereas the great m ajority o f high explosives
will burn without detonating when ignited by a flame especially if
a relatively small amount o f the explosive is ignited, mercury fu l
minate is one o f the so-called “ primary” or “ initiating” explosives
which detonate completely on being heated to their ignition point
by means o f a flame or hot wire.
(2) The presence o f even small amounts o f moisture in mercury
fulminate greatly reduces its efficiency, and as little as 1 percent is
said to cause failure to detonate. However, fulminate completely
saturated with water may be detonated by detonation o f dry fu l
minate in contact with it.
e. Sensitivity.— (1) By usual methods o f determining ignition
temperature, mercury fulminate detonates at a temperature o f about
180° C. (about 356° F .), but under varying conditions detonation
may result at much lower temperatures. Sensitivity to shock is
much greater at elevated temperatures than under storage conditions.
(2) When loaded into commercial detonators, mercury fulminate
is usually compressed at pressures o f about 3,000 pounds per square-
inch. In this condition its explosive properties are not appreciably
different from those o f loosely compressed material. A t greater
densities obtained by higher pressures, there is a gradual reduction
in sensitivity, until at such extreme pressures as 25,000 to 30,000
pounds per square inch fulminate entirely loses its property o f deto
nating when ignited and will only burn. In this condition it is
referred to as “ dead pressed.” If, however, such highly pressed ful
minate is initiated by loose fulminate or other initial detonating
agent, it will detonate at even higher rates than are obtainable at
low densities.
(3) Although fulminate can be pressed under very high pressures
without explosion, the presence o f any particles o f sand or grit is
very dangerous in any pressing operation. Presses for loading are
always carefully protected by heavy barricades, and no one is per
mitted to be near the press during operation.
(4) The readiness with which dry mercury fulminate detonates
from the effect o f blows or friction is the chief reason for the fact that
its transportation and storage in the dry state is not permitted. Tests
with a special type o f impact machine showed that mercury fulminate
118
TM 9-2900
detonated from the blow o f the falling weight dropped from a height
o f only 2 centimeters (about 0.8 inch), while TN T in the same ap
paratus required a drop o f about 120 centimeters (48 inches).
f. Detonation.—For a number o f years mercury fulminate was con
sidered to have special properties which made it an especially favor
able initiating agent and numerous theories were advanced to account
for its so-called “ unique” properties. As a matter o f fact, mercury
fulminate has been used only because o f its extreme sensitivity to flame
or impact. In all other respects mercury fulminate is inferior to other
high explosives such as TN T, tetryl, and picric acid as a detonating
agent. For example, mercury fulminate has a rate of detonation o f
about 4,000 meters per second as compared with 6,800 meters per second
for TN T under the same conditions. In the Trau/.l lead block test,
mercury fulminate produces an expansion o f 213 cc. and TN T 260 cc.
The trend in military and commercial detonators for the past several
years has been gradual replacement of the major portion of the fulmi
nate charge with some high explosive to increase efficiency o f the
detonator, the fulminate being used only as a cover charge to initiate
detonation o f the high explosive forming the base charge in the
detonator.
77. U se.— Mercury fulminate is used only for the purpose of
bringing about the detonation o f other high explosives or the ignition
o f propellent explosives. In detonators fo r commercial or military
use it may be used alone or mixed with from 10 to 20 percent of
potassium chlorate. The usual grades o f detonators contain from 16
to 30 grains o f fulminate or its equivalent.
The ignition o f propellant, explosives, for example, smokeless or
black powder in small arms cartridges, is effected by the flame from
a primer or cap, the charge o f which is usually a composition con
taining mercury fulminate mixed with other flame-producing ma
terials such as potassium chlorate and antimony sulphide. The primer
is initiated by impact o f the firing pin.
78. Storage.— «. Mercury fulminate is always stored thoroughly
saturated with water.
b. When left in the barrels during storage, regular inspection must
be made to insure that the barrels are kept always full o f water and
are not leaking.
c. Fulminate must not be stored with any other explosives for the
reason that explosion of even a relatively small amount o f dry ful
minate may cause detonation o f the wet material, effect o f which
might be to detonate any other high explosives stored in the same
building.
119
TM 9-2900
d. In case o f breakage, or other cause by which wet fulminate may

be spilled on the floor, it must not be allowed to dry out before
cleaning up. Dry fulminate is very sensitive to friction and must
be handled with extreme care. Spilled fulminate may be destroyed
by washing floors, benches, etc., with a saturated solution of sodium
thiosulphate.
79. In sp e ctio n .— a. Specifications.— Chemical and physical re
quirements for mercury fulminate as prescribed by U. S. Arm y
specifications are—
(1) Fineness o f such a degree that not more than 15 percent by
weight, will be retained on a No. 100 U. S. standard screen, and that
not more than 75 percent will pass through a No. 200 IJ. S. standard
screen.
(2) Acidity, none.
(3) Material insoluble in sodium thiosulphate, not more than
2 percent.
(4) Free mercury, not more than 1 percent.
(5) Chlorine, not more than 0.05 percent.
(6) Mercury fulminate, not less than 98 percent.
(7) Sand test: Not more than 0.27 gram will be required to det
onate completely 0.4 gram o f T N T having a melting point o f at
least 80.5° C., and o f such granulation that it will completely pass
through a No. 80 U. S. standard screen.
b. Tests.— Methods prescribed for testing are as follow s:
(1) Giumilation.— A known weight, approximately 10 grams of
the dried fulminate obtained by drying at a temperature not exceed
ing 60° C. to constant weight, is added to water and transferred to
a 6-inch or some convenient size No. 100 U. S. standard sieve pro
vided with a brass pan, and thoroughly shaken fo r 10 minutes under
water. The residual fulminate is transferred from the No. 100 U. S.
standard sieve to a tared filter paper, washed twice with alcohol and
once with ether, and dried at 50° C. to constant weight. The fulm i
nate which passes through the 100-mesh sieve is washed on a No.
200 U. S. standard sieve, and -well shaken under water for 10 min
utes. The fulminate passing through the sieve is transferred to a
tared filter paper, washed twice with alcohol, once with ether, and
dried in the same manner as the fulminate which remains on the
100-mesh sieve.
(2) A cid ity .— A known weight, approximately 10 grams o f the
thoroughly dried material, is placed in a porcelain Gooch crucible
provided with a filter paper disc in place o f the customary asbestos
mat and washed with two successive 25-cc. portions o f boiled distilled
120
T M 9 -2 9 0 0
water, '['hofiltrate so obtained should show no red tinge upon the ad
dition o f three drops o f methyl orange solution prepared by dis
solving 1 gram o f methyl orange in water and making up to 1 liter.
(3) Insoluble matter.— A. known weight of mercury fulminate,
approximately 2 grams, is transferred to a 250-cc. beaker. One hun
dred and fifty cc. of freshly filtered 20 percent C. P. sodium thio
sulphate solution at room temperature is added and the solution stirred
for about 1 minute or until the mercury fulminate is apparently in
solution. It is then filtered at once through a fared Gooch crucible.
Any free mercury remaining in the beaker is completely washed into
the crucible with distilled water. The crucible is washed with three
or four 10-cc. portions o f cold water to free it from sodium thio
sulphate and dried at 70° C. to constant weight.
(4) Free mercury.— The residue in the Gooch crucible obtained
from the insoluble determination is treated with 60 cc. of a sodium
thiosulphate-potassium iodide solution containing 6 grams sodium
thiosulphate and 3 grams potassium iodide dissolved in water and
made up to 50 cc. The solution is decanted through the Gooch
crucible containing the insoluble material and the crucible thor
oughly washed with distilled water and dried at 80° to 90° C. for
2 hours and weighed. The residue remaining is taken as„the mercury
content and the percentage so determined.
(5) Chlorides.— A known weight, approximately 5 grams of the
thoroughly dried material, is placed in a porcelain Gooch crucible
having in its bottom a filter paper disk instead o f an asbestos mat
and washed with two successive 25-cc. portions of distilled water
having a temperature between 90° and 100° C. To the filtrate, which
is most conveniently caught in a test tube, three drops o f pure nitric
acid having a specific gravity of approximately 1.40, and 10 drops
of a 10-percent solution of silver nitrate are added. No greater
turbidity will appear than when a solution containing 0.0042 gram
o f pure sodium chloride dissolved in 50 cc. of distilled water is
treated exactly as the filtrate from the sample of fulminate. This
represents 0.05 percent o f chlorine.
(6) Mercury fulminate.— Exactly 0.3 gram of the thoroughly dried
material is placed in a wide-mouthed Erlenmeyer flask of approxi
mately 250-cc. capacity, containing approximately 50 cc. distilled
water. 30 cc. of a 20-percent sodium thiosulphate solution at room
temperature is added quickly and the mixture shaken for exactly
1 minute and then titrated with standard 0.1N HC1 solution, using
three drops o f methyl red as indicator.
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TM 9-2900
It is important that the titration begin exactly 1 minute after

addition o f the thiosulphate. The bulk o f the IIC1 should be added
immediately, and the total time o f titration should not exceed 1
minute. A blank determination should be run and the necessary
correction made. The calculation is as follow s:
T> , . , . . 0.711565 ( A - B ) O
Percent mercury fulminate.— - - A ---------
where A = c c . o f HC1 used.

B = cc. required for blank.
C =N orm ality factor for HC1.
D = W e ig h t o f sample taken.
(7) Sand test.— (a) Lauding the five raps.—0.4 gram TN T having
a melting point o f not less than 80.5° C. weighed to the nearest milli
gram is placed in the empty shell of a No. G blasting cap (composed
o f copper or gilding metal, 1.46 inches long by 0.211 inch inside
diameter) which is held in a loading block. A plunger 0.20 inch
in diameter is inserted in the shell and a pressure o f approximately
3,000 pounds per square inch is applied to the T N T for 3 minutes.
0.27 gram o f mercury fulminate weighed to the nearest milligram is
placed in the shell and covered with a reinforcement cap (having a
diameter o f approximately 0.217 inch at the lower end and a hole o f
0.11 ±0.03-inch diameter in the top). The same pressure of approxi
mately 3,000 pounds per square inch is applied for 3 minutes.
The powder train in one end of a piece of miner’s fuse 8 or 9 inches
long is pricked with a pin, and a loaded cap crimped on to this
pricked end of the fuse. Care should be taken to crimp near the
mouth of the cap in order to avoid danger o f squeezing the fulminate.
The cap should be held away from the body when the crimp is being
made.
(6) Method.— E ighty±0.1 grams o f standard Ottawa sand which
have been previously sieved through a No. 20 Bureau o f Standards
sand screen and retained on a No. 30 Bureau o f Standards sand
screen (opening 0.0223 inch, wire diameter 0.011 inch) are poured
into the cavity o f the sand test bomb and leveled by striking the bomb
two or three times (see fig. 29). The fuse is inserted through the hole
in the cover o f the bomb and the cap lowered into the bomb cavity
until the bottom touches the sand. 120 ±0.1 grams more o f the sand
(making a total of 200 grains) are then poured around the cap and
the bomb tapped as before.
To avoid possible loss o f sand caused by the explosion blowing
(he burned fuse out o f the hole of the cover, a piece of rubber tubing
TM 9-2900
F igure
t s fC^
1V * ;
¥ X-_-
V
9
k
I
SL
! \ \V x^w \N \
- 9-
123
TM 9-2900
about Yd inch long and o f such inner diameter that it fits the fuse
snugly is slipped over the fuse and adjusted at a point on the fuse in
such a manner that when the detonator is in position the rubber will
be against the inner side o f the bomb cover. The cover is then
securely fastened to the bomb, taking care not to displace the cap in
the sand. The fuse is lighted and after the explosion has taken
place the sand is emptied onto a smooth glazed piece of paper, caro
being taken to remove completely any sand adhering to the sides o f
the bomb, or to pieces o f the detonator or shell, or burnt fuse. All
o f the sand is emptied onto the No. 30 Bureau o f Standards sand
sieve and the amount which passes through after shaking for 2
minutes is weighed. The TN T is considered as having been com
pletely detonated if the average amount o f sand passing through the
30-mesh sieve in five trials is not less than 42 grams.
S ection V II I
AM ATOL
Paragraph
General____________ ... __________ _______ ________ ___________ 80
Properties---------------------------------------------------------------- 81
Manufacture-------------------------------------------------------------------------------------------- 82
Inspection----------------------------------- S3
80. G eneral.— Amatol is a mixture o f ammonium nitrate and

TNT. Due to the shortage o f toluene during the early stages o f the
W orld W ar, the British Government developed this explosive and
adopted it after exhaustive tests as a bursting charge for high-explo
sive shell. The United States Government shortly after its entrance
into the W orld War and for similar reasons authorized its use as
follow s: 50/50 for shell from 75 mm. up to and including 4.7 inches;
80/20 for shell from 4.7 inches up to and including 9.2 inches. The
ingredients are mixed by weight. The first figure refers to ammo
nium nitrate, the second to TNT.
81. P rop erties.— Amatol is hygroscopic, insensitive to friction,
but can be detonated by severe impact. It has no tendency to form
dangerous compounds with metals other than copper. It is more
insensitive to explosion by initiators than TNT. 50/50 amatol
lias approximately the same rate o f detonation and strength as TNT,
but 80/20 amatol is slightly lower in rate o f detonation and brisance.
On detonation the ammonium nitrate oxidizes the excess carbon o f the
TN T with the result that 80/20 amatol produces a white smoke on
detonation and 50/50 amatol a smoke less black than straight TNT.
T M 9 -2 9 0 0
82. M a n u fa ctu re.— a. $0/50 amatol.— The- ammonium nitrate as

received may contain some moisture and must be dried to a moisture
content o f not more than .25 percent. It may also be found that
caking has occurred in the barrels or drums in which it has been
shipped. To break up the lumps it is often necessary to first run the
material through a crusher, after which it is dried to the proper
moisture content. After drying, the material is screened to remove
any foreign material with which it may have become contaminated.
It is now ready for addition to molten TNT. The speed o f adding
ammonium nitrate to T N T can be increased greatly if the ammonium
nitrate can be added while it is still hot. It must be added at a rate
so that no solidification o f the molten TNT takes place in the melting
kettle. Proportions for use in mixing 50/50 amatol range from 45
percent to 55 percent ammonium nitrate. This variation is permitted
to take care o f the various granulations, fine material requiring more
TN T than coarse material. Temperature o f the mixture when it is
ready for pouring in the shell is 80° to 85° C.
b. 80/20 Amatol.— (1) 80/20 amatol is a plastic mass resembling
wet brown sugar and cannot be loaded by the casting method. The
principal difficulty experienced with 80/20 amatol is to obtain am
monium nitrate which has proper granulation. W ith very fine
material, plasticity o f the mass is such that when loaded density falls
below the point desired, namely, not less than 1.38. W ith coarse
material molten TNT is not completely absorbed and a relatively
large amount leaks out in the extruding operation which results in
a charge o f low density. It is therefore essential that granulation be
such as to give a mixture which will not permit leaking of TNT and
which will be sufficiently plastic to consolidate well from the extruder.
It has been found that, a mixture of coarse and fine material is the
most suitable for this operation. Granulation requirements are
through a No. 10 U. S. standard sieve not less than 99.0 percent;
through a No. 10 on No. 35, 32 to 48 percent; through a No. 100,
15 to 30 percent.
(2) Preparation of 80/20 amatol is conducted in a mixing kettle
having a capacity of about 500 pounds of amatol. The correct amount
o f ammonium nitrate is added to the kettle and heated to the point
where solidification o f T N T will not occur. When the ammonium
nitrate has been raised to at least 90° C., molten T N T is added and
the charge thoroughly mixed for 15 minutes. At the end o f this time
it is transferred to the extruding machine from which it is forced into
the shell by means of a screw working inside of a steel tube. This
125
TM 9-2900
machine is eounterweighted so that the material is forced into the

shell under a definite pressure.
83. In sp e ctio n .— a. Raw materials.— Ammonium nitrate and
T N T used in preparation o f amatol must conform to U. S. Army
specifications governing these materials, as impurities in both have
harmful effects on the resulting product. Oily impurities in the TN T
will cause exudation or leakage, while impurities in ammonium nitrate
such as pyridine, cyanide, etc., will cause formation o f gas or froth
ing, resulting in probable cavitation in the shell. Methods o f analysis
governing inspection o f these materials are given elsewhere in this
manual.
b. Samples.—Samples should be taken from the mixer while the.
stirrers are rotated as the T N T and ammonium nitrate have a tend
ency to segregate. It is desirable to take the sample in an aluminum
or thin sheet-iron vessel, a circular piece o f stout cardboard being
placed in the bottom. To obtain concordant results with duplicate
analyses, experience will show that extreme care must be taken with
the samples.
c. Tests.— (1) Moisture.— Dish and dome method: An aluminum
dish and dome (cover) is heated for 15 minutes, cooled in the desic
cator and weighed. Approximately 5 grams o f the sample is added
to the dish which is placed on the top o f a water oven for 3 hours.
A fter cooling in a desiccator for 20 minutes, the weight is taken. Loss
in weight equals moisture present in original sample. A small quan
tity o f T N T sublimes but condenses on the inside o f the cover which
should bo cleaned thoroughly before using in another test.
(2) TNT. — Extraction with benzene: A dry filter paper folded so
as to leave a small cavity in the center is weighed in a tared weighing
bottle. About 2 grams o f powdered amatol is placed in the filter
paper without removing it from the bottle and the bottle reweighed.
The paper and amatol are transferred to a small funnel and washed
with approximately 75 cc. hot benzene, adding enough at a time to
cover the powder. A fter about one-half o f the benzene has been added
the remainder can be poured in rapidly, taking care to wash thor
oughly the sides of the filter paper. The filter paper and residue are
transferred from the funnel to the top o f a steam oven in order to
remove the greater portion o f the benzene and dried in a tared weigh
ing bottle, for 1 hour. Loss in weight equals T N T plus moisture.
(3) Ammonkm.nitrate.— Extraction with water: A known weight,
approximately 2 grams, is extracted with 50 cc. hot water at a temper
ature not less than 85° C. A fter cooling, the solution is filtered and
the process repeated three times with 50 cc., 30 cc., and 20 cc. suc-
126
TM 9-2900
ccssive quantities o f liot water. The combined filtrates are evaporated

just to dryness in a tared dish and left in a vacuum desiccator over
night. The residue is rinsed two or three times with anhydrous ether,
dried on top o f the oven to remove ether vapors, cooled, and weighed.
The residue equals ammonium nitrate present in the sample.
S e c t io n IX
L E A D A ZID E
Paragraph
Gteneral---------------------------------------------------- 84
Properties______________________________________________________________ 85
Manufacture------------------------------ 86
8torage—- ----- 87
inspection— __________________ 88
84. G eneral.— Lead azide was first prepared and identified by
Curtius in 1891 and in 1893 W ill and Lenze began an investigation o f
lead azide as a military explosive. About 1910 commercial manu
facture o f lead azide was started abroad and has continued up to
the present time. Since 1931 it has been produced commercially in
this country. This commercial lead azide is free from needle crystals
having a maximum dimension greater than 0.1 nun.
85. P rop erties.—Lead azide (PbN„) is an initiating compound
used for bringing about detonation o f high explosives. It is sensitive
to flame but is too insensitive to be used alone where initiation is by
impact o f a firing pin. Lead azide is practically insoluble in water
and its hygroscopicity at 30° C. and 90 percent relative humidity is
only 0.03 percent. It is not easily decomposed by heat as shown by
surveillance tests where it has been stored for 15 months at 80° C.
without any noted impairment in sensitivity or brisancu.
86. M a n u fa ctu re.— a. Formulas.—Lead azide may be produced
according to tiro following reaction:
Fb (OOC.CH3), + 2NuN*= 2NaOOC.CJL + PbN0
Lead acetate Sodium azide Sodium acetate Lead azide
Pure sodium azide (NaNa) may be prepared by converting metallic

sodium to sodium amide in a current o f ammonia and then treating
the sodium amide with nitrous oxide:
NaNH2+ N o 0 = N a N s+ H 20
Sodamlde Nitrous Sodium Water
oxide azide
The water liberated reacts with one-half o f the X aN IL :

N aN IL + IL .O = N H 3+ NaOH
Ammouia Sodium 1)} droxide
127
TM 9-2900
8 6 -8 8 M ILITA R Y EXPLOSIVES
The reaction is completed when no more ammonia is evolved.

The mixture o f sodium azide and sodium hydroxide is separated by
recrystallization from water.
b. Method.— The conversion o f sodium azide to lead azide is carried
out in barricaded equipment. A method described by R. Wallbaum
is as follow s: A 5 percent lead acetate solution is placed in a suitable
reaction vessel at room temperature and a 2 percent solution o f sodium
azide added slowly, the contents o f the vessel being stirred constantly.
In order to avoid danger of handling pure lead azide it is customary
to prepare technical lead azide, 90 to 95 percent pure in granular
form. This is accomplished by adding dextrin to the lead solution
which produces a yellow-white product with no crystal faces observ
able under the microscope (5 0 X ).
87. Storag’e.—Lead azide is always stored thoroughly saturated
with water. It is stored and handled in the same manner as mercury
fulminate (see sec. V I I ). Spilled lead azide may be destroyed by
washing floors, benches, etc., with a solution o f ammonium acetate.
88. In sp e ctio n .— a. Specifications.—Requirements for lead azide
as prescribed in U. S. Army specifications are—
(1) Color, white to buff.
(2) Form, aggregates free from needle-shaped crystals having a
maxium dimension greater than 0.1 mm.
(3) Purity, lead content not less than 68.5 percent nor more than
71.15 percent.
(4) Acidity, none.
(5) Solubility, not more that 1.0 percent, in cold distilled water.
(6) Sand test: When 0.15 gram o f lead azide is used to initiate
0.40 gram o f tetryl, not less than 45 grams o f sand will be crushed.
(1) Golov.— Determined by visual inspection.
(2) Foi'm.—Determined by inspection under a microscope, using
a magnification o f 150. I f needle-shaped crystals are observed,
their maxium dimension is measured by means o f a measuring micro
scope.
(3) Purity.—The sample is dried in a steam oven at 95° C. An
accurately weighed portion o f approximately 1 gram o f the sample is
transferred to a 400-cc. beaker. 50 cc. o f a saturated solution o f am
monium acetate is added and the azide dissolved by stirring and warm
ing. The solution is diluted with 200 cc. o f distilled water and heated
to boiling. With rapid agitation 10 cc. o f a 10 percent solution o f
potassium dichronnite is added slowly. It is digested on a hot plate or
steam bath for 1 hour, with frequent stirring. The precipitate o f lead
128
T M 9 -2 9 0 0
chromate, is caught on a tared Gooch crucible, washed with Hot dis

tilled water, and the crucible and precipitate are dried for 2 hours at
100° C., cooled in a desiccator, and weighed. Weight of the precipitate
in terms of percentage o f lead in the sample is calculated:
PbCrO* X 0.64109=Pb
(4) Acidity .—An accurately weighed portion of approximately 10
grams o f the sample dried at 9.r>° C. is transferred to a tared Gooch
crucible. It in washed with five 20-cc. portions o f cold distilled water
which has been boiled prior to the test. Each portion o f water is al
lowed to remain in contact with the azide for 11 minutes. Five drops
o f methyl orange solution containing 1 gram o f methyl orange per
liter o f solution are added to the filtrate. Development o f a red tinge
indicates presence o f acidity.
(5) Solubility.— The crucible and azide from acidity determination
are dried to constant weight using a vacuum desiccator or a steam oven
having a temperature o f 95° C., weighed, and the loss in weight cal
culated in terms o f percentage solubility of the sample.
(6) Sand test.— (a) Loading caps.—To each of five empty No.
G blasting caps 0.400±0.001 gram o f tetryl complying with Specifica
tion No. 50-13-4 is transferred. Each blasting cap is composed of
copper, gilding metal, or aluminum, and approximately 1.4G inches
long by 0.217 inch inside diameter. With the cap held in a loading
block, a plunger 0.20 inch in diameter is inserted in the shell and
the tetryl subjected to a pressure o f 3.000 pounds per square inch (100
pounds actual load) for 3 minutes. The plunger is removed and
0.150±0.001 gram of dried azide sample is transferred to the shell.
'Fhe plunger is inserted in the shell and a pressure of 3,000 pounds per
square inch applied for 1 minute. The powder train in one end o f a
piece o f miner’s fuse 8 or 9 inches long is pricked with a pin. To the
pricked end, one of the caps loaded as directed above is crimped, taking
care that the end of the fuse is held firmly against the charge in the
cap. Crimping is done near the mouth o f the cap so as to avoid squeez
ing the charge.
( b) Method.— 80±0.1 grams of standard Ottawa sand which passes
through a No. 20 Bureau o f Standards sand sieve (opening, 0.0335
inch; wire diameter, 0.01G5 inch) and is retained on a No. 30 Bureau
o f Standards sand sieve (opening, 0.0223 inch; wire diameter, 0.0110
inch) are poured into the cavity o f the sand test bomb and it is leveled
by striking the bomb two or three times. The fuse is inserted through
the hole in the cover o f the bomb and the cap loAvered into the bomb
cavity so that it is in the center o f the cavity and just touching the
240.'41 °— 40-------o 129

T M 9 -2 9 0 0
sand. 120^0.1 grams more o f llic sand are poured around the cap and
bomb tapped as before to level the sand.
To avoid possible loss o f sand caused by the explosion blowing the
burned fuse through the hole in the cover, a piece o f rubber tubing
about inch long and o f such inner diameter that it fits the fuse
snugly is slipped over the fuse and adjusted at a point on the fuse so
that the rubber will be against the inner side o f the bomb cover when
the detonator is in position. The cover is fastened securely to the
bomb, taking care not to displace the cap in the sand. The fuze is
lighted and after the explosion has taken place, the sand is emptied
onto a sheet o f smooth glazed paper taking care to remove any sand
which may adhere to the side o f the bomb, or to pieces of the detonator
shell or burnt fuse. All the. sand is emptied on the Xo. .‘10 Bureau of
Standards sand sieve fitted with a pan, and the sand which passes
through the sieve after shaking 3 minutes is weighed.
130
C itapi-kr 3
BIBLIOGRAPHY
89. B ib liog ra p h y .
Berthelot, “Explosives and Their Power,” Translation. Hake and
Macnab, John Murray, London.
Buisson, “ Problems Des Poudres,” P. Juillard, Bui. Soc. Chem. 33,
1905, p. 117-2.
Escales, Richard. Dr., “ Die Explosivstoffe mist besondere bcruck-
sichtigung der Neuren Putente Bearbjtet von.”
Humphrey, Journal Industrial and Engineering Chemistry, vol 8,
November, 191G.
Journal o f Industrial and Engineering Chemistry, Analytical Edition,
vol. I, No. 1, 1929, p. 49.
Marshall, “ Explosives,” vol. 1, 1917, pp. 135-136, Blakistons & Co.
Official and Tentative Methods of Analyses of the Association of Offi
cial Agricultural Chemists, Second Edition, pp. 464-477.
Tschappat, “ Ordnance and Gunnery,” 1917, pp. 115, 518, J. Wiley &
Sons, N. Y.
131
'Elaah' Pa 6?
-fW 1 3 2
INDEX
Paragraphs Pages
Acid, picric.................... 56-61 99-104
Amatol........ .................. 80 124
Inspection................... 83 126
Manufacture____ __________ 82 125
Properties______________ 81 124
Ammonium picrate (explosive D i__________ 50 94
Inspection________________________ 54 96
Manufacture........ _................................_ . ............... .................... 52 95
Properties........... ................................................. ......................__ 51 94
Storage.............. 55 98
Use_______________________________________________________ 53 96
Bibliography.......... ............ 89 131
Cannon powders, FNH and N H __________ 17 34
Colloid, formation o f____ _____________________ _______________ 12 20
Cotton, raw, purification....... ........................ 9 6
Definitions______________ 1 1
DuPont nitrometer.......... ................................................................. . 29 61
Explosive D (ammonium picrate i-------- ------------------------------------- 50-55 94-99
Explosives:
A c t io n ............................................................................................ 3 3
Classification...................... 2 2
Composition______________________________________________ 5 4
Definition_________________________________________________ 1 1
High, military................................................................................ 40, 41 84
Nitrostarch_________________ 62-67 105-111
Use.......................... 4 3
Inspection of—
Amatol___________________________________________________ 83 126
Ammonium picrate (explosive D )__________________________ 54 96
Lead azide________________________________________________ 88 128
Mercury fulminate..................................................... 79 120
Nitrostarch explosives..................................................... 67 109
Picric acid------------------ 60 102
Powder:
Black.....................- .............................................................. 38 80
Smokeless.................. 27 52
Tetryl............................... 73 113
Trinitrotoluene (T N T )................................. 48 91
Lead azide......... ................ 84 127
Inspection____________ 88 128
Manufacture.................................................................... 86 127
Properties________________________________________________ 85 127
Storage------------------ ------------------------- ----------- .......................... 87 128
Military high explosives:
Manufacture______________________________________________ 41 84
Requirements.................— ........................................................ 40 84
133
TM 9-2900
M ILITA R Y KXPLOSIVES
Paragraphs Pages
Mercury fulminate_____________________________________________ 74 115
Inspection_________ 79 120
Manufacture______________________ 75 116
Properties____________ 76 117
Storage--------------------- 78 II!'
Use.......................................... 77 119
Nitration------------------------------- 10 9
Trinitrotoluene (T N T )------------- 45 86
Nitrocellulose testing................................... 30 63
Nitrometer, D u P o n t.-------------------------------------- ---------- - .............. 29 61
Nitrostarch explosives.................................................. 62 105
In spection ..------- ------- 07 109
Manufacture__________ - ---------------- 63 105
Properties_______________________ 64 106
Storage__________________________ 66 108
Use...............................................— ........... 65 108
Picric acid_____________________________________________________ 56 99
Inspection.. ............................ 60 102
Manufacture------------------ 58 100
Properties_______________________ 57 99
Storage............................................- ............................................ 61 104
Use_____________________________ __________- ........................- 59 101
Powder:
Black__________________________ 35 77
Inspection____________________ 38 80
Manufacture________ 36 78
Packing.................. 37 79
Storage_______________________ 39 83
Cannon, FNH and N H ____________ 17 34
Double base________________________________ . ---------------- 33 75
E. C ...................................................... 34 76
Smokeless:
Cotton, raw, purification f o r . . ................................. -- 9 6
Form ____________________ 7 5
Grains:
Dimension control.............................................. 20 42
Form and size.............. ..................— ................ .......... 19 36
Granulation........ ............ 18 36
Historical sketch o f..............................................................- 6 4
Inspection................. 27 52
Instability, causes____________ 23 47
Manufacturing processes..................................................... 8 6
Blending..... ................................. 16 32
D ryin g............................................................................. 15 30
Graining and cutting_______ 13 25
Shipment------------ ----------------- . . _____ ______ 26 51
Stability_____________________ _____ - ______ ___________ 21 46
Tests___________________________ 22 46
Stabilizers__________ ___________ _____ - ------------------ 24 48
Storage...... .................................... 21,25 46,49
Testing_______________________ 22,31 46,68
134
TM 9-2900
M I U T A UY K X PI .OS IVES
Paragraphs Pages
Propellants, compound...... .......................................................... . 32 74
Pvrocotton purification........ — ..................................................... 11 14
Raw material testing.......... ......................... ........... ........ ... 28 52
Smokeless powder.................................................................................. 6-31 4-74
Solvent recovery.. ................. .. ...................................... .. 14 26
Storage:
Ammonium picrate (explosive D> 55 98
Lead azide---------------------- ---------- 87 128
Mercury fulminate______ ___ 78 119
Nitrostarch explosives . . . ------- 66 108
Picric acid____________________ 61 104
Powder:
Rlaek.......................... 39 83
Smokeless__________ _________ — --------- ----------- 21,25 46,49
Tetryl..................... 72 113
Trinitrotoluene (T N T )------------- 49 93
Testing:
Nitrocellulose_________________ _________________ - - 30 63
Raw materials------------ 28 52
Smokeless powder----------- ----------------------------------------------- 22, 31 46, 68
Tetryl_________________ 68 111
Inspection_____________________ 73 113
Manufacture................... 69 111
Properties_____________ 70 112
Storage and handling.. ----------------------------------- 72 113
Use....................... ....................................... - .................................. 71 112
Trinitrotoluene (T N T ).................................................. 42 84
Inspection------------------ 48 91
Manufacture------------------------ ----------------------------- ------ 44 86
Nitration----------------------------- 45 86
Properties________________________________________________ 43 85
Purification------------ 46 89
Storage------------ 49 93
Use............. 47 90
[A. O. 062.11 (6-18-40).]
By order of t h e S ecretary of W a r :
G. C. M ARSH ALL,
Chief of Staff.
O f t c ia l :
E. S. ADAM S,
Major General ,
The Adjutant General.
135
U- 5. GOVERNMENT PRINTING OFFICE . 1*»*0

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TM 9-2900

M ILITA R Y EXPLO SIVES

Prepared under direction of the

Chapter 1. Propellants. Paragraphs

1. D efinitions.— a. Explosive.— An explosive may be defined in

of substances, which upon application of a blow to a small portion of

hydrates as nitrocellulose, nitrostarch, and the nitrated derivatives of

known as detonating explosives, disruptives, or more commonly, as

MANUFACTURE OF SMOKELESS POWDER

6. H istorica l sk etch .— The first nitrocotton which was made was

sive and developed it to such a point that he endeavored to sell the

b. Form .— Smokeless powder is manufactured in the form o f small

I' u, uub 1.— Flow sheet for manufacture of smokeless powder.

to decolorize the fibers is employed. The excess bleach is destroyed

(Z>) A nitrating unit in this system consists of a battery o f four iron

I ' k j u h e 3.— D u P o n t mechuiiirul-Uipper process, wringing centrifugal door. Plcntluny

c. Cellulose.-— (1) The exact molecular weight of cellulose is not

Pnrls C C . No. Percent

(3) A t the present time considerable doubt exists as to the exact

F kiuke 5. -Roiling tubs for purification of nitrocellulose before pulping, Picatlnny

not less than four changes o f water. Careful attention to details

(1) The type o f beater most generally used in manufacture of

the first stage o f the treatment a washer, consisting o f a large octagonal

c. Poaching .— It has already been pointed out that in the pulping

fibers set free an additional amount o f acid. It is therefore necessary

A fter the boiling treatments the pyrocotton is given at least 10 cold

d. Screening.— A fter purifying the pyrocotton as described above,

amount o f water present. This wringing operation consists merely in

solvent, according to the web thickness o f the powder; thus ap­

that the usual dehydrating press charge o f 25 pounds dry weight

mass in such a manner that the evaporating losses are minimized by

dense, elastic, translucent brown or amber substance. These opera­

F igure 12.— Preliminary blocking presses, Carney's Point, N. J.

13. G raining1 and cutting-.— a. Operation.— The final operation

FlGUiitt 13.— Macaroni and final blocking; presses, Picutinny Arsenal, N. J.

14. S olv en t re co v e ry .— a. Pur pone.— The powder as it comes

F iu u k u 14. Grain ill); proas room, lMoatliinj' Arsenal, N. J.

process in drying powder is one o f solvent recovery, although recov­

to a large metal tank. In all o f these types the operation of removing

the powder, the larger calibers requiring a greater length o f time

( b ) For powder o f heavier web than 0.095 inch—

It is not practicable from an economic standpoint to reduce the

F igure 19.—Interior water-dry house, l ’kiatinny Arsenal, N. J.

to a hopper and then slides by gravity into a shaking screen. This

controlled by the speed at which this shaker is operated and by the

1). Operation and equipment.— (1) The blending operation consists

17. F N H a n d N H p ow d ers fo r ca n n o n . —a. Development.— At

F iourk 21. I’owder weighing and packing room, l'lcntinny Arsenal, N. J.

ether-alcohol, used in manufacture is not completely removed, the

This proved to be a serious objection during the W orld War owing

Eiuuuu 22.— Piual air testing of powder boxes, l ’ieutinny Arsenal, N. J.

b. FNII powder.— (1) The FN H type of powder has been obtained

o f flash-reducing agent in the powder composition, such a procedure

projectile the prescribed muzzle velocity within the permitted limit o f

Ficuiu: 24.— Cross section ot multiperforated powder grains.

(2) Types .— Smokeless powders are granulated in regular geomet­

type o f grains. Our guns are designed to withstand a pressure in­

artillery. “ For each caliber o f gun there is designed a corresponding

(b) Relation between weight of charge and grain dimensions.—

solvent, according to the web thickness o f the powder; thus ap

dense, elastic, translucent brown or amber substance. These opera

process in drying powder is one o f solvent recovery, although recov

(2) Types .— Smokeless powders are granulated in regular geomet

type o f grains. Our guns are designed to withstand a pressure in

(b) Powder shrinkage.— In order to determine the size of die re

21. G eneral.— The subject o f stability o f smokeless powder in

or nitrates o f oxycellulose, hydrocellulose, and other cellulose com

b. Magazines.— (1) Temperature.— Magazines fo r storage o f smoke

number o f cubic centimeters o f normal thiosulphate solution repre

should be o f the quality prescribed for use in manufacture o f smoke

lion. Other small-arms compound propellants used for military pur

(9) Moisture- and ash-free.—Percentages on a moisture- and ash