From Commonly Available

Materials

Desert Publications
El Dorado, AR 717al-1751 U. S. A.

I

TABLE

OF CONT ENTS

Page
INT ROD UCTION.
APPROACH ••
I .. -II •

1
..

.......
FIELD
.,

1

MA.NUFACTURE OF BLACK POWDER POTASSIUM NITRATE·3 ....
It <I

FROM
jt ......

GRADE
~ •••

2

..~.
.:-~. -i :

:

..

Improvised IMPROVISED

Black

Powder

Process

jt

~

~:
e-


,.

'.'

PRl~RY

HIGH EXPLOSIVES
of Fulminate
.... III ~ • III

..

Fi eld Manufacture Experimental P'r o c ed u r e , Field Data. ....
III •

s,
ill

..
,.

.. ..

jt

~

..
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~

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.
'"

. ... . ·. ·... . .. . . . .. ..
• ..
III ..

2

'"

3
3 4

'"

...

III

6
8 8

Manufacture Data

of Double
It • ~

Salt s

...

...

,.

.

Experimental

.. ..
• • • • •



a

.
-III

.. .. .. ..

Field

Manufacture Data.

of I-IMT D ..

8
It • .. ...

Expe rimental

.. .

• ,. • ,. ,.
,.

.. ..
.. l1li

til

9
10

Lrn p r o vi s ed Detonator

Sy st em s ,

,

••

OPTIMIZED PROCEDURE FOR FIELD IMPROVISED DETONATOIZ S •
It •

1v1ANUFACTURE
~ • •

OF
.t .. _

If

~

III

14 14

Proc edure.

••

l1li

..

..

...

I

..

ill

"

·.

It ..

...

IMPROVISED Field

SECONDARY Manufact

11IGH EXPLOSIVES Este r s ,
• ..

<I


...


...

••
111


III

16
16 17

ure of Nit ric

..

Experimental

Data.

."

+

~

..

III'

..

..

<II'

III

~.<:

j,

.

Optimized Process for Field Manufacture of Methyl Nitrate, Ethylene Glycol Dinitrate and Nitroglycerin .. • .. .. .. ., • .. _ • .. .. • •
;10 •

,.

18

Procedure ••

•••••••••• •••••

Acid Recovery Procedure

·....
• l1li' ...

,.

....
...

••

18
21
22
, , , , , ,

Procedure ••
:.

:.:

•• •• • ••• • • ••• •••••
..

Nitrocellulose
:-:
:;

. ,.

• • • ,.

.~.

:~

Urea Nitrate

.. ..

..

..

.
til

..

..

. .. . .. .
••

23

,

•••••••
• • II

26

,
;

,

;:
.~
~

Sprengel Explosives
Nitric Acid! Cellulose

*

••

26
26

Explosives

••••• • •••

'~~.
:-:.:

Nitric Acid/Monomitrobenzene (ffHellhoffite Explosi ve s • • • • • .. .. • .. ,.
!II ..

ttl

J~:

" ~;\:

:~ :> :":~

.,

.. ..
.. '*

29
30

'-::" ~:

\ ::::'

..:-

" r:"

CONCLUSIONS
REFERENCES
APPENDIX •••

AND RECOMMENDATIONS.

. ..
• • •

~\j~

t~;

ri·

<:

••• •••••

..
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DISTRIBUTION.

.... •• • •••••• . .. . · .. .. . .. .. .
• •
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.

y.
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if: ......;

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32
34 50

:~:}.

M

•• ••

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List of Tables Table I.
Impact Sensitivity

Explosives ••

Tests of Improvised Primary ~ •• _ ••••• _ •••• of Ethyl Alcohol
.. !II

5

II.

Field Manufacture

••

6

In.

Initiation Tests of Improvised Compound Caps (5 shots each primary) .. • • • • • • • •
IV

11

"·f·· ~

}
~

Table
,<
:~

Page
Initiation Tests of Improvised (5/1611 c orn p r e s sed columns in 1/ 4n d i a , copper tubes) Straight Caps of each primary .
II • • • • •

..1 :
.'. •<
<

IV.

1·l
.. :-:: .:.. '~ :

'::

... <{ :f· :~: .,
:~. :~

12 14 18

v"
VI.

Field Manufacture
Field

of Improvised of Nitric

Detonators.

~ •

.,
• .,

Manufacture

Este rs.,
II • ~

-=

VII~
VIII. IX.

Improvised
Field Nitric

Dynamites ....

21
.•••

Acid/ Fuel Mixture of Sprengel

Tests

27

Initiation

Tests

Cellulose

Explosives3

List of Illustrations

1.

Schematic Typical

Alcohol

Still

.~

:IJ

•• • •• •

7

2.
3.

Assembly

- Improvised
•.

Cap ..
.. .. ..
II

..
+

"
of,

..
..

...

13 15

Safe Method to Ram Caps

v

INT RODUCTION

Thrust into jungle or underdeveloped areas for lengthy periods, how do Special Forces synthesize and compound explosives and propellants from indigenous materials? This .. in essence, is the problem. With more-or-less sophisticated c orn porrent s and materials like blasting caps; primacord and military explosives it is relatively easy to construct a host of ingenious and effective weapons (e. g. guns, g r enad ea , time bombs, rrrin e s , demolition and incendiary devices). But what if ready-made components and even basic raw materials are not available? This problem was the basis for an investigation into an Improvised Munitions Program. Through this program relatively simple procedures have been developed to fabricate munitions. This study is one such investigation of the program .. The development and dissemination of practical methods for field synthesis of explosives from comm.only available materials may substantially increase the independence, mobility and effectiveness of Special Forces in remote areas while reducing logistic support requirements.

APPROACH

Ways and means were dev eloped! to produce worthwhile quantities of the materials basic to the formulation of a propellant. primary and secondary high explosives. These materials extracted by field processes are described in the Improvised Munitions Handboo.k2 and were considered to be of sufficient quality to manufacture black powder and certain high explosives.. In view of these efforts, the following approach was delineated:
1. Manufacture of black powder with field extracted potassitun by techniques previously evolved.

nitrate

1 See

REF ERENC ES

1

:

.

2. Manufacture of me rcury and/ or silver fulminate (s) or other prirn.ary explosives u ai ng field synthesized~ nitric acid and field grade ethyl alcohol (redistilled whiskey). 3. If the manufacture of fulminates is: successful, construct simple flam.e initiated detonator syste1Tl{ s} using field produced fulrrri.nat e s ... 4. Investigation of other potentially useful primary based on field synthesized or other accessible c herrrrca l e, explosives

5. Investigation of the manufacture of high explosives from field synthesized materials, e_ g. , nitroglycerin and/or Sprengeltype explosi ve mixture s,

MANUFACTURE

FIELD

OF BLACK POWDER FROM GRADE POTASSIUM NITRAT~

of twelve pound s of potassiwn nitrate was extracted and used in the field manufacturing of both black powder and nitric acid. App ro xirnat ely 250 grams of black powder manufactured with field grade pota s ai urn nitrate performed as well as black powder manufactured with comtnercial grades of potassium nitrate. An additional fi ve pounds of black powder was manufactured for further studies.

A total

Improvised

Black Powder

Process

Three cups of pota s s'ium nitrate, 2 cups of powdered charcoal, 1/ Z cup of sulfur and 3 cups of water are mixed in an iron skillet or similar container. 2. hour. The mixture is slowly heated and sti rred for about 1/2

1..

z

.

_, ..-.. :

-

..........................................................................................................................................................................................

3. and stirred

The slurry is poured into 5 pints of alcohol (any kind) for approximately 5 minutes.

4. The slurry is then poured onto a cotton cloth and the alcohol is allowed to drain until the mixture is nearly dry (about 1/2 hour). 5. The mixture is then granulated approximately 1/16" diameter holes. through a screen with

6..
completely

The granules are spread on a dry surface and allowed to dry in open air (about one hour at 900 F)..

IMPROVISED PRIMARY mGH EXPLOSIVES

Field Manufacture

of Fulminates

Fulminating compounds were prepared as early as the 18th century, however, until Howa rd t s research in the beginning of the 19th century J: little reliable information appears in the literature. 5 Mercury fulminate was employed by NobelG in the mid-19th century on a commercial scale. and remained in use for nearly 7"5years until supplanted by lead azide and other materials. 7,8 Test s indicated that it is practical to rna nufa ctu r e both mercury and silver fulminate in the field. Both fulminates are readily synthesized; both have drawbacks: 1.. areas.
2..

Mercury

metal

may not be readily available

in many

Silver fulminate

is extremely

sensitive

to impact or

abrasion .. Since silver is commonly available (silverware, jewelry) some effort was devoted to reducing the impact sensitivity of the silver fulminate. This was accomplished with partial success by adding easily available desensitizers such as cornstarch to the wet fulminate.

3

Experimental

Data

The requisite materials for the production of silver or mercury fulminates are the rn eta l s , nitric acid and ethyl (grain) alcohol. Early probe tests, using commercial reagents, indicated that field production of fulminates was quite practical. Subsequent tests, using field synthesized Ing r edi ent s , brought to light several pr-obl.erns ; Field synthesized nitric acid is ahnost anhydrous and there is almost no reaction between the metal and the acid. This p r ob l ern was simply eliminated by gradually adding water to the acid until a vigorous reaction was initiated. Ethyl alcohol posed a somewhat greater p r obl ern , Cornrn.e r c ia l whisky was found to be too dilute to work properly. However. whisky and! or 'Nine can be redistilled to produce a sati sfactory grade of concentrated ethyl alcohol. (See Figure 1.) Apropos J the quality of ethyl alcohol produced by field distillation technique s was briefly inve stigated. A crude distillation unit was built from a IS-gallon trash can and fitted with a condenser coil made from 15 feet of 3/8 inch diameter copper tubing. A rna sh of crushed corn and water was prepared, yeast added and the mixture allowed to ferment for five days. On distillation the brew yeilded a substantial am.ount of a pp r oxi.rna.te Iy 870/0 ethyl alcohol; a concentration satisfactory for fulminate manufacture. Alcohol production was not investigated at great length as competent technology in this a rea is almost uni ... v e r s a l , A typical method for field manufacture of ethyl alcohol is described in the following pages. Initially I: fulminate wa s produced by di s solving fi ve grams of the metal in 30 cc of diluted field grade nitric acid and adding the solution to 50 cc of field grade ethyl a l.c ob o.l, Sub sequent tests showed that satisfactory yields coul.d be produced with reduced amounts of acid; the optimized proc edure is pre sented in the Appendix. Generally, a batch of fukrndriat e can be produc ed in 1/2 hour or less, although we have occa sionally observed, with silver Jo delayed reactions of up to 1-1/2 hour e. While the fulminate reaction is relatively sa fe , the dense furn e s evolved are toxic and the entire procedure should be carried out in a well ventilated area or outdoors ..

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:

Since silver (in the form of coins) is generally more readily available than mercury. attempts were made to reduce the silver aa lt t s extreme impact sensitivity.

We found that the addition of cornstarch and! or tapioca to wet fulminate would significantly reduce irn.pact sensi tivity, On a crude falling-weight test device .. it appeared that cornstarch would double and tapioca triple the drop height necessary to detonate silver fulminate. (See Table I)

TABLE

I.

Impact Sensitivity Tests Primary Explosives

of Im.provised

Prin;,ary
Pure Ag fulminate Dime Ag fulminate Mercury fulminate Cornstarch/ Ag fulminate Tapioca/Ag fulminate Double Salts HMTD*

Minimum Detonation Hei&ht dsLin:t1.
IIlwl

Average Detonation
I

zzL_

Z

3
4

3.4 4.4 5.4
7. 2 10. 5 14. 1

6

9
12

18

19. 1

*Hexamethylenetriperoxidediamine

It is believed that diluent desensitization of silver fulminate in the field is not reliable; differences in particle size and purity of both the fulminate and the desensitizer are likely to produce .. erratic results. For this reason silver fulm.inate should be· used only when no other alternatives are available.

5

TABLE

Il ,

Field Manufacture

of Ethyl Alcohol

Materials Required ____________ ~----I--~ Grain (wheat, corn, Large drums Metal tubing
Yeast

Sources -

rice,

etc ..)

Crops, silos. rice paddies, Clean oil drums; etc.

etc.

Plunabing, vehicles
Bakeries,

food stores

Buckets Stirring stick or paddle Heat source

Procedure

1. Fill a gallon bucket with dry grain and moisten with three cups of water. Cover bucket lightly and allow grain to sprout (about 1 week).

2,. 3.

When the grain has spz-outed, Crush or grind additional

c rush or grind it. of drr grain.

5 gallons

4. Mix the crushed dry and sprouted grain and add 3/4 gallon of water. Heat this rna sh until hot but riot unbearable to the hand. Maintain at this temperature for 3 hours. Remove heat and allow mash to cool to about blood temperature.

5. Add 6 teaspoons of yeast to the mash and stir well: cover but do not seal and stand in warm place for 5 days. After 5 days, pour- fermented mash into the still and heat as shown in Figure 1. Stop heating and disca rd mash after 1 pint of alcohol per gallon of mash has been collected.

6

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Field

Manufacture

of Double Salts

While not generally well known, and not used c ornrn e r i ca Il.y , the double salt of silver ac etylidel silver nitrate (Ag2 C2 / AgNOs) appears to be a suitable material for im.provised initiators. Double salts may be synthe sized in the field from silver (silverwa:re, jewelry) , field synthesized nitric acid, and acetylene generated from calcium carbide.

Experitnental

Data

Our first attempt at producing double salts followed the preparation given in the literature. 9, 10111 This preparation called for the purification of the acetylene by bubbling it through perrnanganic acid. We quickly determined that not only was this step unnee es sary J- but in fact quite dangerous: a pp r oxi rna t eky 10 second s after the acetylene contacted the perrnanganic acid, there was a sharp explosion that demolished the apparatus. After elimination of this at ep , the process appeared to be relatively safe, and subsequent field production tests proceeded without Lncid ent , The optimized proc edure for the fi eld manufacture of double salts is presented in the Appendix.

Field

Manufacture

of IDvlTD

Hexamethylenetriperoxidediamine (H1v1TD) is perphaps the only organic peroxide that has been seriously considered for commercial initiators. 12 This prim.ary explosive is probably the ea si e st and safest to manufacture in the field. The requisite materials for the production of HMTD are as follows:

HexamethylenetetralTIine, a corrrm on drug used for bladder infections and marketed under the narrre s Urotropine, Methenatnine,. Hexarnin and ot he r s ,

1.

8

--------

.. _

.

2.
3. under

Hydrogen

peroxide
in drug stores

Citric acid, obtainable the name "Sour Sa lt ",

and in food store s

ExperiITIental

Data

Davis

4

gives the following

preparation

for I-ThIIT D:

"Pr epa ratron of Hexamethylenetriperoxidediamine" Fourteen grams of h exa m et hy Ien et.et r-arrrin e is dissolved in 45 grams of 300/0 hydrogen peroxide solution which is sti rred mechanically in a beaker standing in a freezing mixture of cracked ice with water and a little salt. To the solution 21 grams of powdered citric acid is added slowly in small portions at a time while the stirring is continued and the t ernp e rat.ur e of the mixture is kept at 00 or b el.ow, Aite r all the citric acid has di s solved, the mixture is stirred for 3 hours longer while its temperature is kept at 0°. The cooling is then d i s co ntdrrued , the mixture is allowed to stand for 2 hours at room temperature, and the white crystalline product is filtered off, washed thoroughly with wat e r , and rinsed with alcohol in order that it may dry out more quickly at ordinary temperatures. "

Our efforts were focused On the examination of Davis' cedure and its potential modification fo r field use.
A brief

pro-

analysi s of the availability of the components indicated that only the 300/0 hydrogen peroxide would be a problem. Howev e r , drug stores commonly carry a 60/0 hydrogen peroxide solution for use as a hair bleach. We found that I-nv1TD could be produced with bleach grade pe r-o.xid e, In addition" Davis 1 s preparation calls for extended agitation of the solution at 0 C. to obtain maximum yields .. It was found that sati sfactory yields could be obtained with little agitation at room temperature if the precipitation time was extended. The opti.rrii z ed process for H1v1TD in presented in the Appendix.
G

9

'I'!!!'l!!!'I!I'I'!I!I!I!'!I!'!P.I!I'!I!I'!I!~---

__

---

__

---"""""""'~----

.

Improvised

Detonator

Systems

Once a p r i.rn a ry explosive has been improvised the next problem is to safely and effectively utili ze it. To this end, tests were conducted 'With improvised primary explosives to determine optimum method( s} of u s e, A standa rd Irn pr ovi s ed cap and alte rnate systems were evolved; an arbitrary cap was used to check performance of various improvi sed h ig h explosives. Figure 2 illustrate s a standard cap configuration.

It is evident that the cap envelope should be capable of being manufacturable f r orn readily available material s, On the surfac e this seems to be a simple problem; one merely needs a small tube in which to load the explosive. This, howeve r t is not the case. For example, caps fabricated with tubes made f'r orn rolled paper or aluminum foil did not provide adequate confinement; henc e , such caps did not reliably initiate high explosive s, In addition. foil or paper tube caps tended to leak when used in conjunction wi th liquid explosive s, With the exc eption of ~ 22 caliber long rifle ca s e s and 5. 56mm ca s e s , small arms cartridge cases are generally too large .. The optimum cap envelope material.; judging f r orn probe te s t s , s e ern S to be small diameter rn eta l tubing and, specifically; 1!4u d.ia m et e r soft copper tube such as that used in vehicles ~ plumbing .. etc.
Initial tests we re conducted with 1/ 4~!diameter copper tube caps 3 -1/ 2 H long containing straight J unconfined charges of im-provised mercury- fulminate. These caps were fired into 50 gram target c ha rg es of prilled TNT (duPont tfpelletolO) confined in paper cups. Result s were e r ra.ti c, Radically improved reliability was ob served when the mercury fulminate wa shand ... re s sed into crimped p tubes. A s expected. compres sion also inc reased the initiating efficiency of other improvised primary explosives. Compound caps, that i s ~ ca ps containing a ba se charge of high explosives tare generally the rrro st efficient and reliable. When suitable solid high explosives are available they can be used to extend the supply of improvised primaries and provide more powerful initiators.

10

-------~~-----------------.-

..-

- -.- - -- -----------_

.

To provide boundary data on efficiency and reliability, both compound and straight improvised caps were tested with a variety of military and improvised high explosive target charges. The results of these tests are presented in Tables III and IV.

TABLE

III.

Initiation Testa of Im.provi sed Compound (5 shots each pzirna ry)

Caps

Cap

Base Ch~rs;e 1 in~ Col. TNT 1 in. cei. C4 NOTE:

Target Chars;e 50 grn Pelletol in Paper Cup
50 gm C4

Mercury Fulminate

HMTD
5/5 Positive

Double Salts

5/5 Positive

5/5 Positive

4/ 5 Po siti ve

4/5 Positive

4/ 5 Positive

Caps ignited with. Bickford Safety Fuze. A 11 caps made with 1/4 inch dia rn et e r soft copper tube with 5/ 16 inch hand -pre s sed columns of each primary over base charge. (See Figure 2)
t

In summary it appea r s that i.rnpz-o vi sed rne r c ur y fulminate is generally the most reliable init iat o r , Also, compound caps containing base cha rge s of solid high explosives have greater output and a r e , therefore, rn.ore reliable. Improvised and commercial dynamite appa rently can be reliably initiated with any of the improvis ed caps.

caps (without base c ha r containing inch heights of des enitized silver f ulrrriria.t e failed to detonate pipe-con ... fined and unconfined 50 gram charges of prilled TNT I C4, Urea Nitrate and eTA. However, straight silver fulminate caps reliably initiated all improvised and comme r c ia l 400/0 nitroglyc erin dynamite. Compound silver fulminate caps containing a base charge of 1 inch hand-pre S5 ed PETN ext racted from p rdrna c o rd reliably initiated pipeconfined prilled TNT i eTA; nitric acid/paper and 2.11 unconfined dyarni te s , Initiation of C4 (2 out of 5 shots J unc on fin ed] wa s erratic, and there were no detonations in 5 trails of pipe-confined improvised urea nitrate. Because of the extreme sensitivitiy of silver ful.rnina t e , we do not recommend its manufacture or use if other materials are available.
Straight g e] 5/16 c o l urn n

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--=-===========:.:..:.__....;,;,;,;:.;.;:_ ;;;;,;;;.;.;,; ;;;.;.;, ;;;.;.;, .;.;;.;; :_._;,;,;,;;_;.;..;,; .._.;;;.;.;,;;.;..;;,;;..;,;;; ;,;,;,;,; _.;.;.;,;;._ ;;;.;.;, ;;..;,;;; ..,.;...,;; ;;;.;.;,

_

~~~~~~~~~~~~~

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..-.~----

.

Fuze

1/4 Inch Coppe r Tube

Crimp

Tape to Bring

Fuze to Size

A Few Granules

of Black Powder

5/16 - 3/8 Inch Colum.n of PriITlary Explosive

1 - 1-1/ 2 Inch Column of Seconda ry Explosi ve (If Used)

Small Paper

Wad

Crimp

Figure

2.

Typical AsseJTlbly
13

- Improvised

Cap

OPTIMIZED PROCEDURE FOR FIELD MANUFACTURE OF IMPROVISED DETONATORS

TABLE

V.

Field Manufacture

of lrn.provi.sed

Detonators

Materials

Required

-

Source
Improvised

Prima ry Expko si .re 1/4 in .. diameter Soft Copper or Alwninum Tubing Wood, brass or alwninurn ram to fit tubing Fuze to fit tubing

Plumbing.

vehicles

Black Powder Booste r Explosi ve

Improvised Cornrn e r c ia.l or military fuze Improvised fuze Commercial or military Improvised TNT i C4, PETN

blasting

munitions

Procedure

into

1. Make a 2-1/2 ground behind Figure 3)
small

inch deep hole in a large piece of wood, ba ic into (See
r r ade , or a tree st ump,

or

2. and close

Cut a piece of copper or aluminum tubing 3 inches long one end with rammed paper plug or by harnrne r-ing shut. Place the tube on the wood block or in the hole behind the open end up ..
of crushed with w ood ,

3. barricade,

4. Fi rrnly pres 5 on 1 to 1-1 / 2 inche s column TNT J C4 pieces or PETN extracted from primacord aluminum or brass ram ..

5.
primary

Gently (but firmly) pres 5 in about 3/8 inch column of dry explosive, as shown in s ket c h, Carefully remove zarn ,

14

6. Sprinkle a few granule s of black powder into the tube (opti ona 1) •
7. Wrap fuze with tape or strip of paper to fit inside diameter of cap tube (sliding fit), if necessary.

8. Press or tape securely
.
:::.'

fuze firmly into cap and crimp lightly with pliers in place"

~ ~ .. :~ .

CAUTION! Shield body behind or below barricade and keep head and face clear when pressing in primary explosive •

I',
... :::. ......
:

~I~:(::::

NOTE:

If no secondary explosive is used in ca p.a fired. ZZ caliber long rifle case may be used as a container for the charge.

wooden bar ................
ram

<;<:,p hoi e in stump

nJln kneeling with head below Ieve' of cap

7

ii~
........

Figure

3.

Safe Method to Ram Caps

lill!:~'/"
':':':':':':',:.,,:

..

,!:~:!:!~i
...
:: :

15

-:1P•

.

IMPROVISED

SECONDARY

mGH

EXPLOSIVES

Field

Manufacture

of Nitric

Esters

A lite rature sea rch di sc Io s ed thre e c ornrn on alcohols of potential i nt e r e st: methyl alcohol. ethylene glycol. and gIyc e r'i.n, 12 t 13 Methyl nitrate appears to be the safest and easiest of the three esters to prepa re in the field. Among its advantages are:
1. 2..

low sensitivity

to acid contamination

distillation point much below explosion temperature (BP = 65 cO C., explosion temperature ~ 150:0 C.) thus reducing prepa ration haza rd s ..

Methyl nitrate is relatively volatile a nd , for this reason, is not used comm ercially 13 How ev e r , its volatility may be an advantage in field manufacture as it avoids decontamination problems from spillage. Conversely t explosive mixture s containing methyl nitrate should be well wrapped to avoid undue evaporation. Ethylene glycol dinitrate ranks as second choice for improvi sed production. While slightly more powe rful than methyl nit rate .13 it has the di sadvantage of slower separation from the nitration acids and a greater sensitivity to c ont.arn inat i on,
It:

Glyc eryl t rinit rate (nit roglyc e rin) l:~" 14,,15 is the least desi rable for field manufacture because of greater sensitivity to acid contamination and mechanical shock, Howeve r J the availability of glycerin via anim.al fat is a d i stinct advantage.
All of the latter explosives are liquids and therefore difficult to employ in munitions. Nobel solved the problem by absorbing nitroglyc erin into diatom.ac eous ea rt h, 13, 14 Other common absorbents can, of c our s e , be used in irnprovi s ed manufacture .. Shredded paper J: cloth and sawdust, for example, provide quite satisfactory ab sorbents for improvi sed dynamite s, In addition, any of the latter nitric esters can be used to sensitize and increase the brisance of ammonium nitrate explosives. Thus i relatively small quantities of these powerful high explosives can be greatly extended.

16

Experimental

Data

Prepartion of the nitric esters of methyl alcohol, ethylene 45 glycol and glycerin are quite similar. 6,12 .. 13.1 .1 The simplest procedure is to slowly add the alcohol to concentrated nitric acid and then drown the mixture in a large exceSs of water J permitting the explosive ester to settle out. While this process is relatively safe and easy. it is very wasteful of nitric acid. Nitration wit h mixed acids (nitric and sulfuric) conserves nitric acid and improves explosive yield. And, since sulfuric acid is required to improvise nit ric _ it is beneficial to conserve both materials. sulfuric acid in particular. Hence, our efforts were devoted to evolving a field process that conserved acid and provided for acid recovery after nitration. Field purification of spent acid is a somewhat haza rdous pr oc e s s , This hazard is greater with acid remaining from the nitration of ethylene glycol and glycerin that it is with acid from methyl nitrate p r epa ra ti on, Spent acids contain trace amounts of explosi ve that will not sepa rate on sta.ndi ng , Since purification and recovery of spent acid requires boiling to drive off impurities, there is some change of violent decompo sition of di 5 solved explosi ve , Such decomposition usually splashes acid from the vessel; high order detonation is unlikely unles s there is an acutal layer of explo si ve left in the containe r , Fortunately I spent acid recovery I purification does not r e qri r e close attendance a nd , for this reason, the hazard can be minimized" Optimized proce s s for field manufacture of methyl ni t ra t e , ethylene glycol dinitrate and nit roglycerin are presented along with spent acid recovery procedure. Improvised dynamite formulation procedures are described in the following pages.

::~ .::..

}

'~~(:' .

:~:::.\ vtv-

':.:.

17

Optimized ProceSS for Field Manufacture of Methyl Nit rat e , Ethylene Glycol Dinitrate and Nit roglyc erin

TABLE Material ........

VI.

Field Manufacture

of Nitric

Esters

Required ,.'

Sources ' ,._, Clear battery acid boiled until white fumes appear Field Grade Nitric Acid Methanol Wood alcohol alcohol). Anti ..... freeze Anti-freeze (not denatured

Sulfuric Acid

Nitric Acid Methyl Alcohol

Ethylene Glycol Glycerin Eyedropper
Aluminum Stainle s s Steel Teaspoon Wax Coated Ceramic Sodium Carbonate or Sodi urn Bica rbonate Large Drarn et e r (2qt) Jars Narrow Clear Glass Jar

(pe rrnanent)

Glycol Drug Stores Drug Stores Medicine bottles

,

'

Washing soda Baking soda

1 Optional

j

.:

.1

~

,

'.~
.,
'.

:! ,

.~ .',

Procedure

~i. .
'';:

::~
· .~
; .:i

~·i

<

.:~ ~

1.

Add 24 teaspoons

sulfuric

acid to 16-1/2

teaspoons

nitric

acid in a 2 quart size bottle. CA UTION! Acid will burn skin and destroy clothing. If any is spilled, wash it away with a large quantity of water. Do not
inhale fume s.

18

»X"-"-- •••

2. Plac e the bottle in a stream cold water and allow acid to cool. 3.

or large

basin

(3- 5 gallon) of

Rapidly swirl the bottle to create a whirlpool in the liquid (without spla shing) while keeping the bottom portion of the jar in the water.

... ... .... . .......~.: »::

Step

3.

SVlirling bottle in basin of water while adding alcohol

4. While continually swirling. add", 1/2 teaspoon at a time, 13..1/2 teaspoons methyl alcohol or 9 teaspoon s ethylene glycol or 8 teaspoons glycerin allowing mixture to cool between a.ddi.ti on s, NOTE: Complete addition should take approximately 10 minutes.

CAUTION! If there is a sudden inc rea s e in the amount of fum e s produced or if the solution suddenly turns much darker or begins to froth, immediately dump charge in the wat e r , (Note: within 10 seconds.) This will halt the reaction and prevent an a cc'id ent, Any explosive fo r m ed rna y be recovered if basin is used, See Step 7 in procedure for separation.

19

.---~~~~~------------------------~---

5. After the final addition J 8M r l for anothe r 30- 45 second s and then allow bottle to stand in wat e r until the two layer s s epa rat e , (rn et hy l alcohol 5 rn i n ut e s , glyc e rin 10 minute s. ethylene glycol 20 - 25 minut es) ..

NOT E:

This s epa ration and tho s e to follow a re best done in s m a Il e r , narrower jars to allow a sharper distinction between layers.

6.
ceramic bottle.

or a Iurn i.nurn , stainless steel, or wax-coated s po on ; remove top layer and put in another T'hi s liquid is the explosive.
With an eye dropper.

Ste p 6.

Rern ovi n g top layer

of explosive

with eyedropper 7. Add an equal quantity of water to the e x p l os i v e and swirl. Allow to sepa rate a ga in , The ex pl o s i v e is now the bottom la ye r .. 8. Carefully remove t h e water (see Step 6) and repeat St ep 7 with a s ol ut i on of table spoon of socii um ca rbonate or bicarbonate and water (liZ tablespoon carbonate/quart of wat e r}, i stored er salt l uti If carbonate is not available use plain wat e r
The ex pl o s ve may be und the s o o n,

II

20

Ii

BB.

Ii

.:::~<;'.;:;-.\:~},{:; :
"

,

,

:',',

..

. . ..... ..

_'

...

:'...,
,

.............

:~

.... '. -.' .' -:-:. .:', ..
'

,~>',*,

:.':

.

.. ..

.•~:........:--.r..........

. -,~~_~, ., ............

.

'.' -~,

", ~.:...

.

Step B.

Removing

water

from

explosive

- now the b ott orn layer

Acid

Recovery

Procedure

1.. After removing the explosi ve from the a c id , plac e the acid in a safe place where it will not be d i sturbed for 6-8 hours, and cover lightly to prevent contamination. CA UTION! Acid will burn skin and destroy clothing. any is spilled, wash it away with a la rge quantity water. Do not inhale fumes. After 6-8 hours Step 6 on page 20) 2.
II

If of

remove

any explosi ve on top of the acid

(Se e

Place 1/8 the a c id ' s volume of water in a clean heat-resistant glass or ceramic ja r a nd slowly pour the acid into the wate r , 4. Place the acid/ water jar in a safe plac e (away from. people or materiel) in the Silll; lea ve jar for one da y.

3.

5. Plac e jar on a slow fire at lea st 25 yards f'r orn people or property and watch from that distance. When dense white fumes appear remove from. heat. The liquid remaining is plain sulfuric acid. Allow to cool befor e using again.

21

TABLE. Mate rials Needed:
~ dll 11 I

VII.

Improvised

Dynarrrit ea

Improvisea

Explosive

Methyl nitrate

Nitroglycol
Nitroglycerin Absorbent Fine sawdust Shredded paper Shredded cloth Baking soda Washing soda Slaked Lim e

Stabilizer (optional)

Cup
Pans Teaspoon Wooden stick

Procedure

1. Place one firmly packed cup of absorbent spoon of stabilizer in a small pan.

and 1/2 tea-

Z, While stirring with a wooden stick, slowly add explosive until the mass is very damp but not wet enough to drip... If m.ix gets too wet add more absorbent.

CAUTION! Do not handle liquid explo si ve or allow to contact skin. If thi s happen s, flush away Irnrn edi at e ly with large quantity of water. Keep any grit. sand or dirt out of mix.

If n:F~kiEg am.t::onium L,

n~trate:ba se _~r.~~ite

Place one firmly packed cup of fine ground ammonium nitrate, 1/2 teaspoon of stabilize r and about 1/4 cup loosely packed fine sawdust (if very fine use Ie SSt if coa rse more)" in a small pa n, 22

2"" While stirring with a wooden st ick , slowly add about 4-1/2 to 6 tea spoons of liquid explosive.. When properly made the material is just damp looking, but do not use less than 3 teaspoons of liquid explosive .. - the more used; the more brisant the d ynarrrit e , NOT E: Store rn et hy l nitrate vent evaporation. dynamites in sealed containers to pre-

14
'

.":

..

.. .
)
I

~

.

... ~- .,j~ .:."(
.
..

¥ ..:'.
=.....i:....
... ~~..

:to
.

Step 2.

Adding

explosive to sawdust and shavings

Nit roc ellulose

Some consideration wa s given to field manufacture of nit r ocellulose and subsequent preparation of improvised smokeless powder. The nitration of cellulose suitable for sm.okeless powder manufacture requires relatively large quantities of pure sulfuric and nitric acids. and extensive purification and control p r oc e s se s". In addition, many of the components (e. g. acetone) are not likely to be available in the fi eld, Da vi s f s laboratory preparation" of nit roc el lul o s e , given below, is indicative of the problems.

1'1 ;;',~.:.,~parati0':l of PY,ro,cel~u~?se"
;!!!!:~

Equal volumes of sulfuric acid (1. 84) and nitric acid O. 42) ·::~:::!;!:::::·.·:·are mixed by pouring the sulfuric acid with stirring info the nitric
II@:::

illlli:::
[iIi!:;,

23

acid, and the mixture is allowed to cool to room temperature. Five gram s of absorbent cotton, previously dried at 100 D for 2 hou r s , is thrust quickly Irit o 150 cc , of this mixed acid and allowed to remain there for 30 minutes while it is stirred occasionally with a glass rod. The cotton is removed, freed as much as possible from acid by pres sing against the side of the yes sel , and introduc ed quickly into a large beake r of cold water where it is sti rred about in such manner as to accomplish the prompt dilution of the acid with which it is aat u r at ed , The product is washed thoroughly in running water, and boiled for an hour with distilled water in a large b eak e r , then boiled three times with fresh portion s of di stilled water for a half hour each time. If the water from the last boiling shows the slighte st t race of acidity to litmus paper ~ the pyrocel1ulose ought to be rinsed and boiled one e rn o r e with di stilled wate r , Finally the excess of water is wrung out, and the pyrocellulose is dried in a paper tray for 48 hours at room temperature. rT
j

tt

Guncotton

is made in substantially

the same way as pyrocellulose

except that a stronger mixed acid containing approximately 240/0 nitric acid, 670/0 sulfuric acid, and 90/0 water is used. Long -fiber highgrade guncotton is usually manufactured by the pot process and with the use of mixed acid which is nearly anhydrous. Iron pots are generally used. For the nit ration of 4 pounds of dry cotton, 140 pounds of acid is introduced into the pot and the cotton is irn m e r sed in it, pressed down, and allowed to digest for 20 or 30 minutes. The contents of several pot s a re centrifuged at one e , and the product is stabilized in the sam e way as pyroc ellulose exc ept that it is not pulped. n In view of logistic and stability problems" and the relatively difficult synthesis of nitrocellulose, we discarded it as a candidate for improvised systems. An alternate form of nitrocellulose was ~ how ev e r , evolved in the high explosive system described previously"

RDX

RDX, cyclot rimethyl·enetrinitramine, is the major constituent of a number of powerful military explo ai yes (C4, for instanc e). When first considered, RD:X appeared to be a worthwhile addition to the family of field irnprovi sed explo si ve s ,

24

t et r-arrrrne , a common

urinary

di ai.nfec tant , a vat Iabl.e under many·.:>'.::::};:':;::.;:}:;:(:~\l;:;·;///::::lHHn·\\:)\:)\:)\:)\:\)x:;.:.::.::

and mat erial is poor, explosives

and effa rt is bette r di rected

to higher yi.el<I .:~.:.·.:}/.:;.::':":~·:::~i::~;:~i:;:::::l·:::~\~~::::?~{::~:;I:~::}~~::l:i~~IH~~~~l:{;::;;:\:~}::r:)!:{/;::;··:-:· ...

suc~ as nitri~ e ster~.

.

.'/tc:;;;'i..'~;;'i!;0:jJ~I~~111~~1!:
','

:,' ':.

~:=:.:

In p r epa rrng RDX In the fi e ld we followed Da vi s t a procedure~:'::<.·:·:···~·\·.::;::::;: ·.<·:·.:.::i::·~::::::::~~.)::r::::::::·:.:.:::::·.: ....::: ..: .. (given below), substituting field grade nitric acid and deleting predse/i'<H){(: cooling. .:.:.: :.:././ . ..::.:.::: -. .. /... : ;: . ....... :.. . :...
.....
:.

"It has feebly basic propertie s and forms a nitrate, Cs H12 N4• ZHN03 J m , p. 165 (I.. soluble in wate r .. insoluble in alcohol. et he r , chloroform, and acetone. The p r oduc t , C3Hs0eNe, prepared by nitrating this nitrate and patented by Henning34 for possible use in medicine, was actually c yc loni te , Herz late r pat ent ed'' 5 the same aub» stance as an explosive compound a cyclotrimethylenetrinitramine, which he found could be prepared by treating hexarnethyl enetet ramine directly with st rong nitric a ci d, In his p r oc e s s the tetramine was added slowly in srna.Ll portions at a time to nitric acid (1. 52) at a temperature of 20-30 -0 • When all was in solution, the liquid was warmed to 550 J allowed to stand for a few minutes J: cooled to 200, and the product precipitated by the addition of water. The nitration has been studied further by Hale36 who secured hi s best yi e ld , 680/0, .::.:.::<. in an experiment in which 50 grams of hexamethylenetetramine was ···::·:::~:~·: ... dded during 15 minutes to 550 gram s of 1000/0 nitric acid while the a :ll::··~\.temperaturewas not allowed to rise above 300.. The mixture was ·:·····::·:;:;then cooled to 00 J held there for 20 minutes. and drowned ..
:.;

The formaldehyde which is liberated by the reaction tends o be oxidized by the nitric acid if the mixture is allowed to stand or . warmed, It remains in the spent acid after drowning and interferes :~hthe recovery of nitric acid from it , 34 Ger. Pat. 104,280 (1899). 35 Brit. Pat. 145t 791 (1920); U. S. Pat. 1, 402, 693 (1922). 36 J.Am. Chern. Soc. J 47.2754 (1925). H

25

Urea Nitrate

Urea Nitrate .. mentioned in the literature 1,. 818 a s an explosi ve , also appeared to be a good candidate for field synthesis. While relatively easy to prepare. it suffers from several disadvantages. Namely f urea nit rate requi res heavy confinement and very strong initiation to achieve high order detonation. Additionally ~ improvised urea nitrate. even when succ e s sfully detonated, is not a partie ularly bri sant explosive. Urea nitrate ha s , as its sole advantage J the ready availability of its basic component ... urine. Proc edures for the field preparation of urea nitrate is presented in the Appendix.

Sprengel

Explo si yes

According to Davis~ Sprengel explosives were introduced in 1871 by He rrnan Spr eng e l, The distingui shing features of Sprengel explosives are thei r preparation just prior to use t and that one or more of their components are liquids. Generally, Sprengel explosives contain strong nitric acid and fuel. Accordingly. these explosi ve s are difficult to handle. Sprengel-type explosives are ~ gene rally. b r i sant and easy to manufacture. Since they are normally mixed just prior to use, they are in a sense tailored to field improvisation.

This investigation covered potential candidate fuels to be used in conjunction with field grade nitric acid. Table VIII summarizes the results of this study.

The three candidates from the latter t e st s , cotton cloth, paper towels. and mononitrobenzene were subjected to further evaluation.

Nit ric ACid/ Cellulose

Explosive

s

Several types of commonly available cellulose were tested in combination with field grade nitric acid" The s e included: printed and sized paper, new-dyed and printed cotton cloth .. plain paper

26

TABLE

VIII.

Field Nitric Acid/ Fuel Mixture Test s

Material Turpentine Sugar Kerosene Sawdust
Gasoline

Bore cleaner - Military Bore cleaner Cornrn e rc ia.I Mononit robenzene (oil of Mirbane) Paper towels Washed cotton cloth

Violent reaction Violent reaction Immi scible .. no Violent reaction Immiscible - no Irn:mi scible - no

on contact with acid on contact with acid reaction on contact with acid reaction reaction

Violent reaction on contact with acid Miscible - no immediate reaction
No immediate

No immediate

reaction reaction

towels and well-washed cotton cloth. Printed paper, sized paper. and dyed or printed cotton cloth reacted quickly with the acid and were therefore eliminated. Plain paper towels and washed cotton cloth, however, appeared reasonably stable. Te sts we re then conducted wit h the latter Sprengel-type eXMII plosi yes to determine thei r b r i sanc e and reliability ~ The results of these tests are shown in Table IX. Additional initiation data on cellulose ..Sprengel improvised caps is given in Table IV ..
explosi ve s with

Although these explosives are easy to prepare, there are a number of problems associated with their use and hand Ii ng, The nitric acid component will attack rn o st containers and it is usually necessary to protect surfaces with a coating of wax or acid- r e si stant ~" aint .. Alurninwn-cased p blasting caps resist the acid but wires and/ :'for fuze junctions must be protected. Copper .... cased caps (such as improvised devices) are rapidly corroded and acid protection is man .... ·utory. There is considerable acid fuming when these explosives are prepared and rrri.xtu r e should take plac e only in well ventilated reas or outdoors.

27

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o

c

0
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~

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C 000
+1"""1 +1""'1

.,l...)

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~ '*-" Q) ~

ro t"d nj. ro ro c~~~a o 000a
~

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+~

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+~

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4

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NNNNN ...........__ ...____ -.........
.........t:
.......-I
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-

.......

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~.

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(fJ

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I

-........... ............... .-t ~ ~ t

.,....._I;_.-.1;~~..-4

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rJ)

qJ ~

~,....I

c o

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ro .~
+".....

rct'U\j'1j~
•~

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00

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00

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00

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(i)

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............. ...____ -.............
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d)

Q _.(

m

...............
-~

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ill

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3; 3: ?; ~ ~ o0000
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28

'II

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1 ·1 :1
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:!

Here again, as with urea nitrate and nitrocellulose j the tradeoff of materials is poo r , The cellulose/acid system consumes an inordinate amount of nit ric acid that could be more effectively utilized in producing Ia rge quantities of explosive such a s the nitric esters. Thus J' the Sprengel explosi ve s offe r a.lternate systems that can be employed only where conditions warrant. Proc edure in the Appendix.
for prepa ration

of cellulose

I acid explosives

is given

Nitric

Acid/Monomirrobenzene

(ttHellhoffite

11) Explosives

A Sprengel explosive cornp ei sed of a mixture of mononitrobenzene and nitric acid has been pat ent ed ' and apparently used under the name of "Hellhoffite". The literature recommends an optimum mixture of 28 parts rnononitrobenzene to 72 parts strong nit ric acid. Little work was done with this mixture other than to check its general c ha r a ct e r i sties. In use J the mononitrobenzene is s irn ply poured into the acid and stirred. Attempts to absorb the mixture onto clean cotton or paper were defeated by violent reaction. Tests of mononit rohenzene with field grade nitric acid indicated that the materials were compatible. A 1-1/2 inch diarnete r by 6 inch length .. wax ... oated pipe "b ornb " was loaded with volwnetrically c mixed acid/ 'mononitrobenzene and initiated with a c ornrn e rcial No. 6 wax.-eco at ed electzic bla sting c ap. The bomb detonated high order" with an estiated strength equal to at least 500/0 nitroglycerin dynamite.

IV0"AWMV.·:.

As with other Sprengel explosives, "He Llhoffit e ' is extremely rosive and metal munitions components must be protected by or acid- resi sta.nt paint. The doubtful availability of mononitrozene on the field relegate s thi s explosive to the alte rnate choic e ~SS. Field technique for the manufacture of this explosive is sented in the Appe ndi.x,

29

F)A@MS!::::."",.e."''''''';:::.''''''''ii

-yyy"'''''''''''''"

'''y'.'nnnnn_.

__ ..._

.

CO~~CLUSIONS

AND

RECOMMENDATIONS

Prev-iously procedures were determined1,2 for field synthesis of three critical raw materials: potassiurn nitrate, sulfuric and nitric acids. Wi t h t h e s e rna t e r ia l s , a series of explosives, propellants, a nd n'l urii t.i on s capable of s ucce s s f'ul field i rn p r o vi sation were evol ve d ,

130tlndar-y pa r a.rn et e r s such as safety, reliability and availability of ingreclients and e q ui prn e nt rri u s t be considered ill any improvised unit i xpl si ve s Thus, I nv instances; tradeoffs are rn a nd at o r v , For this reaS011 we have wherever possible) offered alternate c h oi c e s to rn e n in the fi e Id , Ou r data indicates with reaSOllable certainty that c e rtain materials a n d procedures are superior to others", On this basis, we r e c orn rn e nd the following p r e fe r en ti a l lists:
m on sv e o systerr1~ n rn a

-,

.~'
-i:

;

,.

:ft
:~. :

(~.

::~:

?~ ...

a..

Irn p r ovi sed Propellant:

.jJ)

~':':'

1~
b,

Black Powder
sed Prirna
Ty

Im.provi 1.

Explosi v-es :

Mercury

Fulminate

z.
3..,

m1TD
1~Double·· Salts
Desel1sitized Sj l ve r s-F'ral.rrri na t e Caps: base charge)

4. c.

Improvi 1. 2~

sed Bla sting

Compound Straight

Caps (with high explosive Caps (no base charge)

d,

Improvised
1.
2~ 3.

Secondary
Nitrate

I-ligh Explosives

Methyl

Nit roglycol Nit roglyc e r i n

30

4. 5.

Nitric ACid/MonOnitrobe~.e~.ii!~t
Nitric ACid/Cellulose
Urea Nitrate
.
.::. ':::.-:,':

'~:.\::

.r·::.::)::.i;}:/~

There is no totally safe way to hnb.r'ov~:[:8::a1l::: With crude rnaterials and eqWp.tnent. Allf>;li_"..-.:.: ..... :...... ",:. Systems are inherently dangerous; all rnullt;.,~~. and common sense. However. With safety .a 'VVe have attempted to minimize risks by evol:T:~""
. .
'oMI::: ....Ii:&:JII ' .

safe or that give fair \\paming of impending .. ..... ... ~~ I!ri!i!i.w~~-lFtEi . :.~~.:::: of nitric esters. for exall'lPle. iB prOPosed in.. ~~""'I •.. :t"'AIi ties tl,1at offer clearly readable danger Sign8j~'
','

:

We have evolved m.ethods of tnanutact.u ~~""fIo..IIi.::.,::.~.j_ .... ..lllunitions for tnen who are aSBtUnedly in aht,IiiY':'__ dicarnent; men who are Without logistic BUPP9rt A...... ~. .iI,,:.:;.:... 'ed by hostile forces. SUch circumstances .ealcula ted 1" iaks .:. ;:,,:,;;;>.;.'1 .
""'l'-;::::IiII-. _

:::

prese"

1

.

"

': :

'.

. .::.:.:::,"

:

"

'.,

:

-:.:
".:= .. {
'. '

.

.

. .
=;(;::~': . ::~:
::;. '~:.\: .::

:":':.~.: :--:. ':';" ·.r··:·::.:.' .:". .:. ..(.:j '.:<":. ~
• .h •

<>: : . '

'

::::·;·:·i·.:.: ..:. '.':. :::.:~, ':::'. :

.::.

~"':.;.:'

::'.::-

: ~. ~:.
<

'.:.:':'.'~~" : :'.,:.:.:.~:':.:.':' :~.: ..
<

~.

'

..

. ~.".'.:.:::.:.·.~.::.: ...' . is.. .... : ~·;:.·
.
~:

:"=:"
'

'!:'
~:

? ,::
.::.
..:.

... :. .~::~.:

.
», ' ..•

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.. :

r:-:-·: \./

3)

...,'

.:

.

-

REFERENCES

1.

T. J. Hennessy t IIDeveloprn.ent of TechniqueS for Field Synthesio of potasSium Nitrate and Nitric Acid, II 1967, Frankford Arsenal. M67 -1 7 -1, Ammunition Development & Engineering Lab, Phila. , Pa. Special Products Laboratory, "Improvised Munitions Handbook, "

2..

Frankford

Arsenal,

Phila •• Pa. of Black Ammunition
De-

3.

T. J. Hennes sy t "Field Expedient Preparation powders, 111967, Frankford Arsenal,Mb7-16-l, veloplUent &. Engineering Lab, Phila. , Pa.
of powder

4.

T. L. Davis,

'IThe Chemistry

and Explosives,

I'

1943

John. Wiley and Sons, Inc., 5. 6. E. Howard, tlphil. Trans.

New York. Roy.

Soc.,"

204 (1800) 1815,

A. Nobel,
London.

'1A Treatise

on Blasting

Agents,

F. Soc. Arts

7.

Singer, Claredon

et a l , "A History PreSS,
II

of Technology,'1 Treastise

Vol V,

1958,

Oxford. A Practical on the Fabrication of

8.

G. Dussance,

Fulminating' 9. Theoretical

powders,

1864; Phila.

J. W. Mellor,

itA Comprehensive Treatise on Inorganic and Chemistry, Vol. vt , 1939, Longman '5 Green &<

Co •• New York,
10.

London. 1'M.odern InorganiC Green
&. Chemistry. New York. 40
t

J. W. Mellor~ 1939, Longman's

cs.,

I'

Revised

Ed. ,

11.

J. C. Phillip. "The Romanc e of Modern Chemi stry," 19 p. 2.00-202, CuriOUS Action of Carbides, J. B. Lippincott Phila. , Fa.
Federoff, et al , t1AManual 1946, Lefax., Phila. for Explosives , Pa , , Iden. Laboratories, P. H. 8.

Co.

l

12.

Vol IV,

32

13.

P, Naoum, ttNitroglycel'ine and Nitroglycerine Explosives, 1928, Williams and Wilkins cs., Baltimore, Md. A.. Nobel, IITri-Nitro-Glycerine. North and Adams, New York.
It

tI

14.

3rd Ed •• reWrittein,

1674

15.

U. S. Bureau of Mines, "The Behavior of NitrO ... lycerine, G Tech Paper 12, 1912, Washington, D. C.

II

33

APPENDIX Field Expedient Methods Explosive Preparation for

Section I No. JC
MERCURY

FULMINATE

Mere ury Ful minate ls used u a primary expJ.os 1ve in the fabrication of detonators (Secti on VI No ~ 13).. It is to be used with a booater explosive such as picric aetd (Section I" No" 21) or RDX (Section I~
t

NQ. 15)

l'

MATERIAL

REQmRED:

SOURCE!
I II

Nitric Actd, 90% cone. (1 ~48 sp .. gr.)
Mercury

Field

grade (Section I.. No 4) or induetrtal metal processors
4<

Tbermometezs

t:

merculY switches

I:

old radio tube,
Ethyl (grain) al coho] (90 %) Filtering material Paper towels

Teaspoon measure (1/4,
1 teaspoon

1/2. and

stainless Heat source Clean water

capac ity) - aluminum. steel or wu-coated

Clean wooden stick Glaas containers
Tape Syringe
PROCEDURE:

1 . Di 1ute 5 te as poon8 of nJ tri C AC id with 2-1/2; teaspoons of cleln water in a glas e contame r by adding the acid to the 1II&ter
-I

2.

Dissolve

1/8 teaspoon

of

mercury

ill the diluted nitric

acid.

This will yield dark red fumes"

-t

.......

Diluted

Nitric Acid
to the

N()TE: It may be necessary to add water one drop at a time. mer-cury-uctd solutton in order to start reaction ..

34

CA UTI ON; Acid will burn skin and des troy cl oth1ng • If any 18 spilled. was h it away with a la.rge quanUty of water ~ 00 not inhal e fumes ..

3 ~ Warm. 1() teaspoons of the alcohol in a container untll the alcohol feels warm to the 1n.e ide of the wrist.

Metal-Acid

4.

Pour the metal-acid solution into the warm. alcohol. Reaction sbould start in less than 5 minutes. Dense white fumes will be given off durin« reaction.. As time lapses" the fumes will become Iesa dease, Allow 10 to 15 m inure 8 to complete reaction .. Ful rninate will settle to bottom .

Solut!

CAUTION: This reaction generates large quantities of toxic fi&mm.ble fumes. The proces B must be conducted outdoors or in a well ventllat«l
t

are a, a.way from sparks

or open flames.

Do

oot inhale fumes.

.::..

.

/". Fil te r the sol uti on th rough B. paper to\\' el into a con tamer . Cr.ystala may stick to the side of the container. If 8 0 ~ tilt and a qui rt w ate r down the s1des of tbe conta i.ne r un til all the rna te rial coll ects on the fil te r
5.

paper.
Tape

35

6:0 Wash the crystals with 6 teaspoons of ethyl alcohol.

Tape

7.

Allow these mercury fulrntnate crystals

to air dry ~
Do not scrape or 0 r opea flames ~ Store in

CAUTI ON: Handle dry e xpI os ive with great care,

hand! e it roughly _ Keep away from sparks cool a dry place.

36

Section I

No~U
DOUBLE SALTS

Double Salts is used as a primary expl08i ve in the fabrication or detona tors (Section V I, No. 13\ It can be made iD the field from silver (CO ins). ni trlc acid, cal ct u m ca rbi de and water ..
+ t

Nitric acid (90% cone ..) (Section L No~ 4) Silver metal (silver coin. about 5/8 in diameter) Cttlcium carbide facetylene or calcium carbide lampe) Rubber and glass tubing (approxot 1/4 In. lna1de diameter)
Paper towels

Heat-resistant bottles or ceramic jug8~ 1 to 241art capacity J and one cork to fit (Puncb bole in cork to f:lt tubing ~)
to

Teaspoon (aluminum.
measure

sta1nJ.es.8 steel or WlUE-coated) or equtVlJent

01a:5 6 container
Heat source

Long narrow jar (oltve jar)

Tape Water
Alcohol
PROCEDURE!

1. Dilute 2...1/4- teaspoons of uStrtc acid with 1-1/2 teas peons oI watet in a glass container by addiDl the acid to the water ..

2... Dissolve a sUver coin {a silver dime) 11\ the dlIuted nitric acid. 8olutlon will tun to a green color .. NOTE~ It may be necessary dissolve the silver cotn. to warm the container to completely

The

37

····-__....~

.. II"'""-

CAUT10N~

Acid wiB burn skin and destroy clothing,

If any is spilled

t

wash it away with a large

quantity of water , Do not inhale fumes. Silver

~L Pour solution into a long narrow (olive} jar and place it in a bottle of hot water. Crystals will form in
the sol utlon
t

(

heat until crystal s di $Hot

solve. Water
:4 ~ While still heating and after crystals have drssolved, place 10 teaspoons 0 f cal ct u m earbt de in anothe r glas s bottle and add 1 teaspoon of water. Afte r the reacti on has sta rted add another teas poon of wate r ~
Then
$ et

up ass hown .

Oltve Jar With

Rubber Tubing

Silver Solution
Acetylene

Bubbles
Hent

Source
Water

Ca.lcium Carbide and
Water

---.....:----Ll~

Bubble acetylene through the solution tor 5 to 8 minutes ~ A brown v a.por will be g ive n off and whi te flakes wi 11 a ppear ill the :8 ilve r 801uti on • 5.

snver
Remove the stlver solution from the heat sou roe a nd allow it to cool .. Filter the solution through a paper towel into a glass container.. Green crystal s will collect on the paper ~
6.

Paper
Towel

38

7

I

Was h the 8011da cell ecte d on the

White Salida

paper towel with 12 teaspoons of alcohol The solid material will
r

turn white while the solvent in the container will have a green color.

_ ........ .___Green

Solvent
8~

Place the white solid material on • clean paper towel to air dry"

CAUTION ~ Handle dry explos ive with
1

great care ,

Do not

scra.pe or

handle it roughly ~ Keep away from sparks or open 11 &mes• StoN in cool dry_ place.

39

Section

r

No~ 11 HMTD

H~lTD is a primary explostve that can be made from hexamethylenetet ramtne , hydrogen peroxide and csrrtc acid. This explosive ts to be used with a booster explos tve such as picric acid (Section r No. 21) or RDX ~Section I, No. 15) in the fabrication of detonators (Section 6
I

t

No. 13).

MATERIAL

REQ.UIRE_Q:

SOURCES~

Hexamethy lenetetramtne

Hydrogen peroxide
Citric acid

under names of uroeropme, hexamin methenamlne , etc. A rmy heat tablets .. 6f]) hair bleach (or stronger if
t

Drugstores

possible) Drug store 8 0 r food store8
(I tSour

Salt'1

Containers, bottles or glasses Paper towels
Teaspoon Pan

~"ater Tape
PROCEDURE: ~ 1. Measure 9 teaspoons of

hydrogen
2.

peroxide into a container.

In 3 portions .. dissolve 2~ 1/2 te 3-5 poons 0 f cr us he d he xam ethy ...

Ieneterramine

in the peroxide.

Container

Cold water

3 ~ Ke(l:p the sol utton cool for 30 minutes by pl a cing contain€' r in. a

pan of cold water.

4.

In

j.

port ions , dissolve

4 -1 /2 teaspoons of crushed

citric acid in the

hex a m et h y j e ne te t r a 0\ ine- pe roxi de sol uti on .

40

--~~------

.

5.

Permit solution to stand at room tc mper-atur-e unt H solid pa r-

Uc les form at the bottom of con-

tainer. NOTE: Complete prectpltntron will take pt ace in 8 to 24 hours.

CAUTION:

At this point the mixture

is a prjma.ry

explostve

,

Keep

away Irorn flame.

F iller- the mixture through a paper towel into a container to collect the solid particles.
6+

Tape 7. Wash the solid parttcles collected in the paper towel with 6 teaspoons of water by pouring the water over the m , Discard the Hquid in the container ~
8.

Place these explosive

particles in a container

and allow to dry.

CAUTION:

Handle dry explosive

with

great

care , Do not

scrape

or

handle it roughly. cool .. dry place.

Keep away f r-orn sparks or open flames.

Store in

41

',Qg:!!!!~~; "

'."""""'h"."."'''''''''''''''''''''''''

.

SeeUon I

No. 13 UREA NITRATE EXPLOSIVE Urea nitrate can be used as an explosive munition. It Is euy to prepare from nitric acid and urine. It can be detonated with a blutlng
cap~

M~:I:ERIA .. REQ~JRE D!
~r

SOURCE~

Nitric acid. 90~ conc. ~1t48 ap. gr.)
Urine 2 one gallon heat and acid-

Field grade (Section I.. No or industrial metal

t

.)

rest stant containers clay, etc.)
Filtering material

(glass

t

Paper towel or finely textured cotton oloth (8hirt, sbeet etc.)
or Paint

II

AlumJnum. powder (optional if available)
Heat source

swres

Measuring containers (cup and
spoon) Water

Tape
Blastl ng cap Steel pipe and end cap (8) N(YfE!

Prepare

mixture JUlt before use.

PROCEDURE:

1.. Boll a large quantity of ut'lne (10 cups) to approximately 1/10 its volume (1 cup) in ODe of the containers over the heat source.

42

2 ~ FU te r the urine into the other containe r through the filtering material to remove impurities.

Filtering

Mate'rial

3 . Slowly add 1/3 cup of mule aci d to the ftlte red urine:., and let mixture stand for 1 hour ~

....-- Urine
CAUTION; .Acid will burn skin and destroy wash it away with a large quantity of water

FUtert:Jd

-clothing ~ If SJlY is ep.111ed ~ Do not lnhale fum.est

43

it

Q

XiX .......

»

...i

.hO

n

;an ..

Urea Nitrate Crystals
4 ~ Filter mixture as in step 2~ Urea nitrate crylJt8la will collect

on the paper.

5... Wash the urea nitrate by pour1.Dg

water over it"
allow

6. Remove urea nitrate crystals from the ftlterlng material ..

to dry thoroughly (approXimately
NO'tE: The dryinfl: t1me

16 bOUH) ..

can be reduced

boiling) water bath is \l8ed. HtJW" TO USE~
• I

to two hour8 If. bDf. (Dot See step 5 of BectlOD It No.. 15.

1. Spoon the

urea nitnte

ezysbl18 into an iron or &teel pipe wbidl has

an end cap threaded on one end.

BlastmK
Cap

2. Insert blasting cap Just beneath the surface of the urea nitrate crystals.

Urea Nitrate Crystals

44

· ..

.

,,,

_.

··_··'W.W"=h.h_.

_

This explosive can be made more effective by mix,"", with aluminum powder (can be obtained in paint stores) in the ratio of 4: to 1. For example, mix 1 cup of aluminum powder with ... cups of urea nitrate
NarES:

Confining the open end of the contalner will add to the effectiveness of the explosive.

45

....... - .._------------------_

_

_

_---------------------- -~-------.--

.

Section I
N04 OPT1\'llZED 11

PROCESS FOR CELLULOSE/ACID

EXPLOOrVES

acid and white paper or cotton cloth. This explosive can be detonated with a commere tal #-8 or any milita ry blasting cap.
An acid type explosive can be made from nitric I\o1 1 A EH.1AL
Nitric Acid

REQUl

RED.:

SOURCE:

Indu st rial metal proc es s ors 90% concentrated (apeci fie gravity of 1~48)
t

\\thi te unprt nted, unsized Clean white cotton cloth

paper

Acid reststant

container

Field grade {See Section I, No.4) Paper towels, napkins Cl othi ng, sheets, etc. Wax. coated pipe or cant ce ramie pipe, glass jar, etc,
Hcavy -walled glM.~ containers

Al um inurn foil or acid resistant

Food stores

material Protective gloves Blasting cap
Wax

~

PR()CEDURE:
1~

Put on gloves ~

24 Spread out a layer of pape r or cloth on aluminum foU and sprinkle wi.th nitric acid until thoroughly soaked.. If aluminum foll 16 unavailable to use an ac id resistant mater ial (glass Ii' ce ramie or wood') ...

:...

Aluminum

<,

Foil

46

IIImu

SIl!Ss.SS!!llSJ!!l!l!!tltlt.tt"ttt'-l!l!.M •.,UI.Il£.«JI!.!'¥h-""~¥h¥"'h.P"'.h.*.'£'£.hA"'JI!Il!!!I!.£.I!!!Il!!!£.£"'.£'£!!IIl£t.t

1!I!I!IJ!!!!!!!.1!!!'-!!x.x1l!!!lll.x.x~.x.iI!!!l!!!££

__

!I!I!I!I!I!I!I!,tI!!!!!!!E!!?'l!!!'l! ..:<&m&:I!!!'l!l":<;::~,

J","''''~''ok~okok~.;

~;"lmm"IIIITTIT"III~.".":~::I:~:::::~:::~~:::~~:~=:~~~.I.~~ ..=~ ~~~ ~

~

~

~

~

~

~

~

~

~

~. _ ..~ .

-=---=-""::._.h.h.h.h.h".'

.

CA UT ION ! Acid will burn s kin an d destroy clothing.. If any is apUled .. wash it away with a large quantity of water. Do not inhale fumes. 3 . Place another layer of paper or cloth on top of the aci d... oaked s sheet and re pe at step 2 above. Repeat as often as necess ary .

Rolled Sheets

4: •

Roll up the aluminum. foU containing the acid -soaked sheets and Inse rt the roll into the acid re sist-

ant container ..

/
t

Container

NOTE: If glaas , ceramic or wooden tray is used, pick up lheets with two wooden sticks and load into container
5. Wax blasting cap ..

6. lnse rt the bl aa:ting cap in the center of the rolled 8 heets . Allow 5 mj nutea before detonating the explos iVE~
r

47

Section I
No~ 10'

NITRIC

ACID/NITROBENZENE

(tIHELLHOFFITE-!t)

EXPLOSIVE

An explosive munition can be made from mononitrobenezene and nitric acid. It is a simple explosive to prepare .. Just pour the mononit r 000 nzene in to the ac id and :5 tir . MATERIAL Nitric acid
M on on irrobenzene

REQUIRED:

SOURCE: Fie1 d grade or 90% concentr ated (s peci!i c gravity of 1. 48) Drug sto re {oil of m i rbane) Chern leal supply house Industries {used as 801vent)

(also known

&8

nttroben zene)
A cid resistant measuring containers Actd resistant mixing rod BIas ti ng cap
Wax

Glass

I

clay to etc ..

Steel ptpe

l'

end cap and tape

Bottle or jar
NOTE: Prepare mixture just before use ...

PROCEDURE:

'<

,< <

,

1~ Add 1 volume (cup, quart, etc .. )

mononitrobenze ne to 2: vol umes nitric acid in bottle Or jar.

2~ Mix ingredi ents well by sti rri ng
with acid res'istant rod ..

48

CAUTION: Nitric acid wUl burn skill and destroy cloth.ing. $pilled~ wash off immediately with large amount of water.
benzene is toxic ~do not inhale fumes ~
HO'N TO USE:

If any Is Nit~

1• Wax blasting cap ~ pipe and end cap.

2. Thread end cap onto pipe ..

3.. Pou r mixture into pipe.

Pipe
4.. Insert and tape blasting cap just
beneath Burface of mixture.

MixtUre

...

NOTE~ Combining
of the explosive
r

the open end of the pipe will .tId to the .~.

'"

..
,,:

'

"

:..: ..
": ~~:

:..

,':

.
.. .. "!

::.'

.,

:t·,

.'.

. ...

.,

:-'

.

49

-,

::'.,:

.

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