systematic analysis of explosive residues.pdf

8/15/2019 Systematic Analysis of Explosive Residues.pdf

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A . D . B e v e r i d g e , P h . D . ; S . F . P a y t o n , ~ B . S c . ;

R . J . A u d e t t e , 2 P h . D . ; A . J . L a m b e r t u s , ~ B . S c . ; a n d

R . C . S h a d d i c k , ~ M . S c .

Sys t em at ic na lys is o f Exp los ive R e s idues

Examination of bomb scene evidence is an area o f increasing involvement for the

forensic scientist in which incidents may vary from student mischief to mass murder.

To undertake explosive casework responsibilities, the scientist must have personal

experience of the type of physical evidence left after explosions, including device re-

mains, characteristic damage, and chemical residues.

Recognition of device remains is aided by law enforcement agency publications [1-6].

Explosive damage to metal has been studied [7] and the significance of damage in bomb

incident investigations has been discussed in general terms [8]. Chemical residues may

contain unreacted explosive components

[ 9 - 1 3 ]

and also condensed reaction products

[12 14].

Solid products have been studied less than gaseous products, but have been

reviewed for black powder [14 15] and chlorate and perchlorate mixtures [16]. Smokeless

powders yield nitrites which form the basis of propellent powder pattern tests

[17 18].

Since solid reaction products from dynamite do no work, their chemical composition has

been deduced more from thermodynamic calculations than analysis [12 19].

Published methods for explosive residue analysis include microscopic examination for

unreacted explosive

[ 1 0 1 1 ]

chemical spot tests

[10 13 15 20 21]

thin-layer chromatog-

raphy TLC) [9 10 22 23] and infrared spectroscopy [24 25].

This study presents a scheme for systematic analysis of explosive residues isolated by

physical removal or solvent extraction. The techniques are a combination of infrared

spectroscopy, TLC, X-ray diffraction, emission spectrography, microscopy, and

chemical spot tests. Application to residue analysis is demonstrated by test explosions

using black powder, single- and double-base smokeless powder, chlorate/sugar,

dynamite, C4 plastic explosive, and PETN-based detonating cord a glossary of terms

is given in Appendix A).

xperimental

A n a l y s i s

The analytical scheme in Fig. 1 was applied to all of the explosives and their

residues. Figures 2 and 3 expand on the solvent extracts.

Received for publication 11 Nov. 1974; accepted for publication 23 Jan. 1975.

1Section Head, Chemistry Section, Royal Canadian Mounted Police, Crime Detection Labora-

tory, Edmonton, Alberta, Canada.

2Forensic Scientists, Chemistry Section, Royal Canadian Mounted Police, Crime Detection

Laboratory, Edmonton, Alta., Canada.

43

J Forensic Sci, Jul. 1975, Vol. 20, No. 3


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43

J O U R N A L F F O R E N S I C S C I E N C E S

CHE~ICAL~ESIDUE

UNREACTEDXPLOSIVE

IR

I

I

ETHER

R

I

TLC

DEBRS

I

STEREOMICROSCOPE

l

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ETC.

1

EXPLOSIVEWRAPPERS

ACETONE WATER~ INSOLUBLE

R

TLC POLARIZING ICROSCOPE

I

X-RAYIFF IR ES TLC SPOT ESTS

FIG. 1 G ener a l scheme or ana lys is o f exp los ive residues.

RNO

P l a s t i c i z e r

W a x

P e t r o l e u m

I

NaOHIGRIESS

G

EGND

ETHER

I

IR

TLC RNO 2

I NR4N03

CNS

Benzene /n -Hexane ( l : l ) P las t i c i ze r

o r

Xylene/n-He•

T i C 13 D M A B

TIIT

DNT

ACETONE

I

I R

F

i

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NG DNT

EGDN

Benzene/n-Hexa~e(1 : l )

o r Xy lene /n -Hexane {3 :2 )

[ - -

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NESSLERS

FIG.

2 A na l y s i s o f o rgan i c ex trac t s.

7

T L C

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CHCl3/Acetone

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I NaOH/ J

D i p h e n y l

GR~ESS

amine/H2S04 I

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o ~ p E T . I

RDX RDX

E x p l o s i v es a n d E x p l o s i o n s

T a b l e 1 s u m m a r i z e s t h e e x p l o s iv e s a n d c o n d i t i o n s u s e d i n th i s s tu d y . C h a r g e s w e r e

m a d e u p a n d in i ti a te d b y E x p l o s iv e O r d n a n c e D i s p o s a l E O D ) t r a in e d p e r s o n n e l u s i n g

s a f e t y f u s e , n o n e l e c tr i c b l a st in g c a p s , a n d d e t o n a t i n g c o r d b o o s t e r s a s r e q u ir e d . L o w

e x p l o s iv e s w e r e c o n f i n e d i n l / t i n , w a l l st e e l p i p e s w i t h th r e a d e d e n d c a p s . E x p l o s i v e

r e s i d u e r e c o v e r y p r o c e d u r e s w e r e c o n c e n t r a t e d o n r e c o g n i z a b l e d e v i c e r e m a i n s , t h e

c r a t e r , a n d a d j a c e n t s u r f a c e s .


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BEVERIDGE ET L ON EXPLOSIVE RESIDUES 4

I

I R

N O ~

SO ~

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I

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K

N a

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P O L A R I Z I N G M I C R O S C O P E

X - R A Y D I F F .

U N E X P L O D E D P R O D U C T S

N a N O K 2 S O

K N O N ~ 2 S O

N H 4 N O N a 2 C O

I N S O L U B L E

SPOT

T E S T S T L C

1

U L P

NH~

C I - E t O H

F I G 3 Analysis o f aqueous extracts.

1 E t O H

D I P N E N Y L - N E S S L E R S

A N N E I H 2 S O 4 R E A GE N T

[

o ~ N ~

Techniques

ln f ra red Spec t ro scopy- -A

P e r k i n E l m e r M o d e l 4 5 7 A i n f r a r e d s p e c t r o p h o t o m e t e r w a s

u s e d . E th e r a n d a c e to n e l i q u id e x t r a c t s we r e s a n d wic h e d b e twe e n 1 3 - m m KBr d i s k s

a n d r e c o v e r e d b y wa s h in g . S o l i d s we r e a n a ly z e d a s KBr p e l l e t s o r n o n d e s t r u c t i v e ly o n a

d i a m o n d c ell ( H i g h P r es s u r e D i a m o n d O p t i c s, M c L e a n , V a . ).

I n f r a r e d ( I R) a n a ly s i s m a y i d e n t i f y e x p lo s iv e c o m p o n e n t s [24 25] ino rgan ic ions [26] ,

a n d c o n t a m i n a n t s , a n d m a y a id T L C s e le c ti o n a n d i n te r p r e ta t i o n .

Th in -Layer Chroma tography- -TLC wa s r u n o n 0 .2 5 - m m , p r e c o a t e d s i l i c a g e l G g l a s s

p l a te s ( M a c k e r y - Na g e l a n d C o . , D u r e n , Ge r m a n y ) . P r i n c ip a l s o lv e n t s y s t e m s we r e

b e n z e n e [23] b e n z e n e / h e x a n e [10] x y l e n e / h e x a n e [10] e t h a n o l [ 9 ] , a n d c h l o r o f o r m /

a c e t o n e [ 9]. D e v e l o p e rs w e r e N a O H / G r i e s s r e a ge n t [23] t i t a n iu m t r i c h lo r id e /d im e th y l -

a m i n o b e n z a l d e h y d e ( T i C I ~ /D M A B ) [ 9] , d i p h e n y l a m i n e / H 2 S O , , a n d e t h a n o l / N e s s l e r

r e a g e n t . T h e d e v e lo p e r s a r e a p p l i e d a s f o l lo ws .

N a O H / G r i e s s : S p r a y w i t h 1 N N a O H , h o l d i n o v e n a t 1 0 0 ~ f o r 1 0 m i n , c o o l , a n d

s p r a y w i th Gr i e ss r e a g e n t ( 0 .2 5 s u l fa n i l ic a c id a n d 0 .1 a - n a p h th y l a m in e i n 1 :1

a q u e o u s a c e ti c a c id ) . R e d s p o t f o r E G D N , N G , N C , R D X , P E T N . H i g h c o n c e n t r a t i o n s

a p p e a r a s a y e l l o w s p o t w i th r e d e d g e s [ 9 ] . T NT g iv e s b r o wn s p o t s .

T i C l J D M A B : S p r a y w i t h 1 5 T i C I~ /H C 1 , a i r -d r y , a n d s p r a y w i th D M A B r e a g e n t

(1 g D M A B i n 30 m l E t O H , 3 m l H C 1 1 :1 9 , 18 0 m l B u O H ) . T N T a n d D N T g i v e y e l lo w

spots [9] .

P h 2 N H / H 2 S O , : S p r a y w i t h 1 P h 2 N H i n c o n c . H 2 S O , . B lu e s p o t f o r n i tr a te s .

E t O H / N e s s l e r : S p r a y w it h E t O H f o l lo w e d b y N e s s le r r e a g en t . O r a n g e s p o t f o r N H , §

X-Ray Powder Dif fraction--Eqtf lpment was a Ph il ips X-ra y genera to r (PW 1130 /00 /60)

w i t h a c o p p e r d i f f r a c t i o n t u b e ( T y p e R D 6 0 / 2 P W 2 1 0 3 / 0 0 ) , o p e r a t e d a t 5 0 m A ,

4 0 k V , w i th 1 0 t o 2 5 - m in e x p o s u r e . A n i c k e l fi l te r r e m o v e d C u K8 r a d i a t i o n . S a m p le s

we r e c o n t a in e d i n 0 .3 - m m c a p i l l a r i e s i n De b y e S c h e r r e r l 1 4 .8 - m m p o wd e r c a m e r a s .

I l f o r d I n d u s t r i al T y p e G X - r a y f i lm w a s u s e d.


4/24


5/24

BEVERIDGE ET AL ON EXPLOSIVE RESIDU ES 4 5

X- r a y p o wd e r d i f f r a c t i o n p e r m i t s n o n d e s t r u c t i v e i d e n t i f i c a t i o n o f c r y s t a l l i n e m a te r i a l s

b y c o m p a r i s o n t o s t a n d a r d s o r b y u s e o f t h e A m e r i c a n S o c i et y f o r T e s ti n g a n d

M a te r i a l s ( AS T M ) P o wd e r D i f f r a c t i o n F i l e [ 2 7 ] .

Emiss ion Spec trograph--Equipment wa s a J a r r e l l - As h 3 .4 - m E b e r t w i th d c a r c

exc i ta t ion a t 10 A fo r 10 s us ing a 10-/ Jm s li t. Sam ples we re con ta ined in 1A- in . ou ts ide

d i a m e te r c a r b o n c u p s . T h e e m i s s io n s p e c t r o g r a p h wa s e m p lo y e d t o i d e n t i f y e x p lo s iv e

m e ta l l i c c o n t e n t s u c h a s a lk a l i m e t a l s , m in e r a l c o n t a m in a n t s s u c h a s b o r o n i n Ch i l e

s a l t p e t e r , a n d m a n u f a c tu r e r a d d i t i v e s .

Polar iz ing M icroscope--E quipm ent w a s a L e i tz O r t h o p l a n m i c r o s c o p e e q u i p p e d w it h

a n i n t e r f e r e n c e we d g e ( L e i t z S - 1 0 0 ) a n d a M e t t l e r F P 5 - F P 5 2 h o t s t a g e . T h i s i n s t r u m e n t

p e r m i t s n o n d e s t r u c t i v e c l a s s i f i c a t i o n o f c r y s t a l l i n e m a te r i a l s b y m o r p h o lo g i c a l a n a ly s i s

[28]

a n d r e a d y i d e n t i f i c a t i o n o f i s o t r o p i c s u b s t a n c e s la y t h e Be c k e l in e t e c h n iq u e f o r

re f rac t ive index r iD.

Spo t Tes t s - -Spo t t e s t s we r e m a in ly t h o s e d e s c r ib e d b y Am a s a n d Ya l lo p [13 20].

Ch e m ic a l s p o t t e s t s we r e u s e d t o c h e c k c o m p o n e n t s s u c h a s NO~ - , wh ic h i n l o w y i e ld

( < 1 0~ m ig h t b e m i s s e d b y i n s t r u m e n ta l a n a ly s is , a n d f o r r a p id s c re e n in g o f a h ig h

y ie ld o f re s idue .

Resu l t s

T a b le s 2 , 3 , a n d 4 s u m m a r i z e t h e a n a ly s i s o f r e s id u e s f r o m th e e x p lo s iv e s l i s t e d i n

T a b l e 1 , b y u s e o f t h e s c h e m e in F ig . 1 .

i s c u s s i o n

L o w E xplosives

L o w e x p lo s iv e s c o n f in e d i n s t e e l p ip e s w i th t h r e a d e d e n d c a p s e x p lo d e d o n f l a m e

in i t ia t i o n . F ig u r e 4 il l us t ra t e s d a m a g e t o tw o s e ri es o f p ip e s b y c h a r g e s o f b l a c k p o w d e r ,

s i n g l e - b a s e s m o k e l e s s p o wd e r ( r i f l e p r o p e l l a n t ) , d o u b l e - b a s e s m o k e l e s s p o wd e r ( p i s t o l

p r o p e ll a n t) , a n d ( f o r c o m p a r i s o n ) d y n a m i t e . F r a g m e n t a t i o n b y c h l o r a t e / s u g a r w a s

s im i l a r t o s i n g l e - b a s e p o wd e r . T h e d e g r e e o f f r a g m e n ta t i o n i s s e e n t o b e m u c h h ig h e r f o r

d o u b le - b a s e p o w d e r t h a n f o r t h e o th e r l o w e x p lo s ive s .

T a b l e 2 s u m m a r i z e s t h e a n a ly s i s o f t h e l o w e x p lo s iv e s a n d t h e i r r e s id u e s u s in g t h e

scheme in F ig . 1 .

B la c k p o wd e r g a v e p ip e f r a g m e n t s w i th f r e s h r u s ty a r e a s a n d a h ig h y i e ld o f

g r a y i s h re s id u e . Un r e a c t e d g r a n u l e s we r e c o m m o n ly r e c o v e r e d i n p ip e th r e a d s a n d s o m e -

t im e s i n t h e b o d y o f t h e p ip e . T h e s u r r o u n d in g s w e r e u su a l l y b l a c k e n e d . F ig u r e 5 s h o ws

th e e f f e c t o f a 0 .7 5 - 1 b c h a r g e i n a c o r n e r o f a 9 b y 1 2 - f t r o o m . P ip e f r a g m e n t s a r e

s h o w n i n th e b o t t o m r o w o f F i g. 4 . A n a l y s i s o f d e b r is f r o m t h is e x p l o s io n is s u m m a r i z e d

in T a b l e 2 , No . 4 . T h io c y a n a t e w a s id e n t i f ie d b y 1 R s p e c t r o s c o p y i n a n a c e to n e e x t r a c t .

B l a c k p o wd e r r e s id u e c o n s i s t e d p r im a r i l y o f p o t a s s iu m s u l f a t e i d e n t i f i e d b y X- r a y

p o w d e r d i f f r a c t i o n . A n 1 R s p e c t r u m o f t y p i c a l r e s id u e ( F ig . 6 ) s h o w e d s t r o n g s u l f a t e a n d

we a k n i t r a t e . W e a k c a r b o n a t e p e a k s a n d a b s e n c e o f n i tr a t e p e a k s we r e a l s o o b s e r v e d i n

d i f f e r e n t e x p lo s io n s ; t h a t i s , c o m p o s i t i o n a n d d i s t r i b u t i o n o f e x p lo s iv e r e s id u e wa s n o t

u n i f o r m . R e v i e w s [14 15] s u g g e st a h ig h e r p e r c e n t a g e o f p o t a s s iu m c a r b o n a t e , b u t s i n c e

i t wa s n o t o b s e r v e d i n X- r a y p o w d e r d i f f r a c t i o n p a t t e r n s , t h is i n d i c a te s t h a t i ts y i e ld is

le ss t h a n 1 0 . T h e s a f e ty f u s e a l s o g a v e p o t a s s iu m s u l f a t e as p ri n c ip a l re s id u e f r o m th e

b l a c k p o w d e r c o r e .

T h e v a lu e o f p r o d u c t i d e n t i f i c a t io n i s il l u s tr a t e d i n T a b l e 2 , N o . 3 , s in c e if th e f e w


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BEVERIDGE ET AL ON EXPLOSIVE RESIDUES 4 4

FIG. 5 Black powder pipe bomb debris.

granules of unreacted black powder had no t been recognized then identi fication of the

explosive would have to have been based on the reaction product only.

The single-base smokeless powder consisted of NC cylinders coated with graphite and

DNT to control burning. It also contained a small amount of potassium sulfate additive.

Numbers 5 through 7 in Table 2 summarize the analyses. Figure 7 illustrates the effect

of a cap-initiated pipe bom b in a room corner. No wall push was observed unreacted

explosive was thrown aro und the room and a devastating fire was started within the

wall.

The double-base smokeless powder consisted of graphite-coated NG and NC plus a

small amount of potassium sulfate additive. Numbers 8 and 9 in Table 2 summarize the

analyses. A flame-in itiated 0.5-1b charge in a room showed wall push blew out the

windows but left intact a light bulb in the ceiling. Of twelve fragments recovered from

the crater and walls five bore unreacted explosive. All fragments showed fresh rusty

areas and traces of resinous residue. NG and NC were identified by IR and TLC.

Aqueous extraction gave a low yield of con taminants in which sulfate was identified by


12/24

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13/24

BEVERIDGE ET AL ON EXPLOSIVE RESID UES 4 4

FIG.

7 Single base smokeless powder pipe bomb debris.

IR and sodium by spect rography. Spot tes ts showed ni tra te ni tr ite amm onium and

chloride. The X-ray powder pat tern was not identif ied. The danger of rel iance on

chemical tests is apparent since if analysis consisted only of TLC and of spot tests for

sodium ni tra te and amm onium then in the absence of unreacted explos ive the

examiner could be misled tow ard dynam ite; that is the analysis wou ld appear to be NG

NC NH § Na and NO3- of which three are the resul t of contam inat ion f rom the

surround ings. The range o f instrumental analysis applied in Fig. 1 should p revent this

type of error since all dyna mite aque ous extracts were identif ied by X-ray powde r

diffract ion.

Chlorate/sugar produced a f i rebal l and explosion on f lame ini t iat ion. Unreacted

explosive was recovered. Pipe fragments bore brown gummy residue and fresh rust

spots. Analyses are summarized in Table 2 Nos. 10 and 11. Extract ion yielded

unreacted sugar and sodium chlora te ident if ied by IR and the sodium chlor ide product

ident i f ied by polar iz ing microscopy and X-ray powder di f f ract ion. S ince sodium

chlorate is also isotropic the polarizing micr oscop e was well sui ted to this analysis.

Potassium chlorate is anisotrooic.


14/24

JOURNALOF FORENSIC SCIENCES

Hi g h Ex p l o s i v e s

D y n a m i t e - - D y n a m i t e i s t h e e x p l o si v e c la s s m o s t c o m m o n l y e n c o u n t e r e d i n b o m b

i n c i d e n t s . T h e c l a s s es o f d y n a m i t e u s e d i n th i s s t u d y w e r e g e l a t in ( N G , N C ) , a m m o n i a

( N G , N H , N O 3 ) , a n d a m m o n i a g e l a ti n ( N G , N C , N H , N O 3 ) . I n o u r s e rv ic e a r e a a n d e l se -

w h e r e , n i t r o g l y c e r i n e d y n a m i t e s c o n t a i n u p t o 85o7o e t h y l e n e g l y c o l d i n i t r a t e ( E G D N )

w i t h th e n i t r o g l y c e r in e . T h e E G D N d e p r e s s e s t h e f r e e z i n g p o i n t o f t h e N G , w h i c h le s s e n s

t h e ri s k o f d y n a m i t e b e c o m i n g u n s ta b l e t h r o u g h f re e z in g a n d t h a w i n g . T h e E G D N is

m o r e v o l a t il e t h a n N G a n d i s t h e ba s is o f d y n a m i t e s n i f f e rs [1 10]. T h e d y n a m i t e i n

t h i s s t u d y c o n t a i n e d s o d i u m n i t r a t e a n d s u l f u r f o r o x y g e n b a l a n c e , e x c e p t f o r t h e

g e l a t i n w h i c h d i d n o t c o n t a i n e l e m e n t a l s u l f u r . N o n e o f th e s e d y n a m i t e s c o n t a i n e d D N T ,

b u t i t i s a c o m m o n a d d i t i v e .

C o o k

[12]

p r e d i c t s t h a t d y n a m i t e w i t h s o d i u m n i t r a t e s h o u l d y i e l d s o d i u m c a r b o n a t e

a n d t h a t i n t h e p r e s e n c e o f s u l f u r , c o p r o d u c t s m a y i n c l u d e s o d i u m s u l f i d e , s u l f i t e , a n d

s u l f a t e , d e p e n d i n g o n t h e o x y g e n b a l a n c e . F o r t h e a m m o n i a g e l a t i n s , c a l c u l a t e d

p r o d u c t s a r e p r i m a r i l y s o d i u m s u l f a t e a n d s o d i u m c a r b o n a t e i n a ra t i o i n w h i c h th e

s o d i u m c a r b o n a t e p e r c e n t a g e i n c r e a s e s a s t h e e x p l o s i v e p e r c e n t a g e s t r e n g t h d e c r e a s es [19].

T h e s e d a t a p o i n t t o T L C a n d X - r a y d i f f r a c t i o n a s p r i m e i d e n t i f ic a t i o n t e c h n iq u e s .

F o l l o w i n g t h e T L C w o r k o f J e n k i n s a n d Y a l l o p [ 9] , t h is s t u d y c o m m e n c e d w i th b e n z e n e

e l u en t , b u t th i s d id n o t c l e a n ly s e p a r a t e E G D N a n d N G . G o o d s e p a r a t i o n w a s ac h i e ve d

b y b e n z e n e / h e x a n e e l u e n t [29] a n d t h i s s y s te m s u p e r s e d e d b e n z e n e .

T h e r e s u l ts o f a c o m p a r a t i v e s t u d y o f T L C s o l v e n t s y s te m s o n 2 5 0 - ~ m s i l ic a g e l G

p l a t e s a r e s h o w n i n T a b l e 5 .

R f

v a l u e s a r e s i m i l a r t o t h o s e r e p o r t e d b y J e n k i n s a n d

Y a l l o p [9 ] o n 2 5 0 -/a m s i l i c a g e l G , b u t a r e a b o u t t w o t i m e s l e ss t h a n R f v a l ue s r e p o r t e d

b y H o f f m a n n a n d B y a ll [10] o n 2 00 -/a m s i l i c a g e l G . T h i s d i s c r e p a n c y i s p r e s u m a b l y d u e

t o t h e d i f f e r e n c e in t h i c k n e s s o f t h e s i l i c a g e l l a y e r a n d u n d e r l i n e s t h e n e c e s s i ty f o r

r u n n i n g f r e s h s ta n d a r d s w i t h e v e ry T L C . T a b l e 5 in d i c at e s t h a t c h l o r o f o r m / a c e t o n e

( 1 / 1 ) i s t h e b e s t s y s te m f o r in i ti a l T L C a n a ly s i s o f a n u n k n o w n . A m m o n i u m a n d n i t ra t e

T A B L E 5- -T L C systems em ployed fo r explosive analysis.

TLC Systems

Benzene: Xylene: CC I,: Aceto ne:

Hexane Hexane C2H4C 12 CHCL

Explosive Benzene 1 1 3:2 4:1 1 1 Eth ano l

EG DN a 0.23 0.31 0.23

NG a 0.38 0.17 0.21 0.16 0.65 0.64

NC a 0 0 0 0 0 0

PE TN a 0.37 0.15 0.21 0.12 0.71 0.60

RDX a 0 0 0 0 0.46 0.49

DN T b 0.37 0.17 0.22 0.20 0.63 0.65

TN T b 0.40 0.20 0.30 0.15 0.67 0.61

NO3 - c . 0.57

N H + d 0 .1 3

a NaO H/G riess , 250-~m sil ica gel G.

b TiC IJD M A B, 250-~tm sil ica gel G.

c Ph2N H/H~ SO,, 250-1~m sitica gel G.

dE tOH /N ess ler , 250-:~m silica gel G.

* NaNO 3, K NO~, NH~NO~.


15/24

BEVERIDGE ET AL ON EXPLOSIVE RE SIDU ES 5

i o n s m i g r a t e a t d i f f e r e n t r a t e s a n d s o d i u m , p o t a s s i u m , a n d a m m o n i u m n i t r a t e s a r e n o t

d i s t i n g u i s h a b l e b y d e v e lo p in g n i t r a t e o n ly . T h i s h a s b e e n o v e r lo o k e d i n p r e v io u s

p u b l i c a t i o n s o n e x p l o s i v e r e s i d u e a n a l y s i s . A m m o n i u m i o n w a s c o n v e n i e n t l y d e v e l o p e d

u s in g t h e N e s s l er r e a g e n t [13].

T h u s , t o c h a r a ct e r iz e d y n a m i t e b y T L C , a m i n i m u m o f t h re e s y s te m s w a s e m p l o y e d :

b e n z e n e / h e x a n e w i t h N a O H / G r i e s s f o r E G D N , N G , a n d N C ; e t h a n o l w i th P h 2 N H /

H ~ S O , f o r N O 3 - ; a n d e t h a n o l/ N e s s le r f o r N H , + .

T a b l e 3 s u m m a r i z e s t h e r e s u l t s o f 1 8 d y n a m i t e e x p lo s io n s . U n le s s o th e r w i s e n o t e d ,

t h e c h a r g e w a s o n e 8 b y 1 8 8 s t ic k . T h e r e su l t s a r e d is c u s s e d b y c l as s .

A m m o n i a D y n a m i t e E x p l o si o n s w e r e c o n d u c t e d w i th o n e 8 b y 1 8 8 s ti c k o n w o o d

a n d o n e d e t e r i o r a t e d 8 b y 1 8 8 s t i c k o n st ee l. T h e r e su l t s a r e s u m m a r i z e d i n T a b l e 3 ,

N o s . 1 3 a n d 1 4, a n d c l e a r l y d e m o n s t r a t e t h e c o m p le x i t y o f e x p lo s iv e r e s id u e a n a ly si s .

I n b o th c a s e s a w h i t e c r y s t a l l i n e r e s id u e w a s o b s e r v e d , b u t t h i s w a s n o t r e c o g n i z a b l e a s

u n r e a c t e d d y n a m i t e . A c e t o n e e x t r a c t i o n a n d T L C i d e n t i f i e d N G i n t h e w o o d c r a t e r

f r a g m e n t s b u t n e i t h e r o n t h e w o o d c r a t e r s u r r o u n d i n g s n o r o n t h e s t e e l . A q u e o u s

e x t r a c t i o n y i e ld e d w h i t e c r y s t a l s , t h e I R s p e c t r u m o f w h ic h s h o w e d th e p r e s e n c e o f

s u l fa t e a n d c a r b o n a t e p r o d u c t s i n a d d i t io n t o u n r e a c t e d n i t r at e . T h e r e la t iv e p r o p o r t i o n s

in t h e I R v a r i e d a s s h o w n b e lo w , w h e r e s i s s t r o n g , w i s w e a k , a n d m i s m e d iu m .

w o o d c r a t e r f r a g m e n t s 8042- S) C O 3 2 - ( w ) N O 3 - ( w )

w o o d c r a t e r s u r r o u n d i n g s S O , 2 - ( m ) C O 3 2 - ( w ) N O 3 - ( s )

s te el S O , 2 - ( s ) C O 3 2 - ( m ) N O 3 - ( m )

X - r a y p o w d e r d i f f r a c t i o n o f t h e m i x t u r e [30] i d e n t i f i e d t h e p r o d u c t f r o m t h e w o o d a s

N a ~ S O , ( I ) a n d t h a t f r o m s t e e l a s s o d iu m c a r b o n a t e s u l f a t e ( s e e T a b l e 6 ) . T h e I R

s p e c t r u m o f s o d iu m c a r b o n a t e s u l f a t e i s i l l u s t r a t e d i n F ig . 8 ( s t e e l r e s id u e ) a n d t h e

m o r p h o l o g y i n F ig . 9 . T h e s e p r o d u c t s a r e f u r t h e r d i sc u s se d i n A p p e n d i x B . T h e n i t ra t e

in e a c h c a s e w a s i d e n t if i e d a s t h e u n r e a c t e d s o d iu m s a l t b y X - r a y p o w d e r d i f f r a c t i o n

a n d t h e p o l a r i z i n g m i c r o s c o p e . N o a m m o n i u m i o n w a s f o u n d i n t h e w o o d d e b r i s a n d

was no ted on ly by spo t te s t sc reen ing in the s tee l ex t rac t .

T h a t t h e s a m e e x p lo s iv e g iv e s d i f f e r e n t p r o d u c t s o n u n c o n f in e d d e to n a t i o n i s b e s t

e x p l a i n e d b y t h e d e t e r i o r a t i o n o f o n e s t i c k . T h e p r o d u c t c o m p o s i t i o n i s a p p a r e n t l y

d e t e r m i n e d b y t h e m o l e r a t io o f C O 3 2 - : S O , 2 - . T h e s e r e s ul ts s h o w t h e m a j o r d r a w b a c k

t o s o l v e n t e x t r a c t i o n i n t h a t s o d i u m s u l f a t e a n d s o d i u m c a r b o n a t e m i g h t h a v e b e e n

p r e s e n t i n d e p e n d e n t ly , b u t a r e i s o l a t e d f r o m a c o m p le x a q u e o u s s y s t e m a s a s o l i d

s o lu t i o n ( s e e A p p e n d ix B) .

Am mo nia Gelat in Dyn am i te The v e lo c i t y o f 4 0~ F o r c i t e i s a r o u n d 7 0 0 0 f e e t p e r

s e c o n d ( f p s ) u n c o n f in e d a n d 1 3 ,0 0 0 f p s c o n f in e d . V e lo c i t i e s a r e p r o p o r t i o n a t e ly h ig h e r

f o r 6 0 ~ a n d 7 50 70 . T h e v a r i a t i o n o f v e lo c i t y w i th c o n f in e m e n t i s t y p i c a l o f g e l a t in

d y n a m i t e s [31]. F ig u r e 1 0 s h o w s t h e i n c r ea s e d s h a t t e r i n g e f f e c t o f a n 8 b y 1 8 8 s t ic k

o f ex p lo s iv e o n 9 0 p ly w o o d a s t h e v e lo c i t y i n c r ea s e s f r o m 6 0 0 0 t o 2 5 ,0 0 0 f p s . T h e

exp los ives il lu s t ra ted w ere 20 , 40 , and 60070 dyn am i te , and C4 , respec t ive ly (Tab le 3 ,

N o s . 1 3, 1 7 , 2 6 ; T a b l e 4 , N o . 3 4 ) . T e s ts i n re s id e n ti a l p r e m i s e s s h o w e d a m a r k e d c o n t r a s t

t o t h e l o w e x p lo s iv e s . W a l l s w e r e s h a t t e r e d , a s o p p o s e d t o p u s h e d , a n d t h e r e v e r s e b l a s t

b r o u g h t w i n d o w g la s s b a c k i n t o t h e r o o m s . F i g u re 11 sh o w s d a m a g e c a u s e d b y t w o

s t ic k s o f u n c o n f in e d 4 00 70 F o r c i t e i n a 9 b y 1 2 - f t r o o m ( T a b l e 3 , N o . 2 2 ) . W h e n

c o n f in e d i n p ip e s , s o m e p ip e f r a g m e n t s p a s s e d t h r o u g h s e v e r a l w a i l s a n d d o o r s .


16/24

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17/24

BEVERIDGE ET AL ON EXPLOSIVE RESIDUES 7

FIG.

9--S odi um carbonate sulfa te in aqueous extrac t o f explosive residue (crossed polars,

original magnification x25 0).

FIG. lO--Damage by a unit charge o f 20, 40, and 60 dynam ite and C4.

Numbers 16 through 30 in Table 3 summarize the test explosions of this class. In

only three instances Nos. 18, 20, 26) was unreacted explosive recognized in the debris.

The confined explosives, Nos. 23 through 25, were distinguished from the unconfined

explosives by the composition of the reaction product as determined by X-ray powder

diffraction. The confined explosives gave sodium carbonate sulfate, whereas the uncon-

fined gave Na~SO, I). Unlike 20070 stumping powder, unconfined Forcite residue


18/24

8

JO U R N L O F FO R EN SIC SC IEN C ES

TABLE

6--X-ray pow der d iffraction data o f sodium carbonate sulfates.

Na2SO,(I) a

d .~ I/Io

2Na2SO, 9Na2CO3 b 2Na2SO,9Na2CO3 c (Na2SO,)I_ n(Na2CO3)n d

d A I/Io d A I/Io d A I/Io

4.60 10 4.60 20

3.87 63 3.85 90

3.56 40 3.55 70

3.88

3.78

3.51

2.82 100 2.80 100 2.78

2.66 100 2.66 100 2.64

2.58

2.30 2 2.30 10

2.19 8 2.18 50

2.13 1

1 9 3 4 0 1 9 2 9 0

1 78 8 1 77 50

1 5 7 1 0 1 5 6 4 0

1 5 4 7 1 5 3 2 0

9.20 10

4.51 20

70

80 3.798 70

70 3.530 50

3.444 10

3.076 20

100 2.795 100

70 2.645 60

80 2.587 60

2.479 5

2.348 10

2.302 5

2.13 30 2.149 20

2.10 30 2.106 1

1.97 10 1.980 10

1.93 40 1.932 30

1.89 40 1.903 30

1.75 30 1.765 20

1.740 5

1 6 2 5

1 5 0

10

a ASTM Powder Diffraction File No. 1-0990 [27].

b Ramsdell

[33].

c ASTM Powder Diffraction File No. 2-0840 [27].

dThis study.

showed no carbonat e in the IR (Fig. 1 2). The presence of some carbona te was

inferred, however, fr om effervescence with acid. There was insufficient sodium nitrate

in the confined explosive residue for identification in the X-ray powder pattern, but it

was recognizable in the bulk sodium carbonate sulphate matrix by orthoscopic and

conoscopic observation with the polarizing microscope (Nos. 23 and 24).

Sodium nitrate was identified by X-ray powder diffraction in all unconfined explosions

and NG was identified by TLC in approximately three-quarters of the explosions.

However, ammonium nitrate and NC were detected in only 47 and 40% of the tests,

respectively. In the TLC systems tested, N C h ad an Ry value of 0, in com mon with many

solvent-extracted contaminants which often develop a yellow color with Griess reagent

and possibly mask NC. Where a TLC system was used which separates EGDN and NG,

(Nos. 17, 18, 22 through 28, 30) EGDN was found in only one-third of the cases in

which NG was identified. This cautions against complete reliance on a dynamite sniffer

to detect residue.

IR prior to TLC of ether and acetone extracts detected explosive components in 50%

of the tests, as opposed to 80% for TLC. In some TLC analyses, contamination reduced

the

R f

value of explosive compon ents relative to standards, and in these cases IR aided

interpretation.


19/24

BEVERtDGE ET AL ON EXPLOSIVE RESID UES 9

FIG. 11--40

Forcite debris two sticks, unconfined).

No consistent difference in residue composition was found between Forcite 40, 60, or

75070, notwithstanding their calculated products being in varying proportions. The

complexity of the Na2SO4/Na2CO3 aqueous system complicates this issue. For 60 and

7507o Forcite the yield of sulfate product was minor compared to sodium nitrate, but

as No. 16 shows, this is not a consistent difference from 4007o Forcite .

Explosions of 7507o Forcite with and without wrapper paper (Nos. 29 and 30) showed

little difference in products, although CNS- was detected with paper only. CNS- was

also a product of black powder (No. 4), 20070 dynamite (No. 14), and 6007o Forcite (No.

28).

The effect of contamination was not serious, although sodium chloride of unknown

origin was often noted. Gypsum plaster in particular was noted in some X-ray powder

patterns but did not prevent identification of product sulfate in No. 28. Figure 13 shows

the IR spectrum of the aqueous extract from No. 27, 60~ Forcite on gypsum wall-

board, in which sulfate product is identified by a peak at 615 cm -l . Its low yield

precluded further identification from the X-ray powder pattern.

In summary, out of 15 explosions of ammonia-gelatin dynamite, 5 residues could be

classed as being from ammonia-gelatin dynamite (Nos. 18, 20, 26 through 28), 2 from

ammonia dynamite (Nos. 22, 29), 1 from gelatin dynamite (No. 17) , and 7 from

dynamite (Nos. 16, 19, 21, 23-25, 30).

G e l a t i n - - O n e pound of a 5-1b stick o f seismic dynamite was shaped and detonated


20/24

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21/24

BEVERIDGE ET L ON EXPLOSIVE RESIDUES 45

o n s tee l Tab le 3 , No . 32) . A h eav y wh i te c rys ta l l ine res idue was la rge ly sod ium

carbona te . Th is res idue cou ld no t be c lassed as be ing f rom ge la t in dynami te s ince NC was

n o t r e c o v e r e d , b u t t h e i d e n t i f i c a t i o n o f s o d i u m c a r b o n a t e i n d i c a t e s t h a t t h e d y n a m i t e

c o n t a in e d n o e l e m e n ta l s u l f u r a n d a g a in s t re s se s t h e v a lu e o f p r o d u c t i d e n t i f i c a t io n b y

in s t r u m e n ta l a n a ly s i s . T h e p r e s e n c e o f b a r i u m wa s s h o wn s p e c t r o g r a p h i c a l l y i n t h e

in s o lu b l e m a te r i a l , wh ic h e m p h a s i z e s t h e v a lu e o f s y s t e m a t i c a n a ly s i s.

Plas t ic C 4 - - T h e v e l o ci t y o f C 4 is a r o u n d 2 5 ,0 0 0 f p s. C 4 w a s d e t o n a t e d b y e i th e r

b l a s t i n g c a p o r d e to n a t i n g c o r d b o o s t e r . No u n r e a c t e d e x p lo s iv e wa s o b s e r v e d i n t h e

c h a r a c t e r i s t i c b l a c k d e p o s i t . T h e a n a ly s e s a r e s u m m a r i z e d i n T a b l e 4 , No s . 3 4 t o 3 6 . I n

o n l y o n e o u t o f t h r e e ex p l o si o n s N o . 3 6 ) w a s R D X i d e n ti f ie d b y T L C . O n o n e p i e ce

o f d e b r is , P E T N f r o m d e t o n a t i n g c o r d b o o s t e r w a s a ls o i de n ti fi e d.

D e t o n a t i n g C o r d T h e

d e t o n a t i n g c o r d w a s c h a r g e d w i th P E T N . I n o n e o f tw o

e x p lo s io n s T a b l e 4 , No s . 3 8 a n d 3 9 ) P E T N wa s i d e n t if i e d b y T L C. I n b o th c a s e s

t r a c e s o f wr a p p e r we r e r e c o v e r e d .

General

T h e a n a ly t i c a l s c h e m e in F ig . 1 wa s d e r iv e d f r o m p r a c t i c a l e x p e r i en c e a n d t h e c h e m ic a l

l i te r a tu r e a n d u s e s t h e i n s t ru m e n t s r o u t i n e ly u s ed i n Ro y a l Ca n a d i a n M o u n te d

P o l i c e R C M P ) l a b o r a t o ri e s . I t is n o t a n a b s o l u t e a n d i s a d a p t e d a s c o n d i t io n s d e m a n d .

F o r e x a m p le , e t h e r wo u ld n o t b e u s e d t o e x t r a c t r e s id u e f r o m a n e n g in e b lo c k . S im i l a r l y ,

i f v o l a t il e l iq u id s s u c h a s n i t r o b e n z e n e o r g a s o l i n e we r e s u s p e c te d , t h e n h ig h v a c u u m

t e c h n iq u e s , v a p o r p h a s e I R , a n d g a s c h r o m a t o g r a p h y w o u l d b e a p p li e d . T h e t e s t

e x p l os i o ns w e r e p a r t o f a s e rie s o f w o r k s h o p s e m i n a rs r u n b y o u r l a b o r a t o r y f o r

t r a in in g p u r p o s e s , a n d i n v o lv e d p o l ic e a n d f i re i n v e s ti g a to r s a n d I E D s p e ci a li s ts i n

a d d i t i o n t o l a b o r a t o r y p e r s o n n e l .

T h e a n a ly t i c a l r e s u l t s s h o w th a t t h e s c h e m e p e r m i t t e d c o r r e c t c l a s s i f i c a t i o n o f t h e

e x p lo s iv e s , a l t h o u g h s u b c l a s s i f i c a t i o n o f d y n a m i t e wa s n o t a lwa y s a c h i e v e d . Un r e a c t e d

e x p lo s iv e i n d e b r i s wa s r e c o g n i z e d b y m ic r o s c o p i c e x a m in a t i o n f o r m o s t o f t h e l o w

e x p los iv es , f e w o f t h e d y n a m i t e s , a n d n o n e o f t h e p l a s ti c e x p lo s ive s . T h e v a lu e

o f e x p lo s iv e p r o d u c t i d e n t i fi c a ti o n h a s b e e n d e m o n s t r a t e d a n d w i t hi n t h e a m m o n i a -

g e l a t i n s e r i e s i t d i s t i n g u i s h e d c o n f in e d a n d u n c o n f in e d d y n a m i t e . Re s id u e c o m p o s i t i o n

a n d d i s t r i b u t i o n w e r e n o t u n i f o r m a n d t h e m o s t c o m p r e h e n s i v e r e c o v e r i e s w e r e , n o t

s u r p r i s i n g ly , m a d e f r o m th e c r a t e r a r e a , wh ic h r e c e iv e s a p o t e n t i a l h e m i s p h e r e o f b l a s t .

T h e m o s t u se f u l te c h n i q u e s w e re m i c r o s c o p y , T L C , X - r a y p o w d e r d i f f r a c t io n , a n d

in f r a r e d s p e c t r o s c o p y . T h e e m i s s io n s p e c t r o g r a p h r e p l a c e d s p o t t e s t s f o r m e ta l s . S p o t

t e s ts p r o v id e d r a p id s c r e e n in g o f a h ig h y i e ld o f r e s id u e , b u t w e r e u s u a l l y re l e g a t e d t o

c h e c k in g f o r c o m p o n e n t s m i s s e d b y t h e o th e r t e c h n iq u e s . A n e g a t iv e s p o t t e s t wa s o f t e n

g iv e n m o r e we ig h t t h a n a p o s i t i v e t e s t . Ho we v e r , a s p o t t e s t s o lu t i o n a s a T L C d e v e lo p e r

wa s v e r y u s e f u l a n d g r e a t l y e n h a n c e d s p e c if i ci t y .

C a l c i u m s u l f a te b u i ld i n g p r o d u c t s , a m m o n i u m c h l o ri d e f r o m b a t te r ie s , s o d i u m

c h l o r id e o f u n k n o w n o r i g in , a n d r e si ns w e r e th e c o n t a m i n a n t s m o s t o f t e n e n c o u n t e r e d

b y s o lv e n t e x t r a c t i o n , b u t t h e y d id n o t p r e c lu d e r e s id u e i d e n t i f i c a t i o n i n t h e t e s t

series.

T a b l e 7 s u m m a r i z e s t h e c o m p o n e n t s i d e n t i f i e d i n t h i s s t u d y a n d i l l u s t r a t e s h o w

r e s u l t s m a y b e i n t e r p r e t e d i n a n a l y s i s o f a n u n k n o w n . T h e s c h e m e h a s b e e n

r o u t i n e ly a p p l i e d t o c a s e wo r k w i th s a t i s f a c to r y r e s u l t s ,

u mm a r y

A s c h e m e f o r s y s t e m a t i c a n a ly si s o f e x p lo s iv e r e s id u e s i s p r e s e n t e d a n d d e m o n s t r a t e d


22/24

45 JOURNALOF FORENSIC SCIENCES

T A B L E 7 Exp los ive co mp onen ts ident i fi ed and the ir sources .

Com ponen t P robab le Or ig in

NaNO3 dynamite

NH4NO3 am mon ia dynam ite , b last ing slur ry

KNO3 black powd er

K~SO, black pow der, safety fuse, smokeless powders

Na2CO3 dynamite

Na~SO,( I ) dynamite

(Na2SO4) 1 n(Na 2CO 3)n dynam ite

NaC103 chlorate

KC10, chlorate

NaC1 NaC103, pe rm it ted dynam ite , contam inant

KC1 KC103

NH,C1 dry cell bat tery , pe rm it ted dynam ite

NO 3- dynami te , b l ack powder

NO 2- smokeless pow ders, dynam ite

NH , + amm onia dynam ite , NH,NO3 blast ing slur ry , dry cell bat tery

C NS - b l ack powder , dynami te

CO32 - dyn am ite

SO, z- dynam ite , b lack pow der , smokeless pow der

C1- d ry ce ll ba t t e ry , pe rm i t t ed dynami te , con taminan t

Na dynami te , con taminan t

K b lack powder

Ca con taminan t , dynami te

B dynami te

Ba dynamite

Pb blasting cap residue

A1 blasting cap casing

Zn dry cell bat tery casing

E G D N d y n a m i t e

NG dynam ite , double-base smokeless powd er

NC dyn am ite, single-base smokeless pow der

TN T blast ing slur ry , mi l i tary dem ol i t ion charge

DN T dyn am ite, single-base smokeless pow der

PET N de tona ting co rd

RDX C4 plastic explosive

b y t e s t e x p l o s i o n s u s i n g c o m m e r c i a l , m i l i t a r y , a n d h o m e m a d e e x p l o s i v e s . T h e s i g n i f i -

c a n c e o f r e a c t i o n p r o d u c t i d e n t i f i c a t i o n i s d e m o n s t r a t e d .

A c k n o w l e d g m e n t s

T h e a u t h o r s g r a t e fu l l y a c k n o w l e d g e th e c o o p e r a t i o n o f t h e B a se C o m m a n d e r a n d

E O D t e a m o f t h e C a n a d i a n F o r c e s B a s e E d m o n t o n , t h e C h i e f C o n s t a b l e a n d B o m b

D e t a i l o f t h e E d m o n t o n C i t y P o li c e , a n d t h e E x p l o s iv e s D i v i si o n o f C a n a d i a n I n d u s tr i e s

L t d . , E d m o n t o n . W e th a n k t h e O f f ic e r i n C h a r g e o f t h e R C M P C r i m e D e t e c ti o n

L a b o r a t o r y , E d m o n t o n f o r h is e n c o u r a g e m e n t o f t h is w o r k a n d t h e P h o t o g r a p h y

S e c t i o n f o r t h e i r t e c h n i c a l a s s i s t a n c e .

P P E ND I X

G l o s s a r y o f E x p l o s i v e b b r e v i a t io n s a n d T e r m i n o l o g y

B l a c k P o w d e r - - K N O J C / S , u su a ll y 7 5 /1 5 /1 0


23/24

BEVERIDGE ET AL ON EXPLOSIVE RESIDU ES 4 5

B l a s t i n g

Cap--A small high explosive charge in a metal cylinder, used to initiate a bulk

high explosive charge by means o f a shock wave; initiated electrically or by safety

fuse

Booster--A small high explosive charge used in conjunction with a blasting cap to ensure

detonation of a bulk high explosive charge

C--Carbon

C4--Military code for plastic explosive based on RDX

Chlorate/Sugar--Mechanical mixture of potassium or sodium chlorate and sugar

D e t o n a t i n g Cord--A linear explosive consisting of a series of cylindrical wrappings with

a central high explosive core, usually PETN

DNT--2,4-dinitrotoluene, CTH6 NO2)2

EGDN--Ethyleneglycol dinitrate, C2H4 ONO2)2

Foreite --Trade name for dynamite Canadian Industries Ltd.)

G e o g e l

--Trade name for dynamite Canadian Industries Ltd.)

H i g h

Explosive--Explosive with a velocity of detonation greater than 3280 ft/s, for

example, dynamite and plastic explosive

IED--Improvised explosive device

KNO3--Potassium nitrate

Low Explosive--Explosive with a velocity of detonation less than 3280 ft/s , for

example, black powder and pistol and rifle smokeless powder propellants

NaNO3--Sodium nitrate

NC--Nitrocellulose, variable formulation

NG--Nitroglycerine, C3Hs ONO2)3

NH,NO3--Ammonium nitrate

PETN--Pentaerythri tol tetranitrate, C~Hs ONO2),

Pla s t i c

Explosive--High explosive plus plasticizer to enable shaping of the charge,

for example, C4

Po la ~ --Trade name for dynamite Canadian Industries Ltd.)

RDX--Research and development explosive, cyclotrimethylenetrinitramine, C3H~N3 NO2)3

S--Sulfur

Safety Fuse--A series of cylindrical wrappings with a black powder core which burns at

a constant rate, usually 40 s/ft

S m o k e l e s s P o w d e r d o u b l e

base)--Propellant based on nitrocellulose and nitroglycerine

S m o k e l e s s P o w d e r s i n g le

base)--Propellant based on nitrocellulose

TNT--2,4,6-trinitrotoluene, C7H~ NO2)3

P P E N D I X B

Na2SO, I) is a metastable form of sodium sulfate which is stabilized by carbonate

[ 2 7 3 2 ] . Sodium carbonate sulfate is reported as the rare mineral burkeite [27] and as a

synthetic material [ 3 3 ] isolated from the sodium carbonate/sodium sulfate aqueous

system [34] . Sodium carbonate sulfate was synthesized in our laboratory by evaporation

of an aqueous solution of sodium sulfate and sodium carbonate, with a sodium

carbonate mole ratio of 0.2 to 0.5. The X-ray powder pattern in this range showed

neither precursor and, due to isomorphous exchange of carbonate and sulfate

[ 3 3 ]

showed no difference in d-spacings or intensities. Comparative d-spacings are given in

Table 6 for variously reported sodium carbonate sulfates. Our synthetic material was

indistinguishable from the carbonate sulfate residues noted in Table 3, Nos. 14 and

23 through 25.


24/24

5 J O U R N A LOF FORENSIC SCIENCES

e f e r en ce s

[ I ] Na t i ona l B omb D a t a C e n t e r , U .S . D e pa r t me n t o f Ju st ic e , F e de ra l B ure a u o f Inve s ti ga ti on ,

P ica t inny Arsena l , Dover , N.J .

[2] C anadian Bom b ~ a ta Cent re , Roy a l Can adian M ounted iPol ice , Ot tawa , Ont .

[3] Blas t ing Cap Recogn i t ion and Ident i f ica t ion M an ua l , Publ ic Secur i ty Cente r , In te rna t iona l

Assoc ia t ion of Chie fs of Pol ice , Ga i the rsbu rg , M d. , 1973.

[4] In t ro duc t ion to Exp los ives , Publ ic Secur i ty Cente r , In te rna t iona l Assoc ia t ion of Chiefs of

Police , Gaithersburg, Md., 1973.

[5] Bo m b Inc ident M ana gem ent , Publ ic Secur i ty Cente r , In te rna t iona l Assoc ia t ion of Chie fs of

Pol ice , Ga i the rsb urg , M d. , 1973.

[6] Bo mb Inc ident Targe t Ana lys i s , Publ ic Secur ity Cente r , In te rna t iona l Assoc ia tion of Chiefs

of Police , Ga i the rsb urg , M d. , 1973.

[7] Tardif, H. P. and Sterl ing, T. S. ,

J o u r n a l o f F o r e n s i c S c i en c e s,

JFS CA , Vol. 12, No. 3, 1967,

pp. 247-272.

[8] Yallop, H. J . , J o u r n a l o f t h e F o r e n s i c S c i e n c e S o c ie ty , Vol. 5, No. 1, 1965, pp. 6 -10 .

[ 9 Jenkins , R . and Ya l lop , H. J . , E x p l o s i v s t o f f e , No. 6, 1 970, pp. 139-141.

[10] Hoffman, C. M. and Bya l l , E . B . , J o u r n a l o f F o r e n s i c S c i en c es , JFSCA, Vol . 19 , No. 1 ,

Jan . 1 974, pp . 54-63.

[ l l l W a sh i ng t on , W . D. a nd Mi dk i f f , C . P . , J o u r n a l o f t h e A s s o c i a t i o n o f O f f i c i a l A n a l y t i c a l

C h e m i s t s , Vol . 55 , No. 4 , 19 73, pp . 811-822.

[12] Cook, M. A. , S c i e n c e o f H i g h E x p l o s e s , R he i nho l d t , Ne w York , 195 8 , C ha p t e r 12;

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