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This is to certify that the

thesis entitled

THE GAS CHROMATOGRAPHIC ANALYSISCOF
INTACT AND POST BLAST EMULSION EXPLOSIVES

presented by

Jeffery Brian Crump

has been accepted towards fulfillment
of the requirements for

M.S. Criminal Justice

degree in

 

 

    

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c:\clrc\datedue.pm3«p.1

THE GAS CHROMATOGRAPHIC ANALYSIS OF
INT ACT AND POST BLAST EMULSION EXPLOSIVES

By

Jeffery Brian Crump

A THESIS
Submitted to
Michigan State University
in partial fulfillment of the requirements
for the degree of

MASTER OF SCIENCE

Department of Criminal Justice

1993

Jay Siegel, Advisor

ABSTRACT

THE GAS CHROMATOGRAPHIC ANALYSIS OF
INT ACT AND POST BLAST EMULSION EXPLOSIVES

By

Jeffery Brian Crump

Emulsions are becoming more common place within the realm of explosives. Their ease
of manufacturing, low cost of production, compositional stability, and performance in the
field make emulsions a valuable and desired tool by mining companies. However, their
case of manufacturing has also allowed criminals to manufacture emulsions for potentially
illegal purposes. Forensic chemists and criminal investigators will eventually become
involved with a bombing case dealing with emulsions. Therfore, this thesis was based
on the gas chromatographic analysis of intact and post blast emulsion samples. The
emulsion samples were extracted using several different solvents to obtain the best
extraction quality. Extracts were analyzed on a Perkin Elmer 8500 gas chromatograph.
The resulting chromatograms revealed the wax, oil, and emulsifier combinations used
within the various emulsions tested. These results prove to be a useful tool in the

identification of emulsion explosives.

was

 

DEDICATION

This Thesis is dedicated to the person who has given me incentive, encouragement,
and hope. Her patience and support is greatly appreciated.
Thank you, Kymberly Anne McElgunn!

iii

ACKNOWLEDGMENTS

During the Summer of 1992, I was involved in an internship program through the
Criminal Justice Department, at Michigan State University. I had the pleasure of
completing this internship at the Bureau of Alcohol, Tobacco, and Firearms National
Laboratory in Rockville, Maryland. It was there where I was given the opportunity to
complete the experimental research on emulsion explosives needed for this thesis project.
I would like to extend my thanks and gratitude to Mr. Rick Tontarski, Mr. Richard
Strobel, Mr. Ed Bender, and the rest of the staff at the ATF laboratory. Their abundant
knowledge and help is greatly appreciated!

I would also like to thank Professor Jay Siege] for his patience and guidance in
helping me write this thesis!

And to my family, who has believed in me from the beginning, I thank you very

much!

iv

VHF;

 

TABLE OF CONTENTS

List of Tables

Gas Chromatograph Conditions

Individual Components and Compositions

Intact and Post Blast Emulsion Samples

Carbon Standard Sample Amounts

Individual Component Sample Amounts

Intact Emulsion Sample Amounts Prepared with TCE (Trial 1)
Intact Emulsion Sample Amounts Prepared with TCE (Trial 2)
Intact Emulsion Sample Amounts Prepared with TCE (Trial 3)
Intact Emulsion Sample Amounts Prepared with TCE (Trial 4)

Intact Emulsion Sample Amounts Prepared
with Methylene Chloride

Intact Emulsion Sample Amounts Prepared with
Hexane and TCE (Trial 1)

Intact Emulsion Sample Amounts Prepared with
Hexane and TCE (Trial 2)

Intact Emulsion Sample Amounts Prepared with Isa-Octane

Soil, Control, and Post Blast Sample Amounts Prepared
with TCE and Hexane

20

21

22

27

30

46

51

57

63

69

75

9O

98

List of Figures xiii

Chromatogram of Carbon Standards C22, C32, and C44 29
Chromatogram of Individual Component #1 31
Chromatogram of Individual Component #2 32
Chromatogram of Individual Component X—5 33
Chromatogram of Individual Component #3 36
Chromatogram of Individual Component TNOl 15 37
Chromatogram of Individual Component TNOl46 38

Chromatogram of Atlas Powermax 140
Prepared with TCE (Trial 1) 4O

Chromatogram of Atlas Powermax 440
Prepared with TCE (Trial 1) 41

Chromatogram of Atlas Apex 840 '
Prepared with TCE (Trial 1) 43

Chromatogram of Atlas Apex Blasting Agent 240(old)
Prepared with TCE (Trial 1) 44

Chromatogram of Austin Emulex 720
Prepared with TCE (Trial 1) 45

Chromatogram of Atlas Powermax 140
Prepared with TCE (Trial 2) 47

Chromatogram of Atlas Powermax 440
Prepared with TCE (Trial 2) 48

Chromatogram of Austin Emulex 720
Prepared with TCE (Trial 2) 50

Chromatogram of Atlas Apex 840
Prepared with TCE (Trial 3) 52

vi

THE!“

 

 

 

 

Chromatogram of Atlas Powermax 140
Prepared with TCE (Trial 3)

Chromatogram of Atlas Powermax 440
Prepared with TCE (Trial 3)

Chromatogram of Austin Emulex 720
Prepared with TCE (Trial 3)

Chromato gram of Atlas Apex 840
Prepared with TCE (Trial 4)

Chromatogram of Atlas Powermax 140
Prepared with TCE (Trial 4)

Chromatogram of Atlas Powermax 440
Prepared with TCE (Trial 4)

Chromatogram of Austin Emulex 720
Prepared with TCE (Trial 4)

Chromatogram of Atlas Powermax 140
Prepared with Methylene Chloride

Chromatogram of Atlas Powermax 440
Prepared with Methylene Chloride

Chromatogram of Atlas Apex 840
Prepared with Methylene Chloride

Chromatogram of Austin Emulex 720
Prepared with Methylene Chloride

Chromatogram of Atlas Powermax 140
Prepared with Hexane

Chromatogram of Atlas Powermax 440
Prepared with Hexane

Chromatogram of Atlas Apex 840
Prepared with Hexane

Chromatogram of Austin Emulex 720
Prepared with Hexane

vii

53

55

56

58

59

60

62

64

65

67

68

70

71

73

74

{HER

 

 

 

Chromatogram of Atlas Powermax 140
Prepared with Hexane and TCE

Chromatogram of Atlas Powermax 4-40
Prepared with Hexane and TCE

Chromatogram of Atlas Apex 840
Prepared with Hexane and TCE

Chromatogram of Atlas Apex Blasting Agent 240(old)
Prepared with Hexane and TCE

Chromatogram of Austin Emulex 720
Prepared with Hexane and TCE

Chromatogram of Atlas Apex Blasting Agent 240(new)
End 1 Sample Prepared with Hexane and TCE

Chromatogram of Atlas Apex Blasting Agent 240(new)
Middle Sample Prepared with Hexane and TCE

Chromatogram of Atlas Apex Blasting Agent 240(new)
End 2 Sample Prepared with Hexane and TCE

Chromatogram of Atlas 7D End 1 Sample
Prepared with Hexane and TCE

Chromatogram of Atlas 7D Middle Sample
Prepared with Hexane and TCE

Chromatogram of Atlas 7D End 2 Sample
Prepared with Hexane and TCE

Chromatogram of Atlas Powermax 140
Prepared with ISO-Octane

Chromatogram of Atlas Powermax 440
Prepared with Iso-Octane

Chromatogram of Atlas Apex 840 Prepared with Iso-Octane

Chromatogram of. Atlas Apex Blasting Agent 240(old)
Prepared with ISO-Octane

viii

76

78

79

8O

81

83

84

85

86

88

89

91

92

94

95

Chromatogram of Austin Emulex 720 Prepared with ISO-Octane 96

Chromatogram of Atlas 7D Prepared with Iso-Octane 97
Chromatogram of Soil & Intact Atlas Powermax 440 Mixture

Prepared with TCE 99
Chromato gram of Sample Control Soil Prepared with TCE 100

Chromatogram of Soil & Atlas Powermax 440 Post Blast Mixture
Prepared with TCE (Trial 1) 101

Chromatogram of Soil & Atlas Powermax 440 Post Blast Mixture
Prepared with TCE (Trial 2) 102

Chromato gram of TCE Filtrate through a Supelco Supelclean
LC-Sl Column 104

Chromatogram of Soil & Atlas Powermax 440 Post Blast Mixture
Prepared with Hexane 105

Overlay Chromatogram of Individual Component X-S

and Atlas Powermax 440 106
Introduction 1
Literature Review 4
Methods and Materials 17

Preparation of Standard 20

Preparation of Individual Components

from Atlas Powermax Formulations 21

Preparation of Intact Samples Using Trichloroethylene(TCE) 22

Preparation of Intact Samples Using Methylene Chloride 23

Preparation of Intact Samples Using Hexane 23

Preparation of Intact Samples Using Iso—Octane 24

Method of Post Blast Recovery 25

Preparation of Post Blast Samples 25
Experimental Results 27

Reslts of Standard Analysis 27

Results of Individual Components Prepared with TCE 30

Results of Intact Emulsion Samples

Prepared with TCE (Trial 1) 39

Results of Intact Emulsion Samples

Prepared with TCE (Trial 2) 46

Results of Intact Emulsion Samples _

Prepared with TCE (Trial 3) 51

Results of Intact Emulsion Samples

Prepared with TCE (Trial 4) 57

Results of Intact Emulsion Samples

Prepared with Methylene Chloride 63

Results of Intact Emulsion Samples

Prepared with Hexane and TCE (Trial 1) 69

Results of Intact Emulsion Samples

Prepared with Hexane and TCE (Trial 2) 75

Results of Intact Emulsion Samples

Prepared with Iso—Octane 90

Results of Post Blast Analysis 98
Discussion 107

Discussion of Results from Analysis of Individual Components 107

Discussion of Results from Analysis of Atlas Powermax 140 110

Discussion of Results from Analysis of Atlas Powermax 440
Discussion of Results from Analysis of Atlas Apex 840

Discussion of Results from Analysis of Atlas Apex
Blasting Agent 240(old)

Discussion of Results from Analysis of Austin Emulex 720

Discussion of Results from Analysis of Atlas Apex
Blasting Agent 240(new)

Discussion of Results from Analysis of Atlas 7D

Discussion of Results from Analysis of Post Blast Samples

Discussion of Basic Methodology, Including Solvents
Conclusions

Bibliography

111

113

114

114

116

116

117

118

120

124

Table 1:

Table 2:

Table 3:

Table 4:

Table 5:

Table 6:

Table 7:

Table 8:

Table 9:

Table 10:

Table 11:

Table 12:

Table 13:

Table 14:

LIST OF TABLES

Gas Chromatograph conditions.

Individual components and compositions.

Intact and Post-blast Emulsion samples.

Carbon standard sample amounts.

Individual component sample amounts.

Intact Emulsion sample amounts prepared with TCE (Trial 1).
Intact Emulsion sample amounts prepared with TCE (Trial 2).
Intact Emulsion sample amounts prepared with TCE (Trial 3).
Intact Emulsion sample amounts prepared with TCE (Trial 4).
Intact Emulsion sample amounts prepared with Methylene Chloride.
Intact Emulsion sample amounts prepared with Hexane and TCE (Trial 1).
Intact Emulsion sample amounts prepared with Hexane and TCE (Trial 2).
Intact Emulsion sample amounts prepared with iso-octane.

Soil, Control, and Post-blast amounts prepared with TCE and Hexane.

xii

Figure 1:
Figure 2:
Figure 3:
Figure 4:
Figure 5:
Figure 6:
Figure 7:
Figure 8:

Figure 9:

Figure 10:

Figure 11:

Figure 12:
Figure 13:
Figure 14:
Figure 15:
Figure 16:

Figure 17:

LIST OF FIGURES

Chromatogram of carbon standards C22, C32, and C44.
Chromatogram of individual component #1.

Chromatogram of individual component #2.

Chromatogram of individual component X-S.

Chromatogram of individual component #3.

Chromatogram of individual component TN0115.

Chromatogram of individual component TN0146.

Chromatogram of Atlas Powermax 140 prepared with TCE (Trial 1).
Chromatogram of Atlas Powermax 440 prepared with TCE (Trial 1).
Chromatogram of Atlas Apex 840 prepared with TCE (Trial 1).

Chromatogram of Atlas Apex Blasting Agent 240 (old) prepared with TCE
(Trial 1).

Chromatogram of Austin Emulex 720 prepared with TCE (Trial 1).
Chromatogram of Atlas Powermax 140 prepared with TCE (Trial 2).
Chromatogram of Atlas Powermax 440 prepared with TCE (Trial 2).
Chromatogram of Austin Emulex 720 prepared with TCE (Trial 2).
Chromatogram of Atlas Apex 840 prepared with TCE (Trial 2).

Chromatogram of Atlas Powermax 140 prepared with TCE (Trial 3).

xiii

Figure 18:
Figure 19:
Figure 20:
Figure 21:
Figure 22:
Figure 23:
Figure 24:
Figure 25:
Figure 26:
Figure 27:
Figure 28:
Figure 29:
Figure 30:
Figure 31:
Figure 32:
Figure 33:
Figure 34:

Figure 35:

Figure 36:

Chromatogram of Atlas Powermax 440 prepared with TCE (Trial 3).
Chromatogram of Austin Emulex 720 prepared with TCE (Trial 3).
Chromatogram of Atlas Apex 840 prepared with TCE (Trial 4).
Chromatogram of Atlas Powermax 140 prepared with TCE (Trial 4).
Chromatogram of Atlas Powermax 440 prepared with TCE (Trial 4).
Chromatogram of Austin Emulex 720 prepared with TCE (Trial 4).
Chromatogram of Atlas Powermax 140 prepared with methylene chloride.
Chromato gram of Atlas Powermax 440 prepared with methylene chloride.
Chromatogram of Atlas Apex 840 prepared with methylene chloride.
Chromato gram of Austin Emulex 720 prepared with methylene chloride.
Chromatogram of Atlas Powermax 140 prepared with Hexane.
Chromatogram of Atlas Powermax 440 prepared with Hexane.
Chromatogram of Atlas Apex 840 prepared with Hexane.

Chromatogram of Austin Emulex 720 prepared with Hexane.
Chromatogram of Atlas Powermax 140 prepared with Hexane and TCE.
Chromatogram of Atlas Powermax 440 prepared with Hexane and TCE.
Chromatogram of Atlas Apex 840 prepared with Hexane and TCE.

Chromatogram of Atlas Apex blasting agent 240 (old) prepared with Hexane
and TCE.

Chromatogram of Austin Emulex 720 prepared with Hexane and TCE.

xiv

“HF

 

 

Figure 37:

Figure 38:

Figure 39:

Figure 40:
Figure 41:
Figure 42:
Figure 43:
Figure 44:
Figure 45:

Figure 46:

Figure 47:
Figure 48:

Figure 49:

Figure 50:

Figure 51:

Figure 52:

Figure 53:

Figure 54:

Chromatogram of Atlas Apex blasting agent 240 (new) End 1 sample prepared
with Hexane and TCE.

Chromatogram of Atlas Apex blasting agent 240 (new) middle sample
prepared with Hexane and TCE.

Chromatogram of Atlas Apex blasting agent 240 (new) End 2 sample prepared
with Hexane and TCE.

Chromato gram of Atlas 7D End 1 sample prepared with Hexane and TCE.
Chromatogram of Atlas 7D middle sample prepared with Hexane and TCE.
Chromatogram of Atlas 7D End 2 sample prepared with Hexane and TCE.
Chromatogram of Atlas Powermax 140 prepared with iso-octane.
Chromatogram of Atlas Powermax 440 prepared with iso-octane.

Chromatogram of Atlas Apex 840 prepared with iso-octane.

Chromatogram of Atlas Apex blasting agent 240 (old) prepared with
iso-octane.

Chromatogram of Austin Emulex 720 prepared with iso-octane.
Chromatogram of Atlas 7D prepared with iso-octane.

Chromatogram of Soil & Intact Atlas Powermax 440 Mixture Prepared with
TCE.

Chromatogram of sample control soil prepared with TCE.

Chromatogram of Soil & Atlas Powermax 440 Post Blast Mixture prepared
with TCE (Trial 1).

Chromatogram of Soil & Atlas Powermax 440 Post Blast Mixture prepared
with TCE (Trial 2).

Chromatogram of TCE filtrate through a Supelco Supelclean LC-Sl column.

Chromatogram of Soil & Atlas Powermax 440 Post Blast Mixture prepared
with Hexane.

XV

Figure 55: Overlay. Chromatogram of individual component X-5
and Atlas Powermax 440.

xvi

INTRODUCTION

Emulsion explosives are becoming more commonly used in
criminal bombings since explosive manufacturers are turning
away from the production of the once popular commercial
dynamite, water gels, and slurries. Dynamite poses health
risks while gels/slurries have limited shelf lives.
Emulsions, however, avoid these disadvantages due to their
composition. With the decrease in production of dynamite and
increase in production of emulsions, the same pattern of usage
has been observed in criminal bombings within the United
States.

In 1990 there were 1,573 actual and attempted bombings
according to data from the Bureau of Alcohol, Tobacco and
Firearms (ATF) , Federal Bureau of Investigation (FBI), and the
United States Postal Service (USPS). Those bombings caused
the deaths of 22 persons, injuries to 251 persons, and
approximately $13 million in property damage. The most common
targets are residential buildings, mail boxes, vehicles, and
commercial buildings with motives typically of vandalism and
revenge (Dept. of Treasury, ATF, 1990) . The deaths and
damages caused by bombings are gruesome and severe, while the

potential destructiveness of further bombing incidents is

 

2
high. Although the destruction caused by bombings cannot be
reversed, justice can be served if investigators are able to
determine the type of explosive used, and the person
responsible for making and planting the device.

Identification and characterization of the explosive can
be paramount in the investigation of any bombing incident, and
can serve as a case breaking lead for the investigator. With
this information the investigator can concentrate his/her
efforts on.aicertain manufacturer or supplier, and.on evidence
collected in connection with a certain suspect.
Unfortunately, emulsions are made with the same or similar
materials by all manufacturers making identification of a
particular manufacturer quite difficult.

Essentially, emulsions are made with a carbonaceous fuel
which serves as the fuel phase and acts like a catalyst, an
inorganic oxidizer salt which acts as an oxidizing agent,
microspheres which.provide sensitization and density control,
an oil/wax combination which helps retain consistency and adds
to the fuel phase of the emulsion, an emulsifier to emulsify
the mixture, aluminum which is used as an auxiliary fuel, and
water which is needed in the reaction with the oxidizer salt
(Wade 1978). Different ingredients can be used to act as an
oxidizer, emulsifier, fuel, oil, or wax and it is assumed.that
manufacturers change ingredients depending upon price
variation and the conditions (weather and soil) under which

the emulsion will be used. Also, explosive manufacturers

“HES

 

3
consider their formulations to be proprietary, making it
difficult t1) obtain compositional information” Therefore,
analysis of emulsions may yield results that cannot be used to
individualize a sample to a particular manufacturer, but
analysis of an intact sample and a post—blast sample can yield
data that will permit comparison.

The research completed.here utilized.a gas Chromatograph
(GC) to analyze the organic components (oil/wax/emulsifier) of
five intact emulsions, one emulsion blasting agent, and one
post—blast sample.

From the results obtained it is hoped that chromatograms
from GC analysis will provide the necessary information to
determine if different intact samples can be distinguished
from each other, and if post-blast samples can be identified
as emulsions and to one particular intact sample.

Combining the analysis of organic components in emulsions
by GC with the analysis of inorganic components by spot tests,
X—ray diffraction (XRD), and ion chromatography, allows
forensic chemists to make a responsible conclusion as to
whether an unknown explosive is an emulsion or if a post-blast
sample reveals emulsion explosives that can be compared with

suspect intact samples.

LITERATURE REVIEW

The era of high explosives began in 1846 when a chemist,
named Ascanio Sobrero, at The University of Torino, nitrated
glycerin and partially destroyed his lab in the process
(Hopler, 1991). However, it was not until 1866 when Alfred
Nobel received his patent on a mixture of kieselguhr and
nitroglycerin (NG) commonly called dynamite (Hopler, 1991).
Nobel solved the problem of NG exploding unexpectedly by
making it more stable with the use of kieselguhr (diatomaceous
earth) since this material is an absorbant and acts to protect
the NG from shock. Giant Powder Company and Dupont were the
two major companies to produce dynamite in the late 1800’s
after learning how to make it mbre stable and packageable.
Mining and construction companies then learned that dynamite
could produce a more desirable effect than could black powder
so the use of dynamite spread rapidly.

Improvements in dynamite formulations began after
recognizing that kieselguhr was an inert product, but other
materials such as sodium nitrate would act as an oxidizer
adding more strength to the mixture. NC was also mixed with
nitrocotton to produce a very high strength explosive where

the NG wasn't in the liquid form. Ammonium nitrate was also

4

1":ng

 

5
used to replace part of the NG, leaving a powerful, water—
resistant product.

In 1925 Hercules Powder Company marketed a brand of
dynamite with a high ammonium nitrate concentration (Hopler,
1991). This product utilized inexpensive ingredients but
still had strength enough to produce desired effects.

Then in 1935, Dupont marketed a mixture of AN, fuel oil,
and. dinitrotoluene (DNT) that had. advantages of extreme
insensitivity, easy handling, and decreased toxcicity (Hopler,
1991).

In the mid 1950’s an explosive composed of only AN and a
fuel oil was introduced. It was called ANFO (ammonium nitrate
fuel oil). ANFO had the major advantage of low cost, but
lacked.water resistance and density. Therefore, it had to be
packaged in water resistant liners for use in wet holes, which
didn't allow for the cross-section of the hole to be
completely filled. The low density limited the amount of the
ANFO that could be used, thus limiting the energy released
from detonation. In answer to this problem Dr. Melvin A. Cook
invented an ammoniuninitrate based explosive called a slurry,
in 1957 (Hopler, 1991). Unlike ANFO the slurry itself
contained water and a gelling agent, usually a guar gum, to
thicken the solution. This added the water resistance and
higher density lacking in ANFO.

In addition to slurry components, companies began adding

sensitizers, which increase the detonation propagation. This

HE

 

 

 

6
eliminates the need for a separate sensitizer. Commonly used
components were chemical gassing, microballoons, aluminum
powder or chips, Methylamine nitrate (MAN), ethylene glycol
mononitrate (EGM), hexamethyl enetetramine nitrate (HMTAN),
and monoethanol amine nitrate (MEAN) (Hopler, 1991).

Slurries became extensively used, especially “Tovex, "
produced by Dupont. Slurries had advantages over ANFO,
however they had the disadvantages of exhibiting unexpected
variability in performance, having a limited shelf-life, and
having detonation problems at ambient temperature and pressure
(Kaye, 1980).

In the 1980’s a new explosive called.an emulsion.emerged
with advantages over slurries. Emulsions exist either as an
oil-in-water or water-in-oil composition where both exist as
small droplets of one material enclosed in a continuous matrix
of another material (Hopler, 1991). Emulsion explosives are
usualLy of the water-in-oil type, where water droplets are
surrounded by oil making the mixture water resistant. The
water droplet however'isiactually'a supersaturated solution of
ammonium nitrate surrounded by the hydrocarbon fuel.

According to Hopler (1991) ANFO is the most used
explosive material in the'United States, but does not have the
most efficient detonation reaction due to AN particle size.
In emulsions the AN' particle size has been drastically
reduced, which increases the detonation reaction.

Besides the microscopic AN particles, emulsions contain

7
water, one or more inorganic nitrate oxidizers, oil with or
without dissolved wax, and emulsifying agents. Emulsions
generally contain a sensitizer such as a metal perchlorate,
but all emulsions manufactured at Atlas contain bubbles or
microspheres as a sensitizer (Midkiff 1992). Microspheres
also provide density control as well as sensitization.

A more detailed composition comes from.a patent by Wade
(1978), but can also be found in a variety of patents on
emulsion explosives and blasting agents. The cap—sensitive
emulsion described by Wade (1978) contains from 3.5% - 8% by
weight of a hydrocarbon fuel with an emulsifier. Typical
fuels used are paraffins, olefins, naphthenes, aromatic
compounds, and saturated or unsaturated hydrocarbon fuels.
Included within the fuel is a combination.of a wax and an oil.
The wax content can range from 2.5% - 4.5% by weight in the
emulsion, and the oil can range from 0.5% - 5.5% by weight in
the emulsion (Wade, 1978). The waxes used can include
petrolatum wax, microcrystalline wax, paraffin wax, mineral
waxes, animal waxes, and insect waxes. Examples of oils used

are petroleum oils, vegetable oils, or highly refined mineral

oils.

The emulsifier is also combined with the carbonaceous
fuel ranging from, 0.5% - 2.0% by ‘weight of the total
composition (Wade, 1978). Examples of the emulsifiers are
sorbitan monolaurate, sorbitan monooleate, sorbitan

monopalmitate , sorbitan monostearate , and sorbitan

8
tristearate. Mono- and diglycerides of fat—forming fatty
acids and polyethylene sorbitol beeswax derivative materials
can also be used as emulsifiers.

Particulate aluminum can be used as an auxiliary fuel
within emulsions ranging up to 15% by weight (Wade, 1978).

Water is present from 10% - 22% by weight of the total
emulsion (Wade, 1978).

An oxidizer salt ranging from 65% - 85% by weight of the
emulsion is typically present (Wade, 1978). The salt is
generally ammonium nitrate, however-there may be up to 20% of
another inorganic nitrate combined with AN, such as an alkali
or alkaline earth metal. An ammonium perchlorate or earth
metal perchlorate could also be used.

Ranging from 0.9% - 15% by weight are glass microbubbles
(Wade, 1978) . These can range from 10 - 70 microns in size,
where the bulk density ranges from 0.1 - 0.4 g/cc. The
microbubbles are used to achieve a density in the emulsion
from 0.9 -1.35 g/cc (Wade, 1978) . Commonly used microbubbles
are sold by 3M Company with a trade designation of B15/250.
Emerson & Cumming, Inc. sell microbubbles with a trade
designation of Eccospheres. Philadelphia Quartz Company sells
microbubbles under the trade designation Q—CEL.

Blasting agents are described as being an explosive,
either a slurry or emulsion, that cannot be initiated by a
No. 8 blasting cap, thus requiring a primer for detonation

(Midkiff, 1992) .

9

Emulsion blasting agents contain the same general
components as do emulsion explosives except for the use of a
sensitizer such as inorganic metal compounds like aluminum
(Brockington, 1980)(Bluhm, 1969).

Published laboratory analyses of emulsion explosives or
blasting agents is limited since emulsions are relatively new.
However, due to the inorganic components within emulsions,
unrelated experimental studies performed on inorganic
materials can be applied to the analysis of emulsions.

Glass microspheres were analyzed.by Midkiff (1992) using
Scanning Electron Microscopy/Energy Dispersive X-Ray (SEM/EDX)
which determined elemental composition of the microspheres.
The elemental compositions were found to be different among

samples allowing them to be associated with their respective

producers. Particularly, elements of 3M glass microspheres
are calcium and silicon. Philadelphia Quartz (PQ) glass
microspheres contain sodium and silicon. PQ ceramic

microspheres contained aluminum, calcium, iron, potassimm,
sulfur, silicon, and titaniumu . An. unknown. producer of
phenolic mdcrospheres contains aluminum, chlorine, iodine,
sodium, sulfur, and silicon. An unknown producer of glass
microspheres with.a Hercules brand name contains the elements
aluminum, calcium, chlorine, potassium, sulfur, and silicon.

Further inorganic analysis can be accomplished by a
variety of tests such as spot tests, crystal tests, ion

chromatography (IC), Fourier Transform Infrared (FTIR), and

10

XRD. ILnorganic components of emulsion.explosives and.blasting
agents can vary depending upon the different oxidizers and
sensitizers used during manufacturing. As noted in several
patents, inorganic oxidizing salts within emulsions are
ammonium nitrate, sodium nitrate, potassium nitrate, calcium
nitrate, ammonium perchlorate, sodium perchlorate, potassium
perchlorate, or calcium perchlorate (Bluhm 1969)(Wade
1978)(Brockington 1980).

Spot tests and crystal tests offer a quick and easy
determination of the inorganic composition of an emulsion.
Nitrates and nitrites can be detected by the dipheynlamine,
Griess, or nitron spot tests. With the addition of
diphenylamine reagent to the test solution a deep blue color
will appear (Hoffman and Byall, 1973), a blue to blue-black
color indicating nitrates, and blue—black color indicating
nitrites (Parker, Stephenson, McOwen, Cherolis, 1974). As
noted by Hoffman et al. (1973) the diphenylamine test will
also produce a blue color in the presence of other oxidizing
agents, therefore this test is most useful as a screening
test.

The Griess test will produce a pink to red color in the
presence of nitrates when the reagent is added to the test
solution. In the presence of nitrites a red to yellow color
will appear (Parker et al. 1974). Hoffman et al. (1973)
states that after the addition of the Griess reagent to the

test solution addition of zinc dust will reduce the nitrate

11
ions to nitrite ions producing a deep red color.

The nitron reagent will produce a white precipitate in
the presence of nitrates and a dirty white precipitate in the
presence of nitrites (Parker et al. 1974).

The detection of ammonitun is performed by the addition of
Nessler’s reagent to the test solution where a orange/brown
color will appear (Hoffman et al. 1973)(Hayes, 1980)(Midkiff
et al. 1992).

Perchlorates were detected by Parker et al. (1974) by
adding cupric tetrapyridine reagent to the test solution
yielding a purple crystalline precipitate, or by adding
methylene blue reagent yielding a purple color to a purple
precipitate. Midkiff et al. (1992) also used
triphenylselenium chloride to detect perchlorates, which forms
a white precipitate or white needles in clusters within the
test solution. Tetrabutyl ammonium chloride, when added to
the test solution will form a white precipitate or small
crystals resembling glass chips in the presence of chlorates.

Sodium, potassium, and calcium can be detected through
the use of a flame test on the dried extract. An intense
yellow color will appear in the presence of sodium, A lilac
flame coloration will appear under two thicknesses of cobalt
blue glass to indicate the presence of potassium" .An orange—
red flame coloration will indicate the presence of calcium,
however, this test is inconclusive if sodium is also present

(Hayes 1980).

12

Chemical spot tests can also be performed on sodium,
potassium, and calcium. The detection of sodium is performed
by the addition of zinc uranyl acetate reagent to solution
yielding er slow developing yellow/green fluorescence under
ultraviolet light. Potassium is indicated when a white
precipitate forms upon addition of sodium tetraphenylboron to
the test solution. Ammonium.ions should be removed prior to
this test by boiling with 2N sodium hydroxide. Calcium is
indicated when a violet precipitate forms after addition of
freshly prepared 0.2% aqueous sodium.rhodizonate solution and
1N sodium hydroxide solution (Hayes 1980).

Beveridge, Greenlay, and Shaddick (1983) completed
experimental studies on water gels and.a‘wide range of "home—
made" chemical mixtures utilizing IR and XRD in part. Their
samples were confined in steel pipes and ignited leaving
residue and unreacted material to be analyzed. The chemical
mixtures were two component combinations of oxidizers with a
fuel. Potassiuml chloride ‘was identified. by XRD, while
chlorate and some unreacted perchlorate were identified.by IR
and XRD. Entrate oxidizers were reduced to nitrites which
were identified by IR.

Ion chromatography (IC) is increasingly becoming used to
detect inorganic materials within suspect explosives. This
technique is beginning to take the place of traditional
chemucal spot tests and.XRD, or being used.in conjunction with

them» Reutter, Buechele, and Rudolph (1983) believe that the

13
traditional methods have limitations in their efficiency to
detect inorganic materials that IC would readily detect.

When the extortion bombing of Harvey’s Resort Hotel, in
Nevada, occurred in 1980, the extortionist told authorities
that the explosive device contained TNT. However, debris
collected after the bomb detonated was extracted with water
and the extract was analyzed using chemical spot tests and
XRD. These tests only showed positive results for calcium
carbonate and calcium sulfate from pieces of cement and dry
wall (Reutter et al. 1983).

With no success using those techniques they decided to
analyze the water extract with IC where, in fact, traces of
sodium, ammonium, and.nitrates were detected on all fragments
of the improvised explosive device (IED) (Reutter et al.
1983).

Analysis of post-blast residues of a commercial slurry
revealed that IC detected sodium, nitrate, ammonium,
monomethylamine, potassium, nitrite, choride, and sulfate
where XRD of the same residue only detected sodium nitrate
(Reutter et al. 1983).

X-ray diffraction (XRD) is by no means an obsolete tool
in the analysis of pre— or post-blast residues, however, it
proves most useful in the analysis of solid residues versus
that_of traces that may be recovered from.a‘water extraction.

Rudolph et al. (1983) experimented with varying IC

conditions to ‘yield optimum. results. They found that

14
nitrates, nitrites, chlorates, phosphates, and sulfates can be
detected in a single run using a sodium carbonate/bicarbonate
eluent, and sodium, ammonium, potassium, and monomethylamine
were detected using a 0.10 N HCL / 60% H20 / 40% methanol
eluent.

The detection of divalent cations, such as calcium, has
become more important since the use of calcium nitrate as an
oxidizer along with ammonium nitrate. The divalent cations
calcium, magnesium, strontium, and barium were detected using
a 0.0025 N HCL / 0.0025 N phenylenediamine - 2HCL eluent
(Reutter, Buechele 1983).

Aluminum is detectable in pre-blast samples since most
aluminum used as sensitizers in gel/Slurries and emulsions are
in granular or chip form, and can be seen with the naked eye.
Testing the particles for confirmation of aluminum has been
done on a microscope slide with a drop of 10% NaOH. The
aluminum should immediately react with the NaOH to release
bubbles. The same test can be carried out with 6N HCL which
also reacts with alumintun, forming gas bubbles (Midkiff et al.
1992) .

Organic components that exist within emulsion explosives
and blasting agents include oils, waxes, and emulsifiers.
There is a large variety of oils, waxes, and emulsifiers that
can be used in any number of combinations and concentrations,
and since a single emulsion producer will use materials from

different suppliers, the value of characterization of the

15
oil/wax/emulsifier combination as being indicative of a
particular producer is unknown (Midkiff et al. 1992).

It is possible that for this reason little research has
been conducted on the organic analysis of emulsions. Little
information on emulsions in particular, and especially the
organic analysis of such, has been found in the literature.

Midkiff et al. (1992) used hexane and/or pentane to
extract an emulsion sample. The extracts were combined and
filtered through a micro filter to remove suspended particles,
and then evaporated to a small volume to concentrate the
extract.

Rudolph et al. (1983) used GC/MS to analyze the
hydrocarbons of an ANFO sample. A mass spectrum was obtained
through GC/MS to aid in the identification and
characterization of oils and if, according to Rudolph et al.
(1983), the same material is consistentLy being used by a.
particular group, this would reveal the groups identity if an
unclaimed bombing were to occur.

Bender, Crump, and Midkiff (1992) used gas chromatography
(GC) to analyze the organic extract of emulsions. They used
iso-octane as the solvent and a homogenizer to break up the
sample. After filtration the samples were analyzed by GC
where the oil, wax, and emulsifier mixtures were observed.

Front their research. they revealed. that the oil/wax
combinations dominate the chromatograms, however the

emulsifier can still be detected. Bender et al. (1983) also

16
found that the emulsifying packages varied widely among the
samples tested, thus leaving the possibility of using
emulsifier identification as a viable option in the

characterization of emulsions.

METHODS AND MATERIALS

The individual components of Atlas Powermax formulations
were dissolved in Trichloroethylene(TCE), and analyzed on the
Gas Chromatograph for comparison to chromatograms generated by
intact emulsion extractions.

The emulsion samples have been extracted with different
solvents in the hopes of finding a solvent that will better
extract the organic components from the sample, thus producing
better gas chromatographic (GC) results. Approximately 0.5-
1.0 grams of the intact samples were used experimentally per
each solvent. The intact emulsion samples used are listed in
Table 3. After solvation, each sample was concentrated by
evaporation. .All samples were analyzed.on a Perkin Elmer 8500
Gas Chromatograph using 1.0-2.0 ul sample injection sizes. The
injection sizes varied in order to observe if 2 ul injection
sizes produced better chromatographic results over 1 or 1.5 ul
injection sizes.

Post-blast samples, also listed in Table 3, were
prepared for GC analysis by using only Iso-octane as the
solvent. .Approximately 40-50 grams. of each. sample ‘was
combined with 30 m1 of iso-octane to dissolve the organic

components in the soil sample. A Supelco Supelclean LC-Sl

l7

column was used to remove contaminants from the post blast
extractions. .Each post column filtrate‘was then concentrated,

and analyzed on the GC using a 1 ul injection size.

18

19

List of Materials:

Perkin Elmer 8500 Gas Chromatograph

Nelson Analytical 900 Series Interface

Wyse PC 286/10 computer

Pierce Reacti-therm heating module

Pierce Reacti-vap evaporating unit

Tissue Tearor: Model 985-370 type 2, Biospec Products, Inc.

Whatman Autovial: 0.45um, Nylon-66 membrane, w/glass
microfilter prefilter, polypropylene housing

Supelco Supelclean LC-Sl column

Atlas products: Individual components & Intact emulsions.
From: Atlas Powder Company
' P.O. Box 271
Tamaqua, PA 18252

Austin products: Intact emulsions.
From; Austin Powder Company
3690 Orange Place
Cleveland, OH 44122

Sovents were LC Grade, supplied by Burdick & Jackson Co.

20

Table 1. Gas Chromatograph Conditions.

 

Instrument Perkin Elmer 8500 Gas
Chromatograph

 

Quadrex Aluminum clad fused
silica 15 meter "400"
Column methyl silicone 0.25 id.,
0.10um film thickness

 

 

 

 

Initial Temp. 100°C
Temperature Initial Time 5 min.
Program. Rate 10°C/min.
Final Temp. 420°C
Program Temperature
Injector Vaporizer(PTV) 430°C
ballistically
split/splitless
Carrier Hydrogen at 15psi head
pressure
Detector Flame Ionization at 450°C

 

 

 

 

Preparation of standard.
Standards, C22, C32, and C44, were prepared separately

with 1ml of Trichloroethylene(TCE) . The separate samples were
analyzed on the GC, and then mixed together, and analyzed in
combination. The Chromatogram of the combined sample is shown

in Figure 1.

21

Preparation of individual components from Atlas Powermax
formulations.

The samples were prepared as follows: Each sample was
weighed and combined with 2ml of Trichloroethylene(TCE). To
ensure that the sample dissolved as much as possible, shaking
and a little heat was applied. The individual components
themselves and their compositions, as stated by Atlas, are
listed in Table 2. GC sample injection size was 1 ul.

Chromatographic results are shown in Figures 2-7.

Table 2. Individual components and compositions

 

Individual Composition of component
component as stated by Atlas

 

Contains the oils that

are present in the external
#1 or fuel phase of the film
packaged cap sensitive
Powermax formulations.

 

Contains the wax and oil
#2 combination used in fuel
phase of Atlas’ paper
packaged product.

 

Contains the emulsifier

 

 

 

X—5 combination that goes with
#2.
Contains #2 and X—5 in the
#3 approximate proportions in
which they are used.
TN0115 This is the emulsifier used
with #1.
TN0146 This is the mixture of

 

 

 

TN0115 and #1.

 

22

Table 3. Intact and post blast emulsion

 

 

 

samples.
Intact Samples Post Blast
Samples
Atlas
Powermax 140
Atlas Atlas
Powermax 440 Powermax 440

 

Atlas Apex 840

Atlas Apex 240
Blasting Agent

Atlas 7D

 

 

 

Austin
Emulex 720

 

 

 

 

Preparation of Intact Samples using Trichloroethylene (TCEI,

Table 3 shows the intact emulsion samples and the post-
blast emulsion samples that were used in this study. All
samples listed in Tables 6-9 were taken from. different
locations within each packaged emulsion stick. This procedure
was done to determine if any settling of components had
occurred since the time of manufacturing that could cause
differing analysis results. Intact samples were first
dissolved using TCE, and prepared as follows: A spatula was
used to break up the sample as much as possible, and by
stirring and shaking vigorously to complete as much solvation

as possible. After solvation, the entire sample was poured

23
into a Whatman autovial for filtering. The filtered samples
were then ready for GC analysis, where 2 ul of each sample was
used to obtain Chromatograms. Chromatographic results are

shown in Figures 8-23 respectively.

Preparation of Intact Samples using Methylene Chloride.

Methylene Chloride was the next solvent used. Each
sample, shown in Table 10, was mixed separately with 5—10 ml
of methylene chloride, in a 30 ml beaker. The beakers were
placed on a hot plate at 350°C for 5 min. A spatula was used
to stir and break the larger pieces of the emulsion. The
beakers were then.placed into an ultrasonic bath to facilitate
further solvation. The samples were then placed into a
Centrex disposable centrifugal microfilter and placed into the
centrifuge until all liquid had been displaced to the bottom
of the tube. The liquid samples were then separately poured
into test tubes and placed into the evaporating unit to
evaporate all methylene chloride. After evaporation, 2 m1 of
TCE was added to each sample. GC sample injection size was 1

ul. Chromatographic results are shown in Figures 24—27.

Preparation of Intact Samples using Hexane.

Each sample, shown in Table 11, was separately placed
into a 30 md beaker, to which approximately 20 ml of hexane
was added. Each beaker was placed on a hot plate at 350°C,

and the hexane was allowed to boil down to approximately 5 ml

24
This remaining 5 ml was filtered through a Whatman autovial
into a test tube. The test tubes were placed into the
evaporating unit where all hexane was evaporated. To each
sample 2 ml of hexane was added” A.1 ul sample injection size
was used to obtain chromatographic results shown in Figures
28-31.

Table 12 shows previous samples used, plus the addition
of two new samples: Atlas Apex Blasting Agent 240 and Atlas
7D. The corresponding weights used of each sample is also
shown in Table 12. To each sample, approximately 25 ml of
hexane was added in.a 50 md beaker. The beakers were placed
on a hot plate at 350°C. Using a spatula the samples were
broken up as much as possible. The samples were boiled down
to approximately 5 ml and then each sample was filtered
through a Whatman Autovial into a test tube. The test tubes
were then placed into the evaporating unit where all hexane
was evaporated, after which 2 ml of TCE was added to each
sample. A 1.5 ul injection of each sample was used to obtain

the chromatographic results shown in Figures 32—42.

Preparation of Intact Samples using Iso—Octane.

The seven emulsion samples shown in Table 13 had a
representative sample taken from each. The corresponding
weights of each are also shown in Table 13. Each sample was
placed into a sample vial, to which approximately 3-5 ml of

iso-octane was added. The Tissue Tearor was used to

25
thoroughly homogenize each sample, then each sample was placed
into a centrifuge tube and centrifuged for approximately 30
seconds, at 1200 rpm. The supernatant was decanted into a
Whatman autovial and filtered into a clean sample vial. If
need be, the samples were evaporated down to a volume of
approximately 2 ml. Samples were then injected into the GC
for analysis using 1.5ul injections. Chromatographic results

are shown in Figures 43-48.

Method of Post Blast Recovery.

A 1 pound sample of explosive was suspended approximately
1 ft above the ground, using the bare ground as a witness
plate. The samples were detonated using an Austin Rockmaster
instantaneous detonator. The soil from the blast craters was
collected and placed into airtight canisters. Soil samples
from underneath the blast site were taken as control samples

before detonation.

Preparation of Post Blast Samples.

Approximately 40-50 g of each sample was placed in
separate beakers. Thirty milliliters of iso-octane was added
to each, and placed on a hot plate at 300°C, for 5 min. The
mixture was then gravity filtered. Then, using a Supelco
Supelclean LC-Sl column, 2 ml of iso—octane was poured into
the column followed by the filtrate of the separate samples.

The post column filtrate was placed into the Reacti-Vap &

26
Therm unit to concentrate the sample down to approximately 2
ml. A 1 ul sample injection size was used for GC analysis.
Chromatographic results are shown in Figures 49-54.
Figure 55 shows an overlay of the emulsifier sample X—5,

from Atlas, and an intact sample of Atlas Powermax 440.

EXPERIMENTAL RESULTS

The individual components found in most of Atlas’
Powermax formulations, listed in Table 2, have a consistency
ranging from a thick molasses to a hard wax. Table 5 shows
the weight of each individual component dissolved in TCE.
These components were relatively easy to dissolve in the
Trichloroethylene, but at times, a little heat was applied to
fully dissolve the samples.

The GC injection size of each sample was 1ul. Results
from.the GC analysis of the individual components can be seen

in Figures 2—7.

Results of Standard Analysis.

Table 4. Carbon standard sample amounts.

 

 

 

 

I STANDARD WEIGHT SOLVENT
C22 0.0046 g 12ml TCE
C32 0.0049 g 1 ml TCE
C44 0.0018 g 1 ml TCE

 

 

 

 

 

Table 4 lists the standards, and their corresponding
weights that were prepared with TCE.

Figure 1 shows C22 appearing at 8 minutes, C32 appearing

27

28

at 15 minutes, and C44 appearing at 22 minutes.

29

 

 

 

 

 

U
-r|s --
‘
6.
O
' LI LI I I I4 I I IJJJI I I_I__.I_I I I I I I I I I I4 I Ij I I I I I I I I

Figure l: Chromatogram of the Carbon Standards C22, C32,
and C44.

30

Results of Individual Components Prepared with TCE.

Table 5. Individual component sample amounts.

 

 

 

 

 

 

 

 

SAMPLE WEIGHL SOLVENT
#1 0.0760 g 2 ml TCE
#2 0.0810 g 2 ml TCE
#3 0.0570 g 2 ml TCE
X-S 0.0239 g 2 ml TCE

TN0115 0.0538 g 2 ml TCE

TN0146 0.0271 g 2 ml TCE

 

 

 

 

 

Figure 2 is of the individual component #1, containing
the oils that are present in the fuel phase of the cap
sensitive Powermax formulations. The GC produced one very
large peak ranging form 7 to 26 minutes. This peak had no
symmetry and had a large unresolved area underneath.

Figure 3 is the result of the GC analysis of individual
component #2, which contains the combination of wax and oil
used in the fuel phase of Atlas’ paper packaged.product. This
Chromatogram shows a series of consecutive sharp peaks ranging
from 7—21 minutes. There is also a small unresolved area
underneath the peaks within the same time range.

Figure 4 represents the individual component X-S, which
contains the emulsifier combination that is used with the
individual component #2. This Chromatogram. shows

approximately 7 peaks of interest. The first two peaks,

31

 

 

giig
3E
..ész °

v. MIILJ I4IIJILLIJIIIII44IILLJIL1441III

Figure 2: Chromatogram of Individual Component #1.

32

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

~ Bag ii .1
283
igr=

WJ—J—I—I leiLl‘JJ—ELIII I

 

Figure 3: Chromatogram of Individual Component #2.

33

 

 

 

J.” A" nm‘ 52 '

 

 

 

 

 

 

.ia
”tag.
“383

v smallnessannegHALLLAAJIAIAIJLllgnlfll111n-

Figure 4: Chromatogram of Individual Component X-S.

34

becoming evident at 6 minutes, are right next to each other,
and are not separated by the baseline. The second peak shows
up at 8 min. and is very evident from its peak height. The
next two peaks of interest show up at 14 min. These two peaks
are not separated by the baseline, and both have a high peak
height. Another peak that shows up at 15 min. is not
completely defined but is combined with a second peak where
they both share the same area beneath. The last peak of
interest shows up at 23 min. This peak does not begin and end
at the baseline, but is very evident from.its height.

Figure 5 represents the individual component #3, which
contains individual components #2 and X-S in the approximate
proportions in which they are used in the packaged emulsion.
Within this Chromatograph a series of consecutive peaks
ranging from 7.5 to 22 min can be seen. Interspersed within
the consecutive peaks are random peaks that are important.
The first being at 8 min., the second at 14 min., the third at
23 minutes.

Figure 6 represents the individual component TN0115,
which is an emulsifier used.with the individual component #1.
This Chromatogram shows somewhat symmetrical groupings of 4
and.5 peaks per group. These groupings appear in the range of
5-26 minutes.

Figure 7 represents the individual component TN0146,
which is the mixture of TN0115 and component #1. This

Chromatogram shows one large unresolved peak, with a large

35
area beneath it, ranging from 6—23 minutes. Ranging from 23—

28 min. are several groupings with 4 small peaks each.

36

 

m a I.“'I." -— ———- —____.

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

i? .
13
ii
31
i
i:
1
El
!' I
’l
“.3
d e E ‘
gs:
‘
{3:153
9
V WMle—Ll‘ll—kIJAJLllamn

 

Figure 5: Chromatogram of Individual Component #3.

 

37

 

 

 

a
fig
~ #23
V a
3:3“

v IIJIIIIIJIILLIJIII—I—I‘LIMLIgLIIIILJ J_I_IJIJI

Figure 6: Chromatogram of Individual Component TN0115.

38

 

 

-—- - ~--— -.-

LIIILJJIJJI4IAIIJIIILLIIIJIHQIIIIJ—LILIII

Figure 7: Chromatogram of Individual Component TN0146.

39

Results of Intact Emulsion Samples Prepared with TCE

(Trial 1).

Table 6. Intact emulsion sample amounts prepared
‘with TCE (Trial 1).

 

 

 

I Sample Weight Solvent
Atlas 0.48 g TCE-2 ml
Powermax 140
Atlas 0.63 g TCE-2 ml

Powermax 440

 

 

 

Atlas Apex 840 0.46 g TCE-2 ml
Atlas Apex 0.61 g TCE-2 ml
(BA) 240

Austin Emulex 720 0.42 g TCE-2 ml

 

 

 

 

 

Table 6 lists each sample and its amount used to obtain
the following chromatographic results.

Figure 8 represents a sample of Atlas Powermax 140.
Within this Chromatogram is a series of consecutive sharp
peaks ranging from 9-21 minutes. There is a small unresolved
area beneath these peaks that spans-most of the same time
range. There is a peak that appears at 7.5 min. with a
substantial height, one at 14:min., and.another at 23 minutes.

Figure 9 represents a sample of Atlas Powermax.440. This
Chromatogram shows the distinct consecutive series of sharp
peaks that range from.9-21 minutes. Underneath this range of
peaks is a somewhat large unresolved area. In addition are
the distinct peaks that appear at 7.5 min., 14 min., and 23

minutes.

40

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

2
l
l
l
l
I!
. l?
. i”
I.
3...
HM
1 il?."?: ‘
. .
1.1"...
. 1‘".
is l 6 '
“3E
no .
I
‘32:
~§sga
I
'0 lllllllllLlJIlLIIIIJIIIIIAIILLLJLIH11141

 

Figure 8: Chromatogram of Atlas Powermax 140 Prepared
with TCE (Trial 1).

 

41

 

 

 

 

 

 

 

 

 

 

 

 

 

.33 ~
Sérg
.3?
V

LJII IJ II._I_I LJ—II I I I I I I I4I_LJ I4JIJ I_I_LI I II__II I I 1

Figure 9: Chromatogram of Atlas Powermax 440 Prepared
with TCE (Trial 1).

 

 

42

Figure 10 represents a sample of Atlas Apex 840. A
series of consecutive sharp peaks range from 9—21 minutes.
Additional important peaks appear at 7.5 min., 17.5 min., and
23 minutes.

Figure 11 represents a sample of Atlas Apex 240 blasting
agent. This chromatogram.shows a series of consecutive peaks
ranging from 7-21 minutes. A quite large unresolved area is
present throughout the same time range. Additional important
peaks can be seen at 7.5 min., 14 min., 17 min., and 23
minutes.

Figure 12 represents a sample of Austin Emulex 720. This
Chromatogram reveals two large unresolved peaks. The first
ranging from 0.5-6 minutes. The second ranging from 7-20
minutes. Near the trailing end of this Chromatogram are two

groups of 4 small consecutive peaks between 21-24 minutes.

 

43

 

 

 

 

 

 

 

 

 

 

 

 

 

 

:33: w u "
F? J _
:35:

V

IIIJIIIIIIuJIJJ4IIIJJIIIIIIJ4JJIJIIIIII

Figure 10: Chromatogram of Atlas Apex 840 Prepared
with TCE (Trial 1).

 

44

 

 

 

 

 

 

 

 

 

 

 

 

 

—-—-
“v

 

 

ziig *
gas
3::

v LIIILJJILLILJIIIIJII4IJIJILJJIIIJIJIIIJ

Figure 11: Chromatogram of Atlas Apex Blasting Agent 240
Prepared with TCE (Trial 1).

 

45

 

 

 

 

 

 

£3 ,
gérg
aéfis

v IIIIIIIIIIIIIII_II_IJ.J+IIIIILIJJIIIJIIIJII

Figure 12: Chromatogram of Austin Emulex 720 Prepared
with TCE (Trial 1).

 

46

Results of Intact Emulsion Samples Prepared with TCE

(Trial 2).

Table 7. Intact emulsion sample amounts prepared
with TCE (Trial 2) .

 

 

 

 

Sample Weight Solvent
.Atlas 0.57 g TCE—2 ml
Powermax 140
Atlas 0.63 g TCE-2 ml
Powermax 440
Austin Emulex 720 0.92 g TCE-2 ml

 

 

 

 

 

Table 7 lists a second sampling of intact emulsion
samples prepared with TCE. These samples were taken from
different locations on the packaged sticks than those samples
listed in Table 6.

Figure 13 represents a sample of Atlas Powermax 140.
Again the familiar series of consecutive peaks ranging front?-
20 minutes can be seen. A small unresolved area beneath the
peaks can also be seen within the same range. Additional
important peaks can be seen at 7.5, 14 and 22.5 minutes.

Figure 14 represents a sample of Altas Powermax 440.
This chromatogram.shows an unresolved peak ranging from 4-6
minutes. The series of consecutive peaks is again present
ranging from.7-20 minutes. The peaks of this series, ranging
from 17-20 minutes, are small in height and not very sharp.
Additional important peaks can be seen at 7.5, 14, and 23

minutes.

 

 

47

 

v

 

 

 

 

 

 

 

 

 

 

 

 

.93
w.

gsrg
«$53

°v IIIIIIIJILIIIIJIIIJJIJJIIIIIJIIIJLIIIIIII

Figure 13: Chromatogram of Atlas Powermax 140 Prepared
with TCE (Trial 2).

 

 

48

 

 

 

 

 

 

 

 

 

 

 

 

.9 i
5231 .

I a
8:!“
V

 

IIIJIJ_JJI_IIII_LII_IIIILJIIIIIIIIIILIII—IIIJI

Figure 14: Chromatogram of Atlas Powermax 440 Prepared
with TCE (Trial 2).

 

49
Figure 15 represents a sample of Austin Emulex 720.
Within this Chromatogram is an unresolved peak of substantial
height: that ranges from 0.5-5 minutes. Another larger
unresolved peak, also at equal height, ranges from 7—20

minutes. From 21-23 min. are two groups of peaks with 4 peaks

to a group.

50

 

 

 

 

 

 

 

.é ,
§§gg l
:53

IIIIIIIIIIIIJIIIIIIIIIIIIILIIIIIIJIJIIJIII

Figure 15: Chromatogram of Austin Emulex 720 Prepared
with TCE (Trial 2).

 

51

Results of Intact Emulsion Samples Prepared with TCE
(Trial 3).

Table 8. Intact emulsion sample amounts prepared
with TCE (Trial 3).

 

 

 

 

 

 

 

 

ll Sample Weight Solvent
Atlas Apex 840 0.92 g TCE—2 ml
Atlas 0.55 g TCE-2 ml
Powermax 140
Atlas 0.80 g TCE—2 ml
Powermax 440
Austin Emulex 720 0.78 g TCE-2 ml

 

 

 

 

 

Table 8 lists a 3rd sampling of intact emulsion samples
prepared with TCE. These samples were again taken from
different locations on the packaged stick than those samples
listed in Tables 6 & 7.

Figure 16 represents a sample of Atlas Apex 840. A
series of consecutive sharp peaks is again present, ranging
from 8-21 minutes, with a small unresolved area beneath the
peaks. Additional peaks are seen at 7.5, and 23 minutes.

Figure 17 represents a sample of Atlas Powermax 140.
Ranging from.8-21 min. is a series of consecutive sharp peaks,
‘with a small unresolved. area beneath the entire range.

Additional peaks of interest are at 5, 7.5, and 23 minutes.

 

52

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

l
A; 1
ti?

.88:
{low

v IIIIIIILIIIIIJIIIII+IIIIIIIII’IIIkJIHIIJII

Figure 16: Chromatogram of Atlas Apex 840 Prepared
with TCE (Trial 3).

 

53

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

5
6
.‘1.
Lil
I H‘-
' l
6
.33
'30.
I
.8
Juno
.00.
God
v IIJIIIIIIIIIIIIIIILIJJLIIIIIJJIIIJIIIIIII

 

Figure 17: Chromatogram of Atlas Powermax 140 Prepared
with TCE (Trial 3).

 

54

Figure 18 represents a sample of Atlas Powermax 440.
Ranging from 8-21 min. is a series of consecutive peaks with
aa considerable area beneath the peaks, covering the entire
time range. Additional peaks of interest are at 5, 7.5, and
23 minutes.

Figure 19 represents a sample of Austin Emulex 720. An
unresolved peak ranging from 0.5-6 min. is shown, with an
additional, larger unresolved.peak ranging from 7-20 minutes.

Ranging from 21-25 min. are 3 groupings of 4 peaks each.

 

55

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

:33
21:3

v I I I4 I_j I I IJI_I I I I I I I I I ILI I I4 IJJJJJ I I I I I I I I I

Figure 18: Chromatogram of Atlas Powermax 440 Prepared
with TCE (Trial 3).

56

 

 

 

E:;E
318°

v0 IIIIIJIJIIIIIIJIIIIgLIIIIJIIIIIJIIIJIIIII

Figure 19: Chromatogram of Austin Emulex 720 Prepared
with TCE (Trial 3).

 

57

Results of Intact Emulsion Samples Prepared with TCE
(Trial 4).

Table 9. Intact emulsion sample amounts prepared
with TCE (Trial 4).

 

 

 

 

 

ll Sample Weight Solvent H
Atlas Apex 840 0.64 g TCE-2 ml
Atlas 0.82 g TCE-2 ml
Powermax 140
Atlas 0.76 g TCE-2 ml
Powermax 440
Austin Emulex 720 0.54 g TCE-2 ml

 

 

 

 

 

Table 9 lists the 4th sampling of intact emulsion samples
from.different locations on the packaged emulsion stick than
those samples listed in Tables 6, 7, & 8.

Figure 20 represents a sample of Atlas Apex 840. Ranging
from.8-20 min. is a series of consecutive peaks with a small
unresolved area beneath these peaks. Additional peaks of
interest can be seen at 5, 7.5, and 23 minutes.

Figure 21 represents a sample of.Atlas Powermax.140. The
familiar series of consecutive peaks ranging from.8—21 min.,
with a small unresolved area beneath these peaks. Additional
important peaks can be seen at 5, 7.5, and 23 minutes.

Figure 22 represents a sample of Atlas Powermax 440. The
familiar series of consecutive peaks is again present, ranging

from.8-21 minutes. Additional important peaks are present at

58

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

.r l
33%?

' IIIIIIJIIIIIAJIMIIIIIIIIIIJJIJJIIIIIJIII

Figure 20: Chromatogram of Atlas Powermax 840 Prepared
with TCE (Trial 4).

59

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

I 11 it

 

33 J
«o.

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v IIIIIIJJ_IIJIIIIIILJIIIIIIIIIIIIIIIIJJJII

Figure 21: Chromatogram of Atlas Powermax 140 Prepared
with TCE (Trial 4).

 

6O

 

 

 

 

 

 

 

 

 

 

 

 

 

ziig l
is}
.33.:

v IIIIIIIiIJIJIIIIJJIIIIIIJIIIILIJIIIIIIII

Figure 22: Chromatogram of Atlas Powermax 440 Prepared
with TCE (Trial 4).

61
7.5, 14, and 22.5 minutes.

Figure 23 represents a sample of Austin Emulex 720.
Ranging from 0.5-6 min. is an unresolved peak of considerable
height. Ranging from 7-19 min. is a larger unresolved peak
with equal height to the first. From 20—26 min., 4 groupings

of peaks can be seen with 4 small peaks per group.

62

 

 

 

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v IIJIIIIIIIIIIIIIIIIJIIJIJLLIJJLILIILIIII

Figure 23: Chromatogram of Austin Emulex 720 Prepared
with TCE (Trial 4).

63

Results of Intact Emulsion Samples Prepared with Methylene
Chloride.

Table 10. Intact emulsion sample amounts prepared with
Methylene Chloride.

 

 

 

 

 

Sample Weight Methylene TCE
Chloride

Atlas 0.35 g 5-10 ml 2 ml
Powermax 140
Atlas 0.40 g 5—10 ml 2 ml
Powermax 440
Atlas Apex 840 0.40 g 5—10 ml 2 ml
Austin Emulex 720 0.44 9 '5-10 ml 2 ml

 

 

 

 

 

 

Table 10 lists the weight of intact samples that were
prepared with Methylene Chloride initially, and then with TCE
for GC use. The amounts of Methylene Chloride and TCE used
are also indicated.

Figure 24 represents a sample of Atlas Powermax 140.
Shown in this Chromatogram is a series of consecutive peaks
that range from 8—17 minutes. Also shown is one peak that
appears at approximately 13.5 munutes. There is aa small
unresolved area that lies beneath the series of peaks.

Figure 25 represents a sample of Atlas Powermax 440.
Again the series of consecutive peaks can be seen that ranges
from 9—15 minutes. A separate peak lies at approximately 13.5

minutes. There is a large unresolved area beneath this series

64

I'll

 

 

 

 

 

 

 

 

 

 

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§érg
“€53
O

v LIAIJnunnuns—nunnnnnlnnnnesnnnmnnnnnnnnn

Figure 24: Chromatogram of Atlas Powermax 140 Prepared
with Methylene Chloride.

65

 

 

 

 

 

 

 

 

 

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C0

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Va IIIIIIIIIJIILLIIIIIIIJJIJIIIIIJJIIIIIIJI

Figure 25: Chromatogram of Atlas Powermax 440 Prepared
with Methylene Chloride.

 

66
of peaks.

Figure 26 represents a sample of Atlas Apex 840. A
series of consecutive peaks ranging from 8-16 minutes can be
seen. Two separate peaks can be seen at appx. 12.5 and 13.5
minutes.

Figure 27 represents a sample of Austin.Emulex:720. This
Chromatogram only shows a large unresolved peak ranging from

7—19 minutes.

67

 

 

 

 

 

 

 

 

 

 

 

 

3 6
2:3." ,—-—
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3:33

v LIIIJIIJLIIII

IJIIIJIIIIJIIIIIIIIIIIII__IJIII

Figure 26: Chromatogram of Atlas Apex 840 Prepared
with Methylene Chloride.

 

68

 

 

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.éa
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“on.

V

LLIJIIIIIIIILLIIIIIIIJIIIIIIIIIILLIJIIkI

Figure 27: Chromatogram of Austin Emulex 720 Prepared
with Hexane.

 

69

Results of Intact Emulsion Samples Prepared with Hexane
and TCE (Trial 1).

Table 11. Intact emulsion sample amounts prepared with
Hexane and TCE (Trial 1).

 

   
   

Sample Weight Initial Final
Solvent: Solvent:
Hexane TCE

Atlas 0.45 g 20 ml 2 ml

Powermax 140

 

 

 

Atlas 0.45 g 20 ml 2 ml
Powermax 440

Atlas Apex 840 0.45 g 20 ml 2 ml
Austin Emulex 720 0.40 g 20 ml 2 ml

 

 

 

 

 

 

Table 11 lists the weights of the intact samples prepared
with the initial solvent of Hexane, and then the final solvent
of TCE.

Figure 28 represents a sample of Atlas Powermax 140
prepared with Hexane and TCE. This Chromatogram shows a
series of consecutive jpeaks ranging from. 12-25 :minutes.
Additional important peaks can be seen at 11, 21, and 26
minutes.

Figure 29 represents a sample of Atlas Powermax 440. A
series of consecutive peaks ranges from.12-25 minutes. Other‘
peaks are shown at 9, 11, 21, and 26.5 minutes. A semewhat
large unresolved area can be seen underneath the range of

peaks.

70

 

 

 

 

 

 

 

 

 

 

 

 

Agg '
:33
ign-

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Figure 28: Chromatogram of Atlas Powermax 140 Prepared
with Hexane.

 

71

 

 

 

 

 

 

 

 

 

 

 

 

 

 

$32

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ii-
Vo LL11Ienaeannngn‘enjneni_m'1;nn_a‘nmn_11Iguanas;

Figure 29: Chromatogram of Atlas Powermax 440 Prepared
with Hexane.

72

Figure 30 represents a sample of Atlas Apex 840. A
series of consecutive peaks can be seen ranging from 12—25
minutes, with additional peaks at 11 and 26.5 munutes. A
small unresolved area beneath the peaks can be seen.

Figure 31 represents a sample of Austin.Emulex:720. This
Chromatogram shows an unresolved peak ranging from 0.5—5
minutes, and another unresolved peak from 11 to 23 minutes.
At 21 minutes is a sharp distinct peak. Ranging from 24—30

minutes are 4 groups of peaks, with 4 peaks per group.

 

 

 

 

73

 

 

 

 

 

 

 

 

 

 

 

A
g 6
:QIE ‘
IE
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to... HA—A—h‘fl—l—l—hl—L—L—‘d—L—hhl—I—H—H—J—l—J—l—l—HA—LJ—w

Figure 30: Chromatogram of Atlas Apex 840 Prepared
with Hexane.

 

 

74

 

 

 

.53
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8:88

v I_IIII4_I_LIIII14IIIIIIIIIIIJIIJIIIIJILJII

Figure 31: Chromatogram of Austin Emulex 720 Prepared
with Hexane.

75

Results of Intact Emulsion Samples Prepared with Hexane
and TCE (Trial 2).

Table 12. Intact emulsion sample amounts prepared with
Hexane and TCE (Trial 2).

 

 

 

 

 

 

 

 

 

 

 

 

Weight Initial Final
Solvent: Solvent:
Hexane TCE
Atlas 0.45 g 25 m1 2 ml
Powermax 140
Atlas 0.47 g 25 mu 2 ml
Powermax 440
Atlas 0.50 g 25 ml 2 ml
Apex 840
Atlas Apex 0.53 g 25 ml 2 ml
BA 240 (old)
Austin 0.50 g 25 ml 2 ma
Emulex 720
Atlas Apex End 1 0.87 g
BA 240 new
( ) Middle 0.89 g 25 ml 2 m1
End 2 0.78 g
Atlas 7D End 1 0.58 g
Middle 0.56 g 25 ml 2 ml
End 2 0.55 g

 

 

 

 

 

 

 

Table 12 lists the intact samples that were prepared with
hexane, and the corresponding weights of each sample used.

Figure 32 represents Atlas Powermax 140. There is a
range of peaks from 12-25 minutes that are in a series and
consecutive, with a very small area beneath the peaks that is

unresolved. Other peaks of interest show'up at 11.5, and 26.5

76

 

 

 

 

 

 

 

 

 

 

 

 

 

 

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“DU?!”

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O 0- SI 0 MIN

LIIIJLJ_14_IJIIIIIIIIIJIIIIIIIIIIIIIIIII

Figure 32: Chromatogram of Atlas Powermax 140 Prepared
with Hexane and TCE.

 

77
minutes.

Figure 33 represents a sample of Atlas Powermax 440.
From 12—25 minutes is a series of consecutive peaks with a
somewhat large unresolved area beneath the peaks in the same
range. ,Again, there are other peaks that appear at 11.5, and
26.5 minutes, and another peak at 17 minutes.

Figure 34 represents a sample of Atlas Apex 840. A
series of consecutive peaks can be seen in the range of 12—25
minutes with a small unresolved area beneath these peaks,
within the same time range. Again, there is the peak that
appears at 11.5 minutes, and the other common peak which
appears at 26.5 minutes.

Figure 35 represents a sample of Atlas Apex 240 BA (old).
A series of consecutive peaks ranging from 12-25 minutes is
again apparant, with a large unresolved area beneath this
series, within the same time range. The commonly seen peaks
at 11.5 and 26.5 minutes are also apparant.

Figure 36 represents a sample of Autin Emulex 720. This
Chromatogram shows a large unresolved peak that ranges from
10-21 minutes, with no series of consecutive peaks showing.
In the range of 22-29 minutes is a grouping of peaks. These

peaks appear as separate groups with 4 small peaks per group.

 

78

 

 

 

 

 

 

 

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0.0- 30.0 MIN

Figure 33: Chromatogram of Atlas Powermax 440 Prepared
‘ with Hexane and TCE.

 

79

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

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w.

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Figure 34: Chromatogram of Atlas Apex 840 Prepared with
Hexane and TCE.

 

80

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

gs;

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Figure 35: Chromatogram of Atlas Apex Blasting Agent 240
(old) Prepared with Hexane and TCE.

 

81

 

 

5::

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V

Figure 36: Chromatogram of Austin Emulex 720 Prepared
with Hexane and TCE.

 

 

82

Figure 37 represents a sample of Atlas Apex BA 240 (new),
taken from end 1 of the sample stick. This Chromatogram does
not ShOW'the common series of consecutive peaks, but does have
the common unresolved area that ranges almost throughout the
entire scale. .At 21 minutes is a very distinct peak, followed
by 4 groups of peaks with 4 peaks per group, ranging from 23—
29 minutes.

Figure 38 represents a sample of Atlas Apex BA 240 (new),
taken from.the:middle of the sample sticku Again, there is no
series of consecutive peaks, but the unresolved area that is
commonly present does exist, ranging throughout most of the
time scale. Again, at 21 minutes is a very distinctive peak
followed by the 4 groups of peaks with 4 peaks per group.

Figure 39 represents a sample of Atlas Apex BA 240 (new),
taken from end 2 of the sample stick. A larger unresolved
area can.be seen.within this Chromatogram, that ranges from.5-
31 minutes. No series of consecutive peaks exists, nor does
groupings of peaks exist.

Figure 40 represents a sample of Atlas 7D, taken from.end
1 of the sample stickg The common series of consecutive peaks
can be seen that ranges from 12-25 minutes, with virtually no
unresolved area beneath this range. Again, peaks of interest

appear at 11.5, 21, and 26.5 minutes.

83

 

 

 

 

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ii:3:

v IIIIIJIIIIIIIJJJIIkLIJJIILILIIIJJIILJIII

Figure 37: Chromatogram of Atlas Apex Blasting Agent 240

(new) End 1 Sample Prepared with Hexane and
TCE.

84

 

 

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Figure 38: Chromatogram of Atlas Apex Blasting Agent 240
(new) Middle Sample Prepared with Hexane and
TCE.

 

 

85

 

 

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“is:

v I I I I I I I I I I I I J I I I I I I I I I I I I I I I I I I I I I I I I I I

Figure 39: Chromatogram of Atlas Apex Blasting Agent 240
(new) End 2 Sample Prepared with Hexane and

TCE.

 

86

 

 

 

 

 

 

 

 

 

 

 

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“83
5...

v LIIIIIIIIIIIIIIIIIII 111111111

Figure 40: Chromatogram of Atlas 7D End 1 Sample
Prepared with Hexane and TCE.

87

Figure 41 represents a sample of Atlas 7D, taken from.the
middle of the sample stick” Ranging from 12—25 minutes is the
series of consecutive peaks, wittra slightly larger unresolved
area beneath this series than shown in chromatogrami40. Peaks
at 11.5, 21, and 26.5 minutes are seen, with the peak at 21
minutes being larger than that shown in Chromatogram 40.

Figure 42 represents a sample of Atlas 7D, taken from.end
2 of the sample stick. Ranging from 12-25 minutes is the
series of consecutive peaks, with a very slight unresolved
area beneath the series. Other important peaks appear at

11.5, 21, and 26.5 minutes.

 

88

 

 

 

 

 

 

 

 

 

 

 

 

 

2
9:3;
gar
343:

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V IIIIILILLIIIIALJIIIIIJIIIIIIII nnnnnnn

Figure 41: Chromatogram of Atlas 7D Middle Sample
Prepared with Hexane and TCE.

 

89

 

 

 

 

 

 

 

 

 

 

 

 

IIIIIIIJIIIILIII

Figure 42: Chromatogram of Atlas 7D End 2 Sample
Prepared with Hexane and TCE.

 

90

Results of Intact Emulsion samplesgprepared with Iso—Octane.

Table 13. Intact emulsion sample amounts
prepared with iso-octane.

 

 

 

 

 

 

 

 

Sample Weight Solvent:
Iso-Octane

Atlas 0.41 g 3—5 ml

Powermax 140

Atlas 0.77 g 3-5 ml

Powermax 440

Atlas 0.86 g 3-5 mu

Apex 840

Atlas Apex 0.46 g 3-5 ml

240(old)

Austin 0.74 g 3-5 ml

Emulex 720

Atlas 7D 1.51 g 3-5 ml

 

 

 

 

 

Table 13 lists the intact emulsion samples prepared.with
iso-octane, including the corresponding weights of each sample
used.

Figure 43 represents a sample of Atlas Powermax 140. In
the range of 12-25 minutes is the common series of consecutive
peaks, with a small unresolved area beneath this series. At
11.5, and 26.5 minutes are two other commonly seen peaks.

Figure 44 represents a sample of Atlas Powermax 440.
Ranging from 12-25 minutes is a series of consecutive peaks,
with a large unresolved area beneath this series. Other

important peaks are seen at 11.5, 18, and 26.5 minutes.

91

 

 

 

 

 

 

 

 

 

 

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V

 

Figure 43: Chromatogram of Atlas Powermax 140 Prepared
with Iso-Octane.

92

 

 

 

 

 

 

 

 

 

5
2
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vo llllllllll‘llJJJILLJlIIIIIIIILLJJLIJIJJ‘

 

Figure 44: Chromatogram of Atlas Powermax 440 Prepared
with ISO—Octane.

 

93

Figure 45 represents a sample of Atlas Apex 840.

The common series of consecutive peaks is again seen from 12-
25 minutes, with a small unresolved area beneath the series.
Two other peaks of interest appear at 11.5, and 26.5 minutes.

Figure 46 represents a sample of Atlas Apex BA 240 (Old).
Ranging from 12-25 minutes is a series of consecutive peaks,
with a large unresolved area beneath this series. Two other
important peaks appear at 11.5, and 26.5 minutes.

Figure 47 represents a sample of Austin Emulex 720. This
Chromatogram reveals one large unresolved peak that ranges
from 11-24 minutes. Ranging from 24—30 minutes are 4 groups
of peaks with 4 small peaks per group.

Figure 48 represents a sample of Atlas 7D. Ranging from
12—25 minutes is the common series of consecutive peaks, with
a small unresolved area beneath this series. At 11.5, and

26.5 minutes are two other common peaks that appear.

94

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

 

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Figure 45: Chromatogram of Atlas Apex 840 Prepared
with ISO-Octane.

 

 

 

 

 

 

 

 

 

 

 

 

 

2

H
34$:
33;
:23:
V
Figure 46: Chromatogram of Atlas Apex Blasting Agent 240
(old) Prepared with ISO—Octane.

III‘IIIIIJIAIIIIIII-IIIAIIIIIIIIAIIIIII

 

96

 

 

 

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23"
ga;
3&33

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Figure 47: Chromatogram of Austin Emulex 720 Prepared
with Iso-Octane.

 

97

 

 

 

 

 

 

 

 

 

 

 

 

 

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0

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Figure 48: Chromatogram of Atlas 7D Prepared with
ISO-Octane.

98

Results of Post Blast Analxsis.

Table 14. Soil, Control, and Post blast sample
amounts prepared with TCE and Hexane.

 

I Sample Weight Solvent I
Atlas Powermax 5.21 g TCE

440 control

 

Atlas Powermax 3.15 g TCE
440 post-blast

Atlas Powermax 40.75 g TCE
440 post—blast

 

 

Atlas Powermax 42.35 g Hexane
440 post-blast

 

 

 

 

 

Figure 49 represents a sample from the mixture of soil
and intact Atlas Powermax 440 extract. Ranging from 8-22
minutes is a series of homologous peaks, with an unrelsolved
area beneath.

Figure 50 represents a sample of the post-blast sample
control soil. Ranging from 14.5—20 minutes is a series of
small consecutive peaks.

Figure 51 represents a sample of the Atlas Powermax 440
post-blast, in which 3.15 grams of sample was extracted.
Ranging from 14.5-20 minutes is a series of small consecutive
peaks.

Figure 52 represents a sample of Atlas Powermax 440 post
blast, in which 40.75 grams of sample were extracted” IRanging

from.10.5-26 minutes is a series of consecutive peaks, with.an

 

99

 

 

 

 

 

 

 

 

 

 

 

 

 

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3&83

v LIIJIIIIIIIILULII'IIIIIIIIILIIIIIIIJIIIII

Figure 49: Chromatogram of Soil & Intact Atlas Powermax
440 Mixture Prepared with TCE.

100

 

 

 

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3:82

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Figure 50: Chromatogram of Sample Control Soil Prepared
with TCE.

101

 

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v IIIIIIIIJJIIIAIIJIlI-IIIIIIIIIIJIII—I—ILJJ

Figure 51: Chromatogram of Soil & Atlas Powermax 440
Post Blast Mixture Prepared with TCE (Trial 1).

 

 

102

 

ggg
géss

v IIIJIIIIIIIIIIIllll‘IlIlIIlllllIIIJIIIIJ

Figure 52: Chromatogram of Soil & Atlas Powermax 440
Post Blast Mixture Prepared with TCE (Trial 2).

 

103
unresolved area beneath.

Figure 53 represents a sample of Trichloroethylene after
being filtered through the Supelco column. A small peak at
14.5 minutes is observed.

Figure 54 represents a sample of Atlas Powermax 440 post—
blast prepared with hexane. Ranging from 11.5-26 minutes is
a series of consecutive peaks with a large unresolved area
beneath this series.

Figure 55 represents a samplerof the individual component
X—5, and a sample of Atlas Powermax 440 that have been

overlaid on the same Chromatogram.

104

 

 

 

 

 

 

.ég
gézg
3:3:

v IIIIIIIIIIIIIIIIIIEIIIIIIIJIIIIIIIIIIII

Figure 53: Chromatogram of TCE Filtrate throught a Supelco
Supelclean LC—Sl column.

 

105

 

 

 

 

 

 

a
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m
3:33

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Figure 54: Chromatogram of Soil & Atlas Powermax 440
Post Blast Mixture Prepared with Hexane.

106

 

 

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100mm
22m

0.0- 30.0 MIN

 

 

 

 

 

 

 

 

 

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figs}!

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Figure 55: Overlay Chromatogram of Individual Component
X—S and Atlas Powermax 440.

 

DISCUSSION

Discussion of Results from Analysis of Individual Components.

Essentially, through gas chromatographic analysis of
emulsion explosives, organic components within the emulsions
will be revealed. The organic materials that are of concern
within emulsion are waxes, oils, and emulsifiers.

Analysis of individual components, that were supplied by
Atlas, on the Gas Chromatograph supplies the standards for
what will be expected when intact and post-blast emulsion

samples are analyzed.

Figure 2: Individual component #1.

This component contains the oils that are present in the
fuel phase of the cap sensitive Powermax fromulations.

Within this Chromatogram appears an unsymmetrical and
unresolved peak between 1 and 5 nunutes. This peak most
likely represents the carbonaceous fuel such as a No. 1 or
No. 2 fuel oil. Because fuel oil ranges from C8—C24 it is a
more volatile oil than that of a vegetable or mineral oil.
Therefore, the larger unsymmetrical and unresolved peak
between 7 and 26 minutes would represent the vegetable or

mineral oil that is less volatile.

107

 

108
Figure 3: Individual component #2.

This component contains the wax and oil combination used
in fuel phase of Atlas’ paper packaged product.

Within this Chromatogram is a series of homologous peaks
that ranges from 7-23 minutes. Since it is known that this
sample represents a wax/oil combination, and that the oils
that are present in the fuel do not generate a series of
homologous peaks, then in conclusion, the homologous peaks
must represent the wax itself. As for the small unresolved
area beneath the peaks this must represent the oils present

where it is partially dominated by the wax.

Figure 4: Individual component X—5.

This component contains the emulsifier combination that
goes with individual component #2.

This Chromatogram is representative of the emulsifier
combination as mentioned above, where Points 1, 2, 3, and 4
are points of interest that will be seen in later figures of

intact emulsion samples.

Figure 5: Individual component #3.

This component contains #2 and X—S in the approximate
proportions in which they are used.

Within. this chromatogranl Points 1, 2, 3, and 4. are
observable, although Point 1 is small. However, these points

do indicate the presence of the emulsifier combination of X—5.

 

 

109
Points 5 and 6 represent the presence of the wax and oil

respectively.

Figure 6: Individual component TN0115.

This component contains the emulsifier used with
individual component #1.

The Chromatogram represented within this figure shows
groupings of peaks with either 4 (n: 5 peaks per group.
Similar smaller groupings will be seen in later figures and

will be labelled as Point 8.

Figure 7: Individual component TN0146.

This component contains the mixture of TN0115 and #1.

The small unsymmetrical and unresolved peak from 1 to 5
minutes most likely represents the carbonaceous fuel found in
component #1, whereas the larger unsymmetrical and unresolved
peak most likely represents a vegetable or mineral oil found
in individual component #1.

Near the end of the Chromatogram, starting approximately
at 23 minutes can be seen 3 groupings of peaks with 4 peaks
per group, labelled as Point 8. Point 8 represents the

individual component TN0115; the emulsifier.

 

110
Discussion of Results from Analysis of Atlas Powermax 140

The Atlas Powermax 140 formulations prepared with
Trichloroethylene and analyzed on the GC show all of the same
characteristics; those being the series of homologous peaks
caused by a paraffinic wax, peaks that are characteristic of
an emulsifier, and some small undefined areas beneath the
peaks that indicate an oil is present.

These chromatograms are consistent.with the chromatograms
of the individual components that show the oils, waxes, and
emulsifiers. Points 1, 2, 3, & 4 show peaks that are
characteristic of the individual component X—5 of the
emulsifier, which. can. be seen in Figure 4. Point 5 is
characteristic of the waxes found in individual component #2,
seen in Figure 3.

The sample of Atlas Powermax 140 in Figure 8 shows a peak
that appears at 17.5 minutes, labelled Point 7. This peak is
not consistent with the other samples of Atlas Powermax 140
prepared. with TCE. It is believed that this peak is a
contaminant arising during preparation of the sample. In
Figures 8 8. 13 the Points 1, 2, 3, & 4 characterize the
emulsifier while Points 5 8: 6 represent the wax and oil
combinations repectively. Figures 17 & 21 also show Points 1,
2, & 4 that represent the emulsifier, and Points 5 & 6
represent the wax and oil respectively.

The 140 sample prepared. with IMethylene Chloride, in

Figure 24, has few distinctive points compared to the other

 

 

111
Powermax 140 samples. What is comparable are points 5 & 6,
which represent the waxes and oils respectively, and Point 3
representing the emulsifier X—5. Due to the injector port
failing to reach 430°C ballistically, the Chromatogram loses
resolution and begins to trail off around 16 minutes.

Figure 28 represents a sample of Powermax 140 prepared
with Hexane. Points 1,2 & 4 are present and indicate that an
emulsifier is present, and again the wax/oil combination can
be seen in points 5 & 6. Once again there is a peak, labelled
Point 7, arising at 17.5 minutes that most likely represents
a contaminant through preparation of the sample.

Another Powermax 140 sample prepared with Hexane is
illustrated in Figure 32. As expected, the emulsifier can be
distinguished from the wax/oil combination by Points 1, 2, &
4, and 5 & 6 respectively.

Figure 43 illustrates a sample of Powermax 140 prepared
with iso—octane, in.which the emulsifier is easily identified
by points 1, 2 & 4, as is the wax/oil combination identified

by points 5 & 6 respectively.

Discussion of Results from Analysis of Atlas Powermax 440

Figure 9 illustrates a sample of Atlas Powermax 440 that
was prepared with TCE. The emulsifier, X-S, is identified by
four specific points within this Chromatogram; points 1, 2, 3
& 4. Points 5 & 6 easily distinguish the wax/oil combination

with Point 6 being more pronounced, indicating a higher oil

 

112
content than that seen in the Powermax 140 samples.

Another Powermax 440 sample, shown in Figure 14 and
prepared. with TCE, distinctively shows Points 2, 3, & 4
representing the emulsifier. Due to the changing of the
millivolt scale during the GC run, Point 1 is not
distinguishable. The wax/oil combination is again
characterized by Points 5 & 6.

Figures 18 & 22 distinctively show the emulsifier by
Points 1, 2, 3 & 4, although Point 3 is not seen in Figure 18.
The ‘wax/oil combination is also 'very distinctive in each
Chromatogram as seen by Points 5 & 6.

Figure 25 represents the Powermax 440 sample prepared
with Methylene chloride. At this point, the injector
temperature was not being achieved, causing the poor
resolution towards the end of the Chromatogram. However, it
is still possible to observe the emulsifier, but only by Point
3. Points 5 & 6 characterize the wax/oil combination once
again.

The remaining samples of Atlas Powermax 440 illustrated
in Figures 29, 33, and 44, prepared with hexane for the first
two and iso—octane for the latter, all show the typical points
as compared to the previous Powermax 440 samples. Although
Point 3 is virtually non—existent in Figure 29, the emulsifier
is still detectable as well as the wax/oil combination.
Again, Point 23 is only slightly observable in Figure 33.

However, the emulsifier and wax/oil combination are

113
distinguishable from one another. Figure 44 unmistakeably
distinguishes the emulsifier from the wax/oil combination,
with point 3 being observable as further characterization of

the emulsifier.

Discussion of Results from Analysis of Atlas Apex 840
Atlas Apex 840 samples prepared with the variety of

solvents produced similar results throughout the GC analysis.
As illustrated in Figures 10, 16, 20, 26, 30, 34, & 45 Atlas
Apex 840 is characterized by its identifiable emulsifier and
wax/oil combination. The only difference is observed in
Figure 10 where a peak, Point 7, appears at approximately 17.5
minutes. Due to the fact that this peak does not appear in
other chromatograms of the Apex 840 product or in
chromatograms of the individual components themselves, it is
concluded that this peak has arisen from contamination during
preparation. Figure 26 has lost resolution near 15 minutes
due to the injector port failing to heat to 450°C
ballistically. The points that characterize the emulsifier
are visable throughout the chromatograms; Points 1, 2, 3, &‘4,
as are the points that characterize the wax/oil combinations;
Points 5 & 6. These samples are similar to the samples of
Atlas Powermax 140, and both are almost identical to the
Chromatogram of individual component #3, which illustrates the
combination of indivdual components #2 and X-5; a wax/oil

combination and emulsifier combination respectively.

114
Discussion of Results from Analysis of Atlas Apex Blasting
Agent 240 gold)

Atlas Apex Blasting Agent 240 (old) was analyzed fewer
times than most of the other emulsion samples since it was
determined that this sample would less likely be found at
criminal bomb scenes, due to the fact that it is not cap
sensitive.

Figures 11, 35, & 46 illustrate the old 240 samples.
These illustrations are almost identical where the emulsifying
package can easily be identified through Points 1, 2, 3, & 4.
However, Point 4 is only observable in Figure 11. In Figure
11 there can also be seen a peak, Point 7, which appears at
approximately 17.5 minutes. Again, this peak is not present
in other Apex 240 samples or individual component samples, and
therefore is most likely the result of contamination during
preparation.

The wax/oil combinations are characterized by Points 5 &
6, and as can be seen, Point 6 has a substantial heighth,
indicating that this emulsion sample has considerably more oil
in its composition than do the Powermax 140 or“ Apex 840

samples.

Discussion of Results from Analysis of Austin Emulex 720

Austin Emulex 720 is a substantially different emulsion,
as composition is concerned, compared to that of the Atlas

products. Figures 12, 15, 19, 23, 27, 31, 36, & 47 illustrate

 

115
this fact.

Essentially the Austin product is a composition of oil
and emulsifier. A wax/oil combination is not indicated here
due to the absence of homologous peaks that dominate other
emulsion samples. Although this is an Austin sample rather
that an Atlas sample it is still similar to the combination of
individual components used by Atlas. From the addition of
indivdual components #1 and TN0115; an oil(s) and emulsifier
respectively, the result is seen in Figure 7 (TN0146), which
is almost identical to all of the Austin samples analyzed.
However it is likely that a different oil combination may have
been used in the Austin sample, but the chromatograms indicate
that the same or similar emlulsifier was used. Austin Emulex
720 is characterized by Points 6, 8, & 9.

Figure 15 shows a sudden change in plotting at 7 minutes
due to a change in the millivolt scale at that time.

Figure 27 lacks any resolution after approximately 15
minutes due to the injector port reaching 450°C at the
beginning of the GC program.

Figure 31 contains a random peak, Point 7, that appears
at approximately 21 minutes. Being that this peak is random
and not found in the other Emulex 720 samples it must have

arisen through contamination of the sample during preparation.

116
Discussion of Results from Analysis of Atlas Apex Blasting
Agent 240 (new)

Three separate samples of Atlas Apex BA 240 (new) were
taken from a different location on the stick of packaged
emulsion.

These samples are illustrated in Figures 37, 38, & 39.
They are characterized by Points 6, 'L 8, & 9 as is the
chromatogranp of Atlas Apex: BA. 240 (old) sample. These
samples do not have the homologous peaks that indicate a wax
is present. These chromatograms only indicate that an oil(s)
and emulsifier are present. It seems as though this newer
sample of Apex 240 has a slightly lesser amount of oil within
its composition as compared to the older sample of Apex 240.

Figures 37 and 38 have a distinctive peak, Point 7,
arising at 21 minutes which has been assumed to be a product
of contamination due to the fact that similar peaks have
appeared randomly throughout analysis of all the different

samples.

Discussion of Results from Analysis of Atlas 7D

Three separate samples of Atlas 7D were prepared with
Hexane, and one sample with iso—octane. The three separate
samples prepared with Hexane were taken from different
locations on the packaged emulsion stick to determine if any
differences in analysis would occur. Figures 40, 41, 42, & 48

illustrate the results of the GC analysis. Atlas 7D can be

 

117
characterized as an emulsion with a wax/oil combination and
emulsifier combination due to Points 5 & 6 and 1, 2, & 4
respectively.

This emulsion is very similar to Atlas Powermax 140 and
Atlas Powermax 840 where neither of the three types of
emulsions appear to have a significant oil composition as they
do a wax composition.

Figures 40, 41, & 42 have a peak, Point 7, that appears
approximately at 21 ndnutes, and although they appear more
times than not, it is still regarded as a product of
contamination due to the lack of a similar peak appearing in

any individual component samples.

Discussion oi Results iiom Analysis oi Post Blast Samples
Figure 49 illustrates a sample of Atlas Powermax 440 that
was manually added to a sample of soil, and tested after
filtration. Most prominent on the Chromatogram is the
appearance of the homologous peaks, Point 5, that indicate a
wax is present. In addition, is the unresolved.peak indicated
by point 6 that suggests an oil(s) is present. There is no
indication that an emulsifier is present because it was
removed during filtration throught the Supelco column.
Figure 50 shows a small series of homologous peaks.
Since this chromatograntillustrates only a soil sample used as
a control it is diffucult to determine what is causing the

peaks other than the possibility of something extracted from

118
the Supelco Supelclean column.

Figure 51 illustrates the GC analysis of a small sample
of 440 post-blast; only 3.15 g of post-blast soil was
extracted. Seeing that the results only yielded a small
series of homologous peaks, much like that of the control
sample, another sample was extracted using 40.75 g of post-
blast soil. Figure 52 illustrates this larger post-blast
sample used in which the series of homologous peaks is more
pronounced, as is the unresolved peak marked.by point 4. This
indicates that a wax/oil combination is most likely present.
But again, there is no indication that an emulsifier is
present, since it was again removed during filtration through
the Supelco column.

Figure 53 illustrates a sample of TCE only that was
filtered through a Supelco Supelclean column to detect if any
contaminants were originating from the column itself.

Figure 54 illustrates the same Atlas Powermax 440 post—
blast sample that was prepared with TCE, that was again
extracted, but with Hexane. Points 5 & 6 respectively mark
the indicators of a wax and oil combination within the
emulsion. The emulsifiers were removed during filtration

through the Supelco column.

Discussion of Basic Methodology, Including Solvents.

The resulting chromatograms do not reveal that any one

solvent has extracted the emulsion samples better than the

119
other. In my opinion, any of the solvents used within this
thesis will adequately extract the samples, however, the
solvents should not be relied upon to perform.all the work in
breaking up the emulsion. To extract as much of the emulsion
as possible, a homogenizer will perform an excellent job.
Filtration through a Whatman Autovial will remove all solid
materials leaving an extract which can then be evaporated
(concentrated) down to approximately 2ml. This extract is

then ready for injection into the gas Chromatograph.

CONCLUS I ON

The purpose of this thesis experiment was to obtain gas
Chromatographic analyses of individual components in emulsion
explosives, of intact emulsion explosives, and of post blast
emulsion residues. The resulting chromatograms provided the

necessary information to determine, if different intact
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results that indicate two samples cannot be from the same
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not be indistinguishable. In this regard, it can be said that
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individualizing emulsions to a specific brand. However, in.my

opinion, GC analysis can be used as a confirmatory test when

120

CONCLUS I ON

The purpose of this thesis experiment was to obtain gas
chromatographic analyses of individual components in emulsion
explosives, of intact emulsion explosives, and of post blast
emulsion residues. The resulting chromatograms provided the
necessary information to determine if different intact
emulsion samples can be distinguished.frongeach other; if post
blast emulsion samples can be identified as emulsions and to
one particular intact emulsion sample.

Chromatograms of intact samples can be used to
characterize each sample as an emulsion since the
characteristics of the individual components are revealed
within the chromatograms. However, the chromatograms cannot
be used to distinguish between one manufacturer or brand of a
particular emulsion since the components of many emulsions are
similaru In certain. instances the Chromatograms reveal
results that indicate two samples cannot be from the same
source, where other chromatograms of two different samples may
not be indistinguishable. In this regard, it can.be said.that
GC analysis can only be used as a screening test when
individualizing emulsions to a specific brand. However, in my

opinion, GC analysis can be used as a confirmatory test when

120

121
identifying an explosive as an emulsion, but not to
individualize the emulsion to a particular manufacturer or
brand.

GC analysis of post blast emulsion residues detected the
wax and oil combination used within the intact emulsion
sample, however the emulsifiers were not detected since they
were removed during separation in a Supelco column. The
experimentation completed within this thesis showed that post
blast emulsion residues were detected by GC when residues were
extracted from a large amount (40—50 grams) of soil. Residues
extracted from a smaller amount (3—5 grams) of soil were not
detected such that they were clearly defined. Consequently,
post blast residues may not always be detected through GC
analysis, depending upon the amount of sample available.

Accordingly, from. the results, GC analysis is an
excellent tool for identifying an intact explosive sample as
an emulsion. Through the use of other analytical techniques,
such.as ion chromatography (IC), spot tests, flame tests, and
SEM/EDX in conjunction with gas chromatography, more precise
data can be obtained to make conclusive identifications of
post blast samples. However, it will always be difficult, if
not impossible, to individualize intact samples and especially
post blast samples to a particular manufacturer.

For forensic scientists and criminal investigators,
identification of the explosive will prove to be satisfactory

in. most instances. Individualizing the explosive to a

122

particular manufacturer or brand.becomes unnecessary in light
of other evidence that can corroborate a suspects connection
xmhfli a certain case. Galvanized pipes, intact explosive
residues, packaging that contained explosives, separate
ingredients used to make explosives, tape, wire, blasting
caps, timing' devices, etc., are all items that can be used as
corroborative evidence.

In conclusion, the research presented here provides a
basic methodology for analyzing emulsions using a gas
Chromatograph, and data that providedevidence that explosives
can be identified as emulsions by their component
characteristics. Future considerations for research on
emulsions should include analysis by gas chromatography
coupled with mass spectrometry (GC-MS). This analytical
analysis should provide results that can be used to confirm
the presence of an emulsion explosive from post blast samples.
However, GC-MS will not be able to provide individualizable
results as to who the manufacturer might be. Therefore, it
would be extremely helpful for forensic chemists if
manufacturers would agree to produce emulsions with an
identifier. For example, taggets are placed within smokeless
powder which allows identification of the manufacturer. If
this method could be repeated for emulsions, the forensic
science community could.greatly benefit in its cases involving
emulsions. Until then, relying upon GC and. previously

mentioned analytical techniques will prove to produce results

123

that will be accurate, reliable, and upheld in a court of law.

BIBLIOGRAPHY

Bender, E.C., Crump, J., & Midldff, C.R. Jr. (1992, September). The Instrumental

Analysis of Inatact and Post Bla_st Wgter Gel ind Emulsion Explosives. Paper

presented at the 4th International Symposium of Analysis and Detection of Explosives,
Jerusalem, Israel.

Beveridge, A.D., Greenlay, W.R.A., & Shaddick, RC. (1983). Identification of
Reaction Products in Residues from Explosives. Proc. Inp Svmp. Angeli. Det. Explos.
(pp. 53-58). March 29-31. FBI, Quantico, Virginia.

Bluhm, H.F. Ammonium Nitrate Emulsion Blasting Agent a_nd Mejhod of Preparing
Same. US 3,447,978 (1969) Assigned to Atlas Chemical Industries.

Brockington, J .W. Water-in-Oil NCN Emulsion Blasting Agent. US 4,218,272
(1980) Assigned to Atlas Powder Co.

Department of the Treasury, Bureau of Alcohol, Tobacco, and Firearms. (1990).
Explosives Incident Report.

Hayes, TS. (1981). A Systematic Procedure for the Identification of Post-Explosion
Samples of Commercial Blasting Explosives. J. Forensic Sci. Soc. 2_l, pp. 307-316.

 

Hoffman, C.M., M.S. & E.B. Byall (1974). Identification of ExplosiveResidues in
Bomb Scene Investigations. J. Forensic Sci. 19(1), pp. 54-63.

 

Hopler, RB. (1991). Histog and Development of Packaged Explosives, Proggessing
from Nobel’s Inventions to the Recent Introduction of Emulsions. Ireco Incorporated.

Unpublished manuscript.

Kaye, S.M. Slu_rg Explosives. Encyclopedia of Explosives and Related Items
Volume 9 PATR 2700, USAARDC. Dover, NJ. 1980. pp. 8121-8147.

Midkiff, C.R. & Walters, A.N. 81m and Emulsion Explosives: New Tools for

Terrorists, New challenges for Detection and Identification. Manuscript submitted for
publication.

124

125

Parker, R.G. (1975). Analysis of Explosives and Explosive Residues. Part 3:
Monomethylamine Nitrate. J. Forensic Sci. 20(2), pp. 257-260.

Parker, R.G., Stephenson, M.D., McOwen, J.M., & Cherolis, IA. (1975). Analysis of
Explosives and Explosive Residues. Part 1: Chemical Tests. J. Forenjsic Sci.. 201 1 1,.
pp. 133-140.

 

Reutter, D.J. & Buechele, RC. (1983). Ion Chromatograph of Explosives and
Explosive Residues. Proc. Int. Sy1_np. Anal. Det. Explos. pp. 199-207. March 29-31.
FBI, Quanticao, Virginia.

Reutter, D.J., Buechele, R.C., & Rudolph, TL. (1983). Ion chromatography in
Bombing Investigations. Analfl'cal Chemisgy, 55114), pp. 1468A-1472A.

Rudolph, T.L. & Bender, EC. (1983). A SCheme for the Analysis of Explosives and
Explosive Residues. Proc. Int. Sm. Anal. Det. Explos. pp. 71-78. March 29-31.
FBI, Quantico, Virginia.

Wade, C.G. Water-in-Oil Emulsion Explosive Composition. US 4,110,134 (1978)
Assigned to Atlas Powder Co.

 

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