Investigation of Explosions E Evidence

84
Investigation of explosions
by
Alexander D Beveridge BSc, LLB, MBA, PhD, FCIC.
Sarah J Benson BSc PhD
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84 - 1
2013 THOMSON REUTERS
Author information
Alexander (Sandy) Beveridge is a consultant forensic chemist and lawyer in
Vancouver, BC, Canada. He spent over 30 years in the Forensic Science Service of
the Royal Canadian Mounted Police, heading the Chemistry Sections in the Edmonton
and Vancouver Laboratories. He is a graduate of the Universities of Glasgow (BSc,
PhD), Alberta (MBA) and British Columbia (LLB). He has held chemistry research
fellowships at the Universities of British Columbia, Western Ontario and Cambridge,
and is a Fellow of the Chemical Institute of Canada.
Sandy is editor of Forensic Investigation of Explosions 2nd Edition (CRC Press, Taylor
and Francis Group, Boca Raton, FL 2012) which reects his long-term interest in this
eld. He has extensive case work experience in domestic and international
investigations of explosions, has testied many times as an expert witness and enjoys
his more recent legal perspective of the eld.
Sarah Benson works with the Forensics portfolio of the Australian Federal Police.
Sarah currently holds the title of Coordinator Criminalistics, where she leads and
manages the Chemical Criminalistics, Document Sciences and Firearms Identication
and Armoury Teams. Sarah joined the AFP in January 2000 upon graduation from the
University of Technology, Sydney (UTS) with a Bachelor of Science (Honours) in
Applied Chemistry Forensic Science.
Sarah has gained signicant experience in the eld of forensic investigation of
explosions, in both the eld and laboratory. Sarahs experience has been drawn
through deployments to Indonesia and the Philippines to assist local authorities with
the examination of post-blast scenes and the subsequent laboratory support in these
matters. Sarah has also played a key role domestically in Australia in developing
guidelines for the examination of secondary scenes in relation to explosive incidents.
Sarah also has a keen interest in research and development in the Chemical
Criminalistics eld, in particular the eld of explosives, which was highlighted through
her PhD thesis titled Introduction of Isotope Ratio Mass Spectrometry (IRMS) for the
Forensic Analysis of Explosives (through the UTS).
We are delighted to announce that the Panel of Advisers of the National Institute
of Forensic Science awarded the 2010 Best Chapter in a Publication in the
Forensic Sciences to this Chapter.
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INTRODUCTION.............................................................................................................. [84.10]
EXPLOSIONS...............................................................................................................................
Classication of explosions ............................................................................................... [84.100]
Mechanical .................................................................................................................... [84.110]
Nuclear.......................................................................................................................... [84.120]
Chemical ....................................................................................................................... [84.130]
Propagation ....................................................................................................................... [84.160]
Deagration................................................................................................................... [84.170]
Detonation..................................................................................................................... [84.180]
Order.................................................................................................................................. [84.200]
Effects................................................................................................................................ [84.220]
Pressure........................................................................................................................ [84.230]
Fragmentation............................................................................................................... [84.240]
Thermal ......................................................................................................................... [84.250]
EXPLOSIVES................................................................................................................................
Classication of explosives ............................................................................................... [84.300]
Low explosives ............................................................................................................. [84.320]
High explosives............................................................................................................. [84.330]
Blasting agents ............................................................................................................. [84.340]
Initiation of explosives ....................................................................................................... [84.370]
The explosive initiation train......................................................................................... [84.380]
Detonators, fuses and boosters ................................................................................... [84.390]
Chemistry of explosives..................................................................................................... [84.400]
Chemical classications................................................................................................ [84.410]
Oxygen balance............................................................................................................ [84.420]
Chemical reactions ....................................................................................................... [84.430]
Product formulations..................................................................................................... [84.460]
Propellants (including black powder and smokeless powders)............................... [84.470]
Pyrotechnics............................................................................................................. [84.480]
Commercial explosives ............................................................................................ [84.500]
Dynamite ............................................................................................................. [84.510]
Blasting agents.................................................................................................... [84.520]
Slurries ................................................................................................................ [84.530]
Emulsions............................................................................................................ [84.540]
Military explosives (including plastic explosives)..................................................... [84.570]
Improvised explosives.............................................................................................. [84.600]
IMPROVISED EXPLOSIVE DEVICES....................................................................... [84.700]
Components ...................................................................................................................... [84.710]
Initiation ............................................................................................................................. [84.730]
Delay initiation .............................................................................................................. [84.740]
Victim initiation.............................................................................................................. [84.750]
Command initiation....................................................................................................... [84.760]
PRE-BLAST INVESTIGATION.................................................................................... [84.900]
POST-BLAST INVESTIGATION ................................................................................. [84.950]
Command and control ....................................................................................................... [84.960]
Police criminal investigation .............................................................................................. [84.970]
Forensic investigation........................................................................................................ [84.980]
FIELD EXAMINATION.................................................................................................. [84.990]
Post-blast scene examination teams ................................................................................ [84.990]
Post-blast scene examiner .................................................................................... [84.1000]
Forensic chemist .................................................................................................... [84.1010]
Protocols at the scene of an explosion........................................................................... [84.1050]
Primary scenes ...................................................................................................... [84.1060]
Emergency response and Search and Rescue..................................................... [84.1070]
Contamination prevention procedures................................................................... [84.1080]
Site safety and clearance ...................................................................................... [84.1090]
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Scene appreciation phase...................................................................................... [84.1100]
Scene assessment phase ...................................................................................... [84.1110]
Scene examination phase...................................................................................... [84.1120]
Analytical phase ..................................................................................................... [84.1130]
Secondary scenes.................................................................................................. [84.1170]
LABORATORY EXAMINATION................................................................................ [84.1200]
Forensic disciplines ......................................................................................................... [84.1210]
Identication materials ........................................................................................... [84.1230]
Fingerprints ............................................................................................................ [84.1240]
DNA........................................................................................................................ [84.1250]
Hair......................................................................................................................... [84.1260]
Physical and trace evidence.................................................................................. [84.1270]
Document examination .......................................................................................... [84.1280]
Metallurgy............................................................................................................... [84.1290]
Damage.................................................................................................................. [84.1290]
Toolmarks/serial number restoration...................................................................... [84.1300]
Pathology ............................................................................................................... [84.1325]
Analysis and identication of explosives......................................................................... [84.1350]
Examination of debris and analytical preparation ................................................. [84.1360]
Vapour analysis for volatile organics ..................................................................... [84.1370]
Visual/microscopical examination for explosives and other trace evidence ......... [84.1380]
Swabs and solvent extraction of debris for trace explosives ................................ [84.1390]
Clean-up procedures ............................................................................................. [84.1400]
Chemical and instrumental analysis ...................................................................... [84.1410]
Bulk explosives ...................................................................................................... [84.1420]
Organic extracts..................................................................................................... [84.1430]
Inorganic extracts................................................................................................... [84.1440]
Insoluble material ................................................................................................... [84.1450]
Identication and interpretation.............................................................................. [84.1510]
Propellants ............................................................................................................. [84.1520]
Black powder and black powder substitutes ......................................................... [84.1530]
Smokeless powders............................................................................................... [84.1540]
Pyrotechnics........................................................................................................... [84.1550]
Commercial explosives .......................................................................................... [84.1560]
Military explosives.................................................................................................. [84.1570]
Improvised explosive mixtures............................................................................... [84.1580]
Fertiliser based improvised explosives.................................................................. [84.1600]
Inorganic salt improvised mixtures ........................................................................ [84.1630]
Nitromethane.......................................................................................................... [84.1640]
Peroxide explosives ............................................................................................... [84.1650]
Reporting................................................................................................................ [84.1700]
QUALITY ASSURANCE............................................................................................. [84.1750]
Accreditation.................................................................................................................... [84.1760]
Contamination prevention................................................................................................ [84.1770]
Control samples............................................................................................................... [84.1780]
Environmental/background controls.................................................................. [84.1790]
Matrix/substrate controls ................................................................................... [84.1800]
Reference samples.......................................................................................................... [84.1810]
Analytical and quality control samples ............................................................................ [84.1820]
CASE STUDY FORENSIC CHEMISTRY IN A COMPLEX PROSECUTION
BASED ON CIRCUMSTANTIAL EVIDENCE.................................................... [84.1900]
Introduction ................................................................................................................. [84.1910]
Jurisdiction.................................................................................................................. [84.1920]
Response teams......................................................................................................... [84.1930]
The scene................................................................................................................... [84.1940]
Forensic chemistry...................................................................................................... [84.1950]
1. Pre-lab ............................................................................................................... [84.1960]
2. Forensic examinations....................................................................................... [84.1970]
3. Initial forensic opinions to investigators............................................................. [84.1980]
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4. Forensic reports to investigators ....................................................................... [84.1990]
5. Consultation with prosecution............................................................................ [84.2000]
6. Organisation of testimony.................................................................................. [84.2010]
7. Testimony as expert witness.............................................................................. [84.2020]
Trial ............................................................................................................................. [84.2030]
Verdict ......................................................................................................................... [84.2040]
CASE STUDY THE BALI BOMBINGS (12 OCTOBER, 2002) ....................... [84.2080]
The incident ................................................................................................................ [84.2090]
The response.............................................................................................................. [84.2100]
The scenes.................................................................................................................. [84.2110]
Paddys Bar............................................................................................................ [84.2120]
Scene interpretation.......................................................................................... [84.2130]
Physical evidence ............................................................................................. [84.2140]
Explosive residue analysis................................................................................ [84.2150]
Device reconstruction........................................................................................ [84.2160]
Identication material ........................................................................................ [84.2170]
Sari Club ................................................................................................................ [84.2180]
Scene interpretation.......................................................................................... [84.2190]
Physical evidence ............................................................................................. [84.2200]
Explosive residue analysis................................................................................ [84.2210]
Device reconstruction........................................................................................ [84.2220]
Identication material ........................................................................................ [84.2230]
Secondary scenes ................................................................................................. [84.2240]
Other aspects ............................................................................................................. [84.2250]
Legal outcomes .......................................................................................................... [84.2260]
Summary ......................................................................................................................... [84.2270]
Acknowledgments....................................................................................................... [84.2280]
APPENDIX A: ANALYTICAL TECHNIQUES FOR THE ANALYSIS OF
EXPLOSIVES........................................................................................................... [84.2310]
Non-instrumental techniques Chemical colour tests (spot tests) and thin layer
chromatography ..................................................................................................... [84.2320]
Chromatography .............................................................................................................. [84.2330]
Gas chromatography (GC) ......................................................................................... [84.2340]
Detection................................................................................................................ [84.2350]
Flame ionisation detectors (FID)....................................................................... [84.2360]
Electron capture detectors (ECD) ..................................................................... [84.2370]
Chemiluminescent detectors (CL)..................................................................... [84.2380]
Mass spectrometers (MS) ................................................................................. [84.2390]
High performance liquid chromatography (HPLC) ..................................................... [84.2420]
HPLC: Partition chromatography ........................................................................... [84.2430]
Detectors................................................................................................................ [84.2440]
Ion chromatography (IC)............................................................................................. [84.2500]
Electrophoresis: Capillary electrophoresis (CE).............................................................. [84.2510]
Spectrometry ................................................................................................................... [84.2520]
Mass spectrometry (MS)............................................................................................. [84.2530]
Ion mobility spectrometry (IMS).................................................................................. [84.2540]
Isotope ratio mass spectrometry (IRMS).................................................................... [84.2550]
Spectroscopy ................................................................................................................... [84.2560]
Infrared spectroscopy (IR) .......................................................................................... [84.2570]
Raman spectroscopy .................................................................................................. [84.2580]
Elemental analysis........................................................................................................... [84.2590]
Scanning electron microscopy/energy dispersive x-ray spectroscopy (SEM/EDX or
SEM/EDS) .............................................................................................................. [84.2600]
Micro x-ray uorescence spectroscopy (XRF) ........................................................... [84.2610]
X-ray powder diffraction (XRPD) ................................................................................ [84.2620]
TABLE OF CONTENTS
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Portable explosive detection instruments........................................................................ [84.2630]
BIBLIOGRAPHY
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[The next text page is 84-7]
INSTRUMENTS/TECHNIQUES
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Instruments/techniques
CE....................................................capillary electrophoresis
CI .....................................................chemical ionisation
CL....................................................chemiluminescence
ECD.................................................electron capture detector
EDX.................................................energy dispersive x-ray spectroscopy
EI .....................................................electron impact ionisation
FID...................................................ame ionisation detector
FTIR ................................................Fourier transform infrared spectroscopy
GC....................................................gas chromatography
HPLC...............................................high performance liquid chromatography
IC.....................................................ion chromatography
IMS..................................................ion mobility spectrometry
IR.....................................................infrared spectroscopy
MEKC..............................................micellar electrokinetic chromatography
MIC..................................................microscopical examination
MS ...................................................mass spectrometry
PGC .................................................pyrolysis gas chromatography
PMDE..............................................pendant mercury dropping electrode
SEM.................................................scanning electron microscopy
SFC..................................................supercritical uid chromatography
TEA..............................................thermal energy analyser (chemiluminescent detector)
TLC..................................................thin layer chromatography
UV ...................................................ultraviolet
XRPD ..............................................x-ray powder diffraction
ABBREVIATIONS
Explosives
AN ...................................................ammonium nitrate
ANFO..............................................ammonium nitrate / fuel oil
Black powder ..................................potassium nitrate/sulphur/charcoal
DADP ..............................................diacetone diperoxide
DATB...............................................1,3-diamino-2,4,6-trinitrobenzene
DCDA..............................................dicyanodiamide
DNT.................................................dinitrotoluene
DPA .................................................diphenylamine
EC....................................................ethyl centralite
EGDN..............................................ethylene glycol dinitrate
HMTD .............................................hexamethylene triperoxide diamine
HMX................................................high melting explosive; octahydro-1,3,5,7-tetranitro-1,3,
5,7-tetrazocine; cyclotetramethylene tetranitramine
MATB..............................................1-mono-amino-2,4,6-trinitrobenzene; picramide; 2,4,6-
trinitroaniline
MC...................................................methyl centralite
MMAN............................................mono methyl ammonium nitrate
NC....................................................nitrocellulose
NG ...................................................nitroglycerine; 1,2,3propanetriol trinitrate
PETN...............................................pentaerythritol tetranitrate
RDX.................................................1,3,5trinitrohexahydroStriazine; cyclotrimethylene
trinitramine
Semtex .............................................RDX and PETN
TATB ...............................................1,3,5-triamino-2,4,6-trinitrobenzene
TATP................................................triacetone triperoxide
TNT .................................................2,4,6trinitrotoluene
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Organisations
AFP..................................................Australian Federal Police
ASCLD/LAB...................................American Society of Crime Laboratory Directors/
Laboratory Accreditation Board
ATF..................................................Alcohol, Tobacco and Firearms; Bureau of Alcohol,
Tobacco, Firearms and Explosives (a branch of the US
Treasury which handles explosives casework)
DRA.................................................Defence Research Agency (United Kingdom)
Dstl ..................................................Defence Science and Technology Laboratory (United
Kingdom)
FBI...................................................Federal Bureau of Investigation (United States of America)
INP...................................................Indonesian National Police
NATA...............................................National Association of Testing Authorities
NRIPS..............................................National Research Institute for Police Science (Japan)
NFPA...............................................National Fire Protection Association (United States of
America)
RCMP..............................................Royal Canadian Mounted Police
UKAS ..............................................United Kingdom Accreditation Service
ORGANISATIONS
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Other
BLEVE............................................boiling liquid expanding vapour explosion
DVI ..................................................disaster victim identication
IED ..................................................improvised explosive device
OH&S..............................................occupational health and safety
PBX .................................................polymer bonded explosives
SPME...............................................solid phase micro extraction
VBIED.............................................vehicle-borne improvised explosive device
VOD ................................................velocity of detonation
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INTRODUCTION
[84.10] A useful denition of the term explosion is provided in the publication NFPA
921 (2011, 921-13):
The sudden conversion of potential energy (chemical or mechanical) into kinetic energy
with the production of and release of gases under pressure, or the release of gases under
pressure. These high pressure gases then do mechanical work such as moving, changing or
shattering nearby materials.
An explosion may occur naturally (eg, the eruption of a volcano), accidentally (eg, the
mechanical explosion of a container due to a build up of excessive pressure) or intentionally
(eg, commercial blasting for mining; military use in munitions; or illegal use in improvised
explosive devices (IED). The effects of the mechanical work will always be observed and may
aid commercial, military or illegal applications. This chapter addresses primarily the illegal use
of explosives and the forensic investigation of such events. A systematic approach to the
investigation of explosions can recover much useful evidence from a post-blast scene. The
most effective investigations of major incidents are often conducted by multi-disciplinary
teams which are brought together as required by the individual circumstances of the incident.
The teams may include experts in post-blast scene examination, device reconstruction,
explosive residue and trace chemical analysis, and others such as pathologists, ngerprint
experts and metallurgists.
When an explosion occurs, a series of underlying questions are asked by the investigating
authorities, including:
did an explosion occur?
what caused the explosion?
is this a clandestine laboratory for manufacturing explosives or IEDs?
who was responsible for the explosion?
how can future incidents of this type be prevented?
This chapter provides an overview of the key aspects of a post-blast forensic investigation that
directly assist in providing answers to the aforementioned questions. Overviews are provided
on:
(1) the nature and classication of explosions and explosives;
(2) the post-blast investigative process including:
post-blast scene examination protocols, including recognition and recovery
of pertinent physical and trace evidence at the scene of an explosion;
scientic disciplines/specialists that may be involved;
laboratory analysis protocols for recovered items, with an emphasis on the
analysis and identication of explosive residues;
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interpretation and reporting of results; and
(3) case studies highlighting the key phases of a forensic post-blast investigation.
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EXPLOSIONS
Classication of Explosions
[84.100] There are three distinct types of explosions: mechanical, nuclear and chemical.
Yinon (1999), Thurman (2011) and Hopler (2012) provide detailed discussions on the
properties and classication of common explosives and explosions.
Mechanical
[84.110] A mechanical explosion is often the result of container failure, for example, the
rupture of a steam boiler under excessive pressure. In the event of a mechanical explosion, no
chemical reaction occurs.
A particularly dramatic example of a mechanical explosion is a boiling liquid expanding
vapour explosion (BLEVE) in which a liquid under pressure above its boiling point is released
by the failure of the container and almost instantly vaporises. BLEVEs can be produced from
objects as small as butane cigarette lighters and aerosol cans to containers as large as railway
tank cars. If the liquid is ammable, then a re almost invariably results. Mechanical
explosions are not covered further in this chapter. A useful discussion of the topic may be
found in NFPA 921 (2011, Ch 21).
Nuclear
[84.120] Nuclear explosions involve splitting the nucleus of atoms (referred to as
ssion), as occurs in an atomic bomb. Alternatively, nuclear explosions involve the
combination of atomic nuclei (referred to as fusion), as occurs in the sun and hydrogen
bombs. Nuclear explosions are not covered in this chapter; however, useful discussions of
these types of explosions may be found in Barnaby (2004), Shiga (2009) and Thurman (2011).
Chemical
[84.130] Chemical explosions involve the rearrangement of atoms in the molecules of an
explosive compound or a mixture of compounds. These rearrangements produce more stable
chemical compounds (primarily gases) through reactions which give off heat (exothermic) and
do work (move things). The reactions are generally oxidation / reduction processes (ie a
chemical change where one reactant loses electrons (oxidation) and another gains electrons
(reduction). Chemical explosions may be initiated by shock, friction, heat and ame. The focus
of this chapter will be on the forensic investigation of events resulting from chemical
explosions.
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Propagation of Chemical Explosions
[84.160] Propagation of the chemical reaction proceeds by one of two mechanisms:
deagration or detonation.
Deagration
[84.170] Deagration is very rapid burning in which the ame front travels through the
unreacted explosive at a speed less than the speed of sound (ie less than 1000 metres per
second). Explosives which typically react by deagration are called low explosives. They are
characterised by a relatively slow rate of pressure increase (also referred to as velocity of
detonation (VOD)) and normally have to be conned in order to explode that is, to release
gases violently into the environment by container rupture.
Detonation
[84.180] Detonation is a chain reaction in which a shock wave travels through the
unreacted explosive at very high pressures and temperatures and faster than the speed of
sound. The shockwave compresses and heats the particles of the main charge (eg, ammonium
nitrate/fuel oil (ANFO) mixture) to a temperature above its decomposition temperature. As a
result, the explosive compound or mixture undergoes an exothermic chemical decomposition
(ie material is rapidly converted into reaction products and produces heat) just behind the wave
front in the chemical reaction zone. This process accelerates the shockwave due to the large
amounts of heat and gas generated referred to as the heat of explosion. This raises the
internal pressure which adds to the high pressures at the front of the wave. The pressure and
temperature in the detonation zone can exceed several hundred thousand atmospheres and
3000C (Mohanty, 2012; Akhavan, 2011). Figure 1 illustrates this detonation process.
Figure 1 Diagram illustrating an instantaneous time lapse of the detonation
process (adapted from Mohanty, 2012)
Explosives which are initiated by detonation are called high explosives. High explosives do
not need to be conned to explode. When such a solid or liquid explodes, the volume can
increase 10,000 to 15,000 times and the gases can expand between 1500 and 9000 metres per
second (referred to as the VOD). Detonation can be achieved by burning to detonation or by an
EXPLOSIONS [84.180]
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initial shock. The reaction occurs almost instantaneously through the bulk of the material
(Urbanski and Vesudeva, 1981; Akhavan, 2011). If the velocity of the shockwave is less than
the velocity of sound, deagration is said to occur.
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Order
[84.200] Explosions may be classied by resultant damage as low order or high order.
If the rate of deagration reaches between 1000 and 1800 metres per second, the reaction may
be classed as a low order detonation. If the rate increases to 5000 metres per second, the
detonation is classed as a high order (Akhavan, 2011).
In a low order explosion there is a relatively low rate of pressure rise that results in large
objects being pushed short distances for example, a fuel/air explosion in a house causes
window frames to be blown out with the glass intact, walls may be bulged and the roof lifted.
In a high order explosion, there is a very rapid rate of pressure rise which shatters the
surroundings and produces small fragments of material which travel considerable distances at
high velocity.
Fuel/air mixtures, in which the fuel is typically hydrocarbon(s) and the oxidiser is oxygen, can
only explode within upper and lower explosive limits. If the mixture contains not enough fuel,
then it is referred to as a lean mixture and if there is too much fuel in the mixture, then it is
referred to as rich. The proportion of the fuel to air must be in the correct range for the
particular fuel type to result in an explosion. Near the limits, such mixtures produce low
order explosions, but may produce high order effects at stoichiometric (optimal)
concentrations. The explosive limits for gasoline/air are approximately 1.7 to 9.7 per cent by
volume in air and for acetylene/air the range is approximately 2.5 to 82 per cent by volume in
air. With respect to these two fuel types, it would generally be easier to create an explosive
mixture utilising acetylene as opposed to gasoline, due to the wide range in which acetylene is
potentially explosive (ie 2.5 to 82 per cent).
Confusingly, the term low order is also used to describe a misre or partial detonation of
a high explosive and high order can be used to indicate detonation at maximum possible
velocity.
EXPLOSIONS [84.200]
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Effects
[84.220] The three major primary effects of an explosion are the pressure (shock) wave,
fragmentation and heat. Secondary blast effects may result from the reection, focusing and
shielding of the shockwave and structural res. The physics of explosions has been described
in detail by Mohanty (2012).
Pressure
[84.230] Most explosion damage is caused by the blast pressure wave (the positive phase)
which is often referred to as the shockwave. The pressure generated in the shockwave is
positive in nature and is referred to as the overpressure (or the positive phase). There is also a
less strong returning (or negative) phase caused by lling of the partial vacuum produced by
the gases rushing outwards (Mohanty, 2012).
Pressure is measured as force per unit area. There are several different scales. The standard unit
is the kilopascal (kPa). Some other units still in use are: atmospheres, bars, millibars, torrs,
millimetres (mm) of mercury and pounds per square inch (psi).
Conversion factors are:
1 atmosphere = 760 mm of mercury = 760 torr = 101.3 kPa = 1013 millibars = 1.013 bar =
14.7 psi.
Some examples of the effect of peak external blast overpressure damage on building structures
are:
windows broken : 37 kPa
concrete walls, unreinforced : 1420 kPa
snap wooden utility poles : 34 kPa
overturn rail cars : 48 kPa
building demolished : 69 kPa
source: NFPA 921 (2011 Ch 21).
Fragmentation
[84.240] When a container or other components of a device (eg, power supply or shrapnel)
are shattered or fragmented by an explosion, the resultant high-velocity fragments are referred
to as primary fragments. These primary fragments can produce extensive damage and injuries
and can also generate secondary fragments from surrounding surfaces/objects. Primary
fragments (and sometimes secondary fragments) may bear explosive residues and the damage
alone can provide an important indicator of the type of explosive used (Strobel, 2012, Ch 5).
Post-blast scene examiners use primary fragmentation to assist in determining the cause of an
explosion.
Shrapnel refers to items or material included in the device construction specically for the
purpose of causing maximum damage, injuries and/or fatalities. Shrapnel can be in the form of
metal items inserted into the container (such as nails, bolts, screws) or actually form part of the
EXPLOSIONS [84.240]
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device container itself such as a hand grenade. The metal casing of a hand grenade is designed
to break apart at the weakest points upon explosion, ultimately generating small pieces of
primary fragmentation which act as shrapnel.
Thermal
[84.250] The high temperature of an explosion reaction can ignite the surroundings. This
is particularly true of deagrating explosives which react at a lower temperature than high
explosives but for a longer time. Detonating explosives can cause a delayed re by initiating
smouldering. This frequently occurs with car bombs.
Fire can destroy evidence, but re suppression can also be a problem not only because many
explosive residues are water soluble and the saturation with water may wash vital evidence
away, but also because chemical re extinguisher powders may contain ions (charged atoms or
compounds) which occur in residues from particular types of explosives. These ions include
sodium [Na
+
], ammonium [NH
4
+
] and bicarbonate [HCO
3
-
]. Therefore, it is important to
educate re departments of the need for minimum suppression at explosion scenes and for
scientists to be aware of re suppression methods and chemicals used at the scene.
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EXPLOSIVES
Classication of Explosives
[84.300] Explosives can be classied using a number of properties eg, rate of reaction,
chemical composition, or their end use/application. A common way to classify explosives is by
the rate of reaction that is as low (generally deagrating) or high (detonating) explosives.
Low explosives
[84.320] Low explosives burn rapidly when ignited by ame or spark, and if conned, can
explode to rupture and fragment the container (for example, pipe bombs). The reaction front
typically moves through the unreacted explosive at less than the speed of sound (ie
1000 metres/second). Examples are propellant powders (including pistol, rie and shotgun
smokeless powders, and traditional black gunpowder), improvised chemical mixtures (for
example, chlorate/sugar) and pyrotechnic compositions (for example, reworks). However,
some of these examples, when conned and initiated with a detonator, can react by detonation
(Oxley et al, 2001; Bender and Beveridge, 2012).
The low explosives classication also includes dispersed explosive mixtures such as fuel/air
and dust/air mixtures which typically deagrate; that is, there is a denable ame front which
propagates the explosion.
The effects of the mechanical work from low explosives are pushing rather than shattering of
surrounding objects/surfaces.
High explosives
[84.330] In high explosives, the reaction front moves through the unreacted explosive at
greater than the speed of sound. High explosives may be subdivided into primary and
secondary explosives.
Primary high explosives
Primary high explosives are extremely sensitive and may be initiated (ie detonated) by heat, as
well as by shock and friction without connement. Detonation velocities are generally between
3500 and 5500 metres per second. The principal commercial use is in detonators. Examples are
lead styphnate (lead trinitroresorcinate) and lead azide in commercial detonators and mercury
fulminate and triacetone triperoxide (TATP) in improvised detonators. Primary explosives are
generally used in initiating devices as opposed to the explosive main charge (refer to Figure 2)
but peroxide explosives are an exception (Akhavan, 2011; Yeager, 2012).
Secondary high explosives
Secondary high explosives explode without connement when initiated by shock from a
primary explosive (eg, detonator). Their detonation velocities are generally between 5500 and
9000 metres per second. Examples include commercial dynamites, slurries, emulsions,
Update: 73
84 - 5051
detonating cords, and military and plastic explosives (Hopler, 2012). Specic explosive
compounds include EGDN, NG, TNT, tetryl, RDX, HMX and PETN.
The detonation of high explosives is characterised by high pressures and a very rapid rate of
pressure rise which shatters the surroundings.
Blasting agents
[84.340] The term blasting agent refers to explosives (such as ammonium nitrate / fuel
oil mixtures (ANFO)) that are utilised for commercial applications such as mining and
demolition. These explosives are commercially manufactured and sold in bulk quantities. They
are occasionally referred to as tertiary explosives because they cannot normally be detonated
with a detonator and in common applications require detonation with secondary high
explosives which act as boosters (refer to Figure 2).
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Initiation of Explosives
[84.370] Commercial and military explosives are initiated by detonators, fuses and
boosters. These are discussed in the following sections. Improvised explosive devices may
similarly be initiated, but more commonly employ improvised initiation systems such as a
homemade detonator containing TATP or HMTD.
The explosive initiation train
[84.380] The explosive initiation train assists in explaining chemical explosions and the
classication of explosives. Figure 2 illustrates a schematic three-step explosive train for an
explosive main charge such as blasting agent.
A primary high explosive in a detonator (eg, lead azide or styphnate) is classically detonated
by ame or a hot wire which then initiates a small quantity of a secondary high explosive also
inside the detonator (eg, PETN). This in turn initiates a booster typically containing tetryl or a
mixture of TNT and PETN. The high velocity shock wave of the booster then detonates the
main charge (eg, a blasting agent such as an ANFO mixture). A secondary explosive like
dynamite or an emulsion can be substituted for a commercial booster.
Typical commercial components of initiation systems are illustrated by Thurman (2011).
Figure 2 Diagram showing a three-step explosive train used to initiate an
explosive main charge (eg a blasting agent)
Detonators, Fuses and Boosters
[84.390] Low explosives, such as propellant powders and improvised chemical mixtures
conned in a pipe bomb, are normally initiated by ame from a fuse such as commercial
(safety) fuse which utilises a burning black powder core. Such fuse is used for blasting and
for model rockets (hobby fuse). Igniter cord is a less common form of fuse and consists of a
central wire covered in a pyrotechnic composition and contained in a plastic jacket. Burned
fuse usually can be recovered from post-blast debris.
Flame can also be produced by mixing certain chemicals whose reaction is so intense that
ames are produced (hypergolic mixtures). These mixtures can be used as silent delay
mechanisms whereby the mixing of the chemicals is delayed.
Flame can also be generated electrically by a squib. Another source of electrically generated
heat energy is a glowing lament (hot wire).
Detonator shells are made from metals such as aluminium, steel or copper. The shell fragments
can be recovered post-blast. Electrical detonators have rubber plugs through which wires pass.
They may also contain delay chemical mixtures. The wires are colour-coded according to the
properties of the detonator. These wires are referred to as lead or leg wires and are often
recovered post-blast. The wires are typically made from copper or tinned copper.
EXPLOSIVES [84.390]
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Test explosions to build databases and liaison with industry can greatly aid identication of
detonator components in post-blast debris. A commonly used primary explosive component is
lead azide (or less commonly, lead styphnate mixed with lead azide) which may leave a
characteristic lead residue on shell fragments (see [84.1900] R v Reyat (1993) 80 CCC (3d)
210; 25 CR (4th) 125n). However, if the detonator functions as designed, no chemical residue
from the high explosive content of the detonator is likely to be recovered.
A common form of detonator is the non-electric detonator which is factory assembled to
include a length of the initiating signal tube (trade names Exel and Nonel). The signal tube
(also known as shock tube) is comprised of a hollow plastic tube coated on the inside walls
with a mixture of the high explosive HMX and aluminium (Al) powder. The tube is often
colour-coded and may consist of a number of co-extruded layers. It can be initiated by a
detonator, detonating cord or high intensity electrical spark provided by proprietary initiating
devices. When initiated, the HMX/Al mixture generates a shock wave by a dust explosion
which propagates at approximately 2000 metres per second which in turn initiates a detonator
(Thurman, 2011). Signal tube will usually survive an explosion and can be recovered from
post-blast debris.
Electronic detonators contain an electronic delay circuit housed in the detonator shell in
contrast to the traditional pyrotechnic delay element used in non-electric and delay electric
detonators. Electronic detonators are tted with electrical lead wires. Chemicals in a wired
metal tube (such as aluminium) are heated by the application of electricity which causes them
to react and in turn initiate a primary high explosive (such as lead azide or styphnate). This
initiation detonates a charge inside the detonator (usually consisting of a secondary high
explosive like PETN) to create the shock wave required to initiate the main explosive charge.
A coded signal (essentially an electronic key) must be received by the electronic delay
circuit to function the detonator and in this respect electronic detonators offer a high degree of
security against illegal use.
Detonators are not usually sufficiently powerful to initiate blasting agents such as ANFO, for
this purpose boosters are used. Boosters may be specically designed for the purpose (for
example, cast boosters) or may simply be a cartridge of a commercial high explosive. Cast
boosters are commonly made from mixtures of TNT and PETN, or TNT and RDX or tetryl,
contained in short plastic or cardboard cylinders. Military explosives and initiating systems
operate in the same manner as commercial ones but may have different specications and
colour codings.
Illustrations and greater detail on these topics may be found in Thurman (2011).
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Chemistry of explosives
[84.400] An understanding of the chemistry of explosives assists in the reconstruction of
events. Detailed information on explosive compositions, chemistry, structural formulae, etc
may be found in many literature sources including: Urbanski (1964; 1965; 1967; 1984);
Urbanski and Vesudeva (1981); Yinon and Zitrin (1993); Russell (2000); Meyer et al (2002);
Manelis et al (2003); Crippen (2006); Agrawal and Hodgson (2007), US Picatinny Arsenal and
the US Army Armament Research and Development Command) (Vols 1 to 10); Akhavan
(2011); Thurman (2011) and Beveridge (2012).
Chemical classications
[84.410] When classied according to chemistry, explosive compounds and chemical
mixtures can be categorised as:
(1) inorganic nitrates containing the nitrate ion [NO
3
-
], for example ammonium nitrate
(NH
4
NO
3
);
(2) nitrate esters containing the structure C-O-NO
2
, for example ethylene glycol dinitrate
(EGDN), and nitroglycerine (NG) (principal ingredients of dynamites) and
pentaerythritol tetranitrate (PETN);
(3) nitramines containing the structure C-N-NO
2
, for example cyclotrimethylene
trinitramine (RDX) and tetryl;
(4) nitroaromatic compounds containing the structure C-NO
2
, where the carbon is part
of a benzene ring, for example 2,4,6 trinitrotoluene (TNT);
(5) nitroaliphatic compounds containing the structure C-NO
2
, where the carbon is not
part of a benzene ring, for example nitromethane;
(6) perchlorates and chlorates containing the ClO
4
-
and ClO
3
-
ions respectively, for
example potassium perchlorate (KClO
4
);
(7) other structures such as fulminate (-O-N=C-), azide (C-N=N=N) and peroxide
(C-O-O-); and
(8) fuels used in chemical mixtures with oxidising agents (eg, nitrates and chlorates). The
fuel may be a nely powdered metal (for example aluminium or magnesium);
sulphur; charcoal; sugar; ascorbic acid (vitamin D) or other organic compound such as
diesel fuel.
Oxygen balance
[84.420] Organic compounds are based on carbon, in which carbon is bonded to some or
all of the hydrogen, oxygen and nitrogen. The primary products of combustion are carbon
dioxide and water. A certain amount of oxygen is required in the formulation of an explosive
compound to convert the carbon and hydrogen (ie fuel elements) to carbon dioxide and water
respectively. The surplus or decit of oxygen in an explosives formula is expressed as a
percentage. The expression oxygen balance is used to describe the percentage of oxygen in
an explosives formula that is required to convert all of the carbon and hydrogen. The chemical
composition of the post-blast products will depend on the amount of oxygen present. A
perfectly balanced explosive compound has an oxygen balance of zero. For example, the two
explosive oils in dynamite, nitroglycerine (NG) and ethylene glycol dinitrate (EGDN), have a
EXPLOSIVES [84.420]
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positive oxygen balance, whereas the primary explosive chemicals in military explosives
(including 2,4,6 trinitrotoluene (TNT), pentaerythritol tetranitrate (PETN) and
cyclotrimethylene trinitramine (RDX)) have a negative oxygen balance. If not enough oxygen
is available (ie negative oxygen balance), then items recovered post-blast may exhibit
signicantly more carbon deposits arising from the unconverted carbon.
Chemical reactions
[84.430] In organic explosive compounds (such as NG, PETN, RDX and TNT), the
chemical reaction which takes place is internal combustion between oxygen, carbon and
hydrogen in the same molecule (compound). The carbon and hydrogen are normally separated
from the oxygen by a buffer element such as nitrogen. It is essential for intramolecular
combustion that the carbon and oxygen in the molecule not be bonded to each other. Thus,
fulminates with the -O-N-C- structure are explosive whereas isocyanates with the -N-C-O-
structure are not (Urbanski and Vesudeva, 1981).
Examples of reactions are (Mohanty, 2012):
Nitroglycerine (NG, nitrate ester) positive oxygen balance
C
3
H
5
(ONO
2
)
3
3CO
2
+ 2.5H
2
0 + 1.5N
2
+ 0.25O
2
Trinitrotoluene (TNT, aromatic nitrate) negative oxygen balance
2(C
7
H
5
(NO
3
)
2
7CO
2
+ 5H
2
O + 3N
2
+ 7C
In explosives mixtures containing inorganic compounds, the reactive oxygen (oxidiser) is
usually in one compound and the fuel (most frequently containing carbon and hydrogen) in
another. The efficiency of such explosives depends on whether the correct proportions of the
oxidiser and the fuel are utilised and how intimately these are mixed. Examples include black
powder and ammonium nitrate/fuel oil (Mohanty, 2012). Black powders efficiency is
somewhat impaired by two of the reaction products being solids (ie K
2
SO
4
and K
2
CO
3
) rather
than just gases.
Black powder
8C + 3S + 10KNO
3
3K
2
SO
4
+ 2K
2
CO
3
+ 6CO
2
ANFO
3NH
4
NO
3
+ CH
2
* CO
2
+ 3N
2
+ 7H
2
O
* generic fuel oil
(Mohanty, 2012).
Product formulations
[84.460] The principal chemical composition of a range of explosive products (under the
sub-headings: propellants, pyrotechnics, commercial, military and improvised explosives) are
discussed in this section. [84.390] refers to detonators, fuses and boosters that can be utilised
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+ 5N
2
for the initiation of the aforementioned products. Additional details on generic formulations are
listed by Yinon and Zitrin (1993); Akhavan (2011); Thurman (2011) and Hopler (2012).
Propellants (including black powder and smokeless powders)
[84.470] Black powder (a mixture of chemicals potassium nitrate, sulphur and carbon in
a ratio of 75:15:10) has been used for over 2000 years as a propellant, but has long been
superseded commercially by smokeless powders based on nitrocellulose (NC). Refer to
[84.1530] for details on black powder and their substitutes, including composition and
identication. [84.1540] provides details on techniques for the identication of components of
smokeless powders.
Smokeless powders are manufactured worldwide and are utilised as propellants for rie and
handgun ammunition. Smokeless powders are relatively easy to purchase in bulk due to their
legitimate use by sportsmen who reload shells for competitive target shooting and hunting.
Smokeless powders are nitrocellulose based and divided into three classes by the chemical
composition of their primary energetic ingredient(s):
single base powder (NC) (widely used in rie ammunition);
double base powder (NC and NG) (widely used in handgun and shotgun ammunition);
and
triple base powder (NC, NG and nitroguanidine [HN = C(NH
2
) NH(NO
2
)]) ([US]
National Research Council, Committee on Smokeless and Black Powder, 1998).
Triple base powders are used in large calibre munitions and are rarely if ever
encountered in IEDs.
In addition to the energetic components, additives are incorporated to control the burn rate and
ash characteristics. The additives are incorporated at different stages of the manufacture
depending on the type of powder and the manufacturing process. Additives include (Joshi et al,
2011):
Stabilisers which inhibit decomposition of nitrocellulose and increase the shelf life
(most commonly diphenylamine (DPA) and methyl and ethyl centralite (N,N
dimethyl diphenyl urea and NN-diethyl diphenyl urea respectively)). West et al
(2007) and Laza et al (2007) provide literature reviews and reaction mechanisms for
several stabilisers.
Plasticisers which assist in making the NC pliable and improve the gelatinising
properties and hygroscopic properties. Ethyl centralite, phthalates (such as dibutyl
phthalate) and 2,4-DNT are commonly used plasticisers (Joshi et al, 2011).
Additives are incorporated into the powder depending on the required combustion rate
and formulation. Additives include: ash suppressants (reduce muzzle ash),
deterrents and opaciers (usually added as a surface coating, modulate burn rate of
the individual grain and enhance the burn reproducibility and efficiency) and dyes
(assist in visual identication) (Perre et al, 2012).The surface coating may include: 2,4
dinitrotoluene (2,4 DNT), carbon, or potassium sulphate.
Pyrotechnics
[84.480] Pyrotechnic compositions are specically designed to produce a lot of energy
which is used to produce:
a ame or glow (ie a matchstick), or
EXPLOSIVES [84.480]
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smoke and light if combined with other volatile substances (ie reworks), or
large quantities of gas (eg, rework rockets and bangers) (Akhavan, 2011).
Pyrotechnic materials contain a fuel and an oxidiser, together with required additives to
achieve the desired outcome (ie generation of heat, delay, smoke, light and/or noise). Akhavan
(2011) describes the different applications and pyrotechnic compositions. Conkling and
Mocella (2011) present a comprehensive reference on the chemistry of pyrotechnics.
Flash powders
Flash powders are dangerous low explosive mixtures of chlorate oxidiser and aluminium or
magnesium powder. They have military applications as explosive simulators and like any
chemical mixture may be used as a pipe bomb ller. Loud bangs and brilliant ashes in
pyrotechnic displays usually are produced by ash powders. Klaptke et al (2013) discuss ash
compositions, specically the sensitivity and explosive power of binary ash compositions
containing aluminium and (per)chlorate oxidisers.
Other pyrotechnics
Black powder provides the lift for aerial pyrotechnic displays and when conned will
explode. Its properties have been discussed at [84.470].
Russell (2000) provides an overview of different pyrotechnic products and their chemistry,
including black powder.
Paragraph [84.1550] discusses the analysis and identication of pyrotechnic mixtures.
Commercial explosives (including blasting agents, slurries and
emulsions)
[84.500] Commercial explosives are relatively safe to use and relatively simple and
inexpensive to manufacture. Commercial manufacturers around the world review, modify and
develop new explosive formulations on an on-going basis to ensure that that the most
cost-effective and safe products are deployed for industry use. Akhavan (2011) and Hopler
(2012) provide an overview of the composition of commercial ammonium nitrate (AN)
products, including slurry and emulsion mixtures. Paragraph [84.1560] discusses the analysis
and identication of commercial explosives. This section provides an overview of a range of
commercial explosives, including those categorised as blasting agents, slurries and emulsions.
[84.510] Dynamite
Dynamite was developed in the 18601870s and formulations have changed little. The name is
derived from the Greek word dynamis meaning power. Dynamites have a long history, but
their production is falling in the face of rising production of AN based emulsions. The basic
components of dynamite are nitroglycerine, inorganic nitrates and carbonaceous fuels. What is
conventionally known as nitroglycerine in dynamite is actually two compounds: ethylene
glycol dinitrate (EGDN) and nitroglycerine (NG, glycerol trinitrate). The EGDN reduces the
risk of freezing (as NG freezes at approximately minus 13C). Due to its high volatility, EGDN
may be readily detected by instrumental explosive sniffers and dogs. Dynamites which contain
nitrocellulose are called gelatins. Most dynamites are gelatins, and also contain sodium
nitrate (SN) to enhance the oxygen balance. The ammonia dynamites contain ammonium
nitrate (AN). Typical fuels are wood pulp, coconut husks and gums. Some dynamites also
contain inert materials such as barium sulphate which can aid propagation of the explosion in
seismic applications. Dynamites are initiated by shock from a detonator.
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[84.520] Blasting agents
ANFO is a blasting agent developed in the 1950s and is made from ammonium nitrate and fuel
oil. Traditionally, bulk slurries and blasting agents are initiated by a booster, which is initiated
by a detonator. In later developments, cap-sensitive slurries were produced that could be
initiated with a detonator. These are packaged in plastic containers about the same size as
sticks of dynamite.
In 2011, 99% of the metric tonnage of industrial explosives sold for consumption in the United
States of America were ammonium nitrate based blasting agents and oxidisers. 71% was used
in coal mining (Apodaca 2013).
[84.530] Slurries
Slurry explosives (also referred to as water gels) consist of oil-in-water formulations
(Hopler, 2012). Slurries of ammonium nitrate and fuels such as diesel, were developed in the
1950s. Typical formulations also incorporate additives including chemical sensitisers (eg,
monomethyl ammonium nitrate (MMAN) or EGDN), or physical sensitisers (eg, air bubbles or
glass microspheres). Commercial use of slurries has declined in the face of competition from
the newer water-in-oil emulsion explosives ([84.540]).
[84.540] Emulsions
The newest development in commercial blasting explosives, which occurred in the 1960s and
1970s, is emulsion explosives. These are water-in-oil emulsions that consist of an internal
phase of a concentrated oxidising salt (typically a solution of ammonium nitrate and sodium
nitrate in water); an external phase of oils, waxes and surfactants; and glass microballoons or
gas bubble void sensitisers to help propagate the explosion (Hopler, 2012). Cap-sensitive
emulsions have made very signicant inroads into the dynamite market (ie products that can be
initiated utilising a detonator alone).
Military explosives (including plastic explosives)
[84.570] Military explosives are manufactured for use in artillery shells, missile warheads
and demolition charges. Military explosives are stable, ie resistant to impact, shock, and
moisture. They usually need to be capable of being stored for long periods of time without
signicant deterioration. All characteristics of military explosives must be completely
understood prior to use; including: power (amount of work conducted by the explosive
charge); sensitivity (relative ease to initiate/detonate); brisance (shattering effect);
hygroscopicity (absorption of moisture from the air) and toxicity. Military organisations around
the world review, modify and develop new explosives on an on-going basis to ensure that that
the most effective and safe products are deployed for use.
The most common military high explosives are trinitrotoluene (TNT), tetryl, pentaerythritol
tetranitrate (PETN), cyclotrimethylene trinitramine (RDX) and cyclotetramethylene
tetranitramine (HMX) (Hopler, 2012). RDX and HMX are British acronyms for Research
Department Explosive and High Melting Explosive respectively. TNT is used for
demolition and is a component, along with HMX, of the explosive octol. PETN is a
demolition explosive which is marketed in several forms including cord (detonating cord),
plasticised sheets and blocks. RDX is the primary component of the plastic explosive C4.
RDX and PETN are components of the plastic explosive Semtex. The United States of
Americas military also uses a product which although called military dynamite contains no
nitroglycerine. Rather it contains RDX, TNT, lubricating oil and starch. Composition B (an
RDX and TNT mix) is also commonly utilised by military organisations in their artillery
rounds and other munitions.
EXPLOSIVES [84.570]
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Plastic explosives are formulated with waxes and oils which make them mouldable. Thus they
can be packed to ll an irregular cavity, or can be moulded into a shape which will concentrate
the maximum force of the blast onto a specic area (shaped charges). Also, such explosives
can readily be disguised.
Polymer bonded explosives (PBX) were originally developed in order to reduce the sensitivity
of the explosive crystals (eg, RDX) by embedding the crystals in a rubber-like (inert) polymer
(Akhavan, 2011). Over the years, products were developed where the crystals were embedded
in energetic polymers in order to increase the explosive performance of the product. Akhavan
(2011) lists a range of available PBXs. The use of PBXs in military warheads is increasing
despite higher production costs compared to melt cast explosives.
Whilst melt cast explosives are commonly employed in low cost, mass-produced munitions
such as artillery and mortar rounds, PBXs are now used widely in high cost, low throughput
munitions where the relative cost of the warhead is small relative to the overall cost of the
missile or munition. (NB. The technique of casting is used for loading explosives into
containers. The process involves melting the composition (eg, TNT) and pouring it into a
container and allowing it to solidify (Akhavan, 2011)).
[84.1570] discusses the analysis and identication of military explosives.
Improvised explosives
[84.600] In stark contrast to commercial and military explosives, improvised explosives
generally have no legitimate uses and their characteristics tend to be unpredictable (ie with
regards sensitivity, power and stability). Terrorists, criminals and enthusiasts employ a range of
chemicals in making improvised explosives that can cause damage, destruction, fatalities,
injuries and general fear amongst the population. The reason for choosing a particular
explosive charge in any given device is generally governed by one or more of the following:
availability of chemicals;
cost;
level of expertise;
size of device and desired level of destruction;
target; and
familiarity and training.
Improvised explosive mixtures are produced by mixing a fuel (eg, aluminium, sulphur and/or
charcoal) with a strong oxidiser (eg, ammonium nitrate, sodium or potassium chlorate or
potassium perchlorate) or by synthesis of chemicals to form an explosive product such as
organic peroxides (Yeager, 2012).
Many precursor chemicals are quite readily available to the public as commercial products
(Crippen, 2006; National Research Council, Committee on Marketing, Rendering Inert, and
Licensing of Explosive Materials, 1998, 126-132, 147; Yeager, 2012). Peroxide explosives are
being used increasingly in terrorist attacks, including the London bombings of 2005 (Broome
and Todd, 2012). Their synthesis is relatively straightforward, requiring hydrogen peroxide as
a necessary ingredient. There are several peroxide explosives, but the most common are
triacetone triperoxide (TATP) which is synthesised from acetone and hydrogen peroxide, and
hexamethylenetriperoxide diamine (HMTD) which is synthesised from hydrogen peroxide and
hexamine. Recipes to make improvised explosives of this type are readily available on the
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internet. Due to the ready availability of recipes and starting materials, and the limited skill
required to make improvised explosives, they are of concern to the law enforcement
community.
Also of increasing concern are the hydrogen peroxide organic mixtures (sometimes referred to
as HPOM or concentrated hydrogen peroxide explosives (CHPX), which can be made by
mixing hydrogen peroxide with an organic material such as our or pepper. Such mixtures are
mentioned in trial transcripts of the attempted London bombings on 21 July 2005 and have
been discussed by Broome and Todd (2012) and Yeager (2012). These mixtures vary in
appearance and consistency. Once again, due to the availability of materials and the ease of
manufacture, these mixtures are of concern to law enforcement and other agencies around the
world. As new explosives continue to emerge, scientists undertake research to characterise and
evaluate the materials to inform procedures and methods.
Improvised explosives, whether they be oxidiser/fuel mixtures or discrete chemical compounds
such as TATP, are generally manufactured and employed by criminals, terrorists, or enthusiasts
(eg, for experimental or nuisance purposes). [84.1580] discusses the analysis and identication
of improvised explosive mixtures.
EXPLOSIVES [84.600]
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IMPROVISED EXPLOSIVE DEVICES
[84.700] Improvised explosive devices (IEDs), also commonly referred to as bombs
(Thurman, 2011 Ch 3; Vermette, 2012 s 4.3; Beveridge, 2013) consist of an explosive charge
with a means of initiation. Low explosives must be contained, and containers are often used
with high explosives to disguise or hide the device, and/or to produce shrapnel.
Components
[84.710] The primary components of an IED are:
initiation device;
explosives; and
container (required for low explosives).
Appropriate application of forensic science can advance investigations on several fronts, both
through the provision of evidence to inform a judicial process or intelligence to direct an
investigation or prevent the occurrence of future events. Each of the IED components is a
potential source of trace chemical, biological and physical evidence which can be related to
bomb makers to:
identify IED components and potential source;
determine the explosive used and potential source;
compare physical evidence from the crime scene to the suspect;
corroborate or dispute statements;
link or exclude explosive incidents; and
identify potential offenders.
Containers are necessary to initiate a low explosive charge including propellant powders and
chemical mixtures. Metal or plastic pipes are commonly used (pipe bombs). Containers for
high explosives are used for concealment and / or fragmentation and range from baggage
through to stereos (radios) to vehicles. Bulk explosives, typically improvised explosive
mixtures, are most frequently used in vehicles known as large vehicle bombs or
vehicle-borne explosives.
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Initiation
[84.730] IED initiation systems generally fall into three main categories: delay initiation,
victim initiation and command initiation.
Delay initiation
[84.740] A common mechanism utilised to create a time delay is a mechanical clock or
electronic timer. These, by a mechanical action or electrical impulse, complete an electrical
circuit from a battery to a detonator (or to another initiation source such as a hot wire) in
order to initiate an explosive.
A measured length of safety fuse also provides a reliable delay mechanism (for example,
commercial safety fuse burns at approximately 130 seconds per metre).
A chemical delay, such as a corrosive substance (eg, an acid) in a plastic or rubber container
(eg, plastic bag or condom) works on the principle that the acid will slowly dissolve the
container and then react with an appropriate chemical mixture inside the device to produce a
ame. The ame will in turn initiate a low explosive and some primary high explosives.
Victim initiation
[84.750] Action by the victim can be used to complete an electrical circuit; for example, a
trip wire, a mercury switch, a motion sensor, or pressure plates. These are commonly termed
booby trap initiation systems when initiated by the target of the explosion. The effect of
pressure change on a barometer or altimeter is another form of physical action which can
complete a circuit.
Command initiation
[84.760] The bomber can initiate a device by remote control action; for example, by using
a mobile telephone to provide the electrical impulse necessary to complete a circuit and initiate
a detonator.
Commercial blasting equipment would also fall into this category. Two systems in common use
are the traditional electrical detonator and a non-electrical shock tube system ([84.390]).
IMPROVISED EXPLOSIVE DEVICES [84.760]
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PRE-BLAST INVESTIGATION
[84.900] Whilst the focus of this chapter is on post-blast investigations, it is important to
note the role of forensic scientists in support of proactive investigations to prevent illegal use
of explosives.
During the course of an investigation, investigators may recover images, notes, manuals or
actual items such as chemicals or device components. These may also be referred to in phone
calls that have been intercepted by police. Investigators draw upon relevant scientic
disciplines to provide advice to assist in identifying whether potentially illegal activities are
underway (ie in planning).
Investigators may request a forensic chemist to provide an opinion as to:
whether a list of chemicals could be utilised to manufacture explosives?
whether a recipe is viable, ie if followed, would it result in the production of
explosives?
what would be the purity and yield of any products?
what specialist equipment would be required to manufacture these explosives?
are any chemicals missing from the list?
what are the legitimate uses of these chemicals?
Similar questions are asked of post-blast scene examiners and bomb technicians in the event of
the recovery of suspected device components.
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POST-BLAST INVESTIGATION
[84.950] The scene of a large explosion initially is one of chaos. Pre-planning is essential.
Strobel (2012, s 5.2.1) articulates the situation well:
Once the event has occurred, the investigating agency which has done no planning can do
little more than play catch up as the investigation unfolds. Preplanning on the part of
investigative agencies largely dictates whether the investigation runs the investigators or
vice-versa.
Command and control
[84.960] Good communication, command and control within and between the investigation
and forensic teams are vital to the success of a post-blast investigation. A command centre is
established to coordinate communication and activities of those involved in the investigation
and to ensure logistical support. Internal information ow must be clearly established through
team briengs and interaction with all involved groups. Media protocols must be clearly
established and followed normally through one spokesperson.
Jurisdiction should be established immediately one person should assume immediate control
of the scene and the investigation (such as a senior investigating officer). This is particularly
critical when more than one agency is involved or in a multi-jurisdictional investigation, for
example, in a suspected aircraft bombing, or when a bomb manufactured in one country blows
up in another ([84.1900] R v Reyat (1993) 80 CCC (3d) 210; 25 CR (4th) 125n), or when
international assistance is provided ([84.2080] on the Bali Bombings).
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Police criminal investigation
[84.970] The head of the investigation (eg, the senior investigating officer) requires good
investigative expertise rather than expertise in bombs and explosives for which he or she
must rely on a team of specialists. Ideally, there will be a pre-planned strategy in place, for
example, calling upon the assistance of trained response teams comprising post-blast experts
and other scientic experts as required by the circumstances. The success of such
investigations relies on the early engagement of the most appropriate specialists. The roles of
some of these specialists are described in this section.
The purpose of a police investigation is generally to identify, charge and prosecute an
offender/s who had the means, motivation and opportunity to commit the crime. The police
investigation seeks answers to the following essential questions (Vermette, 2012 s. 4.2.) and
utilises the team of specialists to assist in providing them. The extent to which these questions
are investigated and answered will usually depend on the scale and prole of the incident. In
major incidents, such questions might only be answerable by large multi-agency, multi-
disciplinary task forces. In minor incidents, one or two police officers assisted by a bomb
technician or a post-blast expert may suffice.
what
materials were used to construct the device?
skill or expertise did the bomber need?
object was damaged by the device?
object was the intended target of the device?
who
was the actual victim?
was the intended victim?
made the device?
placed the device?
had the opportunity?
had the means?
provided the funds?
provided the training?
assisted?
why
was the specic device used?
was the device placed where it was?
was the device constructed as it was?
was the intended target selected?
when
was the device made?
POST-BLAST INVESTIGATION [84.970]
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was the device placed?
was the device initiated?
did the device explode?
where
were the device components/explosives obtained?
how
was the device initiated?
were
all explosives/devices recovered as a result of the investigation?
future intended targets/plans identied as a result of the investigation?
The investigative/police team assists with securing the scene, identifying and interviewing
witnesses, assessing the neighbourhood, doing background checks on the victim/target and
pursuing leads on suspects; that is, conduct a normal police investigation.
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Forensic investigation
[84.980] Many specialist scientic disciplines may contribute to the forensic investigation.
The roles of a number of core disciplines are summarised in the following sections. Examples
of references on this topic include: Vermette (2012, Ch 4) who has described the essentials;
Thurman (2011) who has written a comprehensive book on scene examination; Garstang
(2012, Ch 7) and Baker et al (2012, Ch 8) who have described the expertise brought to bear on
the scene of an air disaster; Foster (2012, Ch 9) who has described the expertise employed at
the scene of a gas explosion in a building and Strobel (2012, Ch 5) who has described the role
of a forensic chemist at a scene.
Field Examinations
Post-blast scene examination teams
[84.990] The composition of a post-blast scene examination team will vary depending on
the scale of the incident, available resources and jurisdiction. In addition to the team leader (or
coordinator), team members will include post-blast scene examiners and other scientic and
technical specialists as required. Scientic and technical specialists may include: forensic
chemists; ngerprint experts; forensic pathologists; forensic anthropologists; metallurgists;
engineers; bomb technicians and/or radio technicians; personnel specialising in surveying,
mapping and photography; and handlers of dogs trained to detect explosives. In smaller
jurisdictions, one person may cover more than one of the specialist areas. If the scene is large,
members from police or military teams may be requested to assist with searching. In large
incidents, logistic and exhibit management support will also be a consideration.
A detailed overview of the various specialists that may be engaged during an investigation is
provided at [84.1210] [84.1300]. The roles of the post-blast scene examiner and forensic
chemist in the eld are outlined in the next section.
Post-blast scene examiner
[84.1000] A post-blast scene examiner performs or oversees the performance of the
following roles:
interpret blast damage;
record the scene;
search the scene for fragments originating from the device;
collect fragments and residue samples;
identify the suspected seat of the blast and type of explosion;
identify the suspected type and amount of explosive;
identify suspected components of a device;
reconstruct the device; and
provide expert evidence in relation to the aforementioned tasks.
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Forensic chemist
[84.1010] At a post-blast scene, a forensic chemist can advise and/or assist with:
scene examination;
explosive residue collection, packaging and storage;
the properties and uses of recovered chemicals;
on-site preliminary analysis of residues or recovered chemicals utilising portable
instruments;
ensuring that appropriate samples are submitted to the laboratory for priority analysis;
and
collection of other items of potential signicance, eg, metal fragments, fabric, bres,
paint and plastics
As mentioned, one of the valuable roles that a chemist can play at a scene is the on-site
analysis of items/samples utilising eld portable instruments for screening for residues or
identifying recovered chemicals. An additional resource for consideration that falls under this
category is the use of explosive detection canines. These are handled by specialist handlers and
not the forensic chemist.
Portable explosive detection instruments offer a number of advantages in the investigation of
explosive-related incidents. Such instruments enable analyses to be conducted close to a
post-blast scene and result in the provision of real-time results to investigators and scene
examiners. The use of portable instruments at or near the scene can also increase the efficiency
of analyses back at the main laboratory through initial sample screening and prioritisation. In
post-blast examinations, portable instrumentation can signicantly decrease the time in which
preliminary results are available, particularly if there is signicant transportation of exhibits
required. For example, the Australian Federal Police (AFP) have used portable instrumentation
to provide preliminary results for investigations in Indonesia and the Philippines, where
transportation of exhibits to the central laboratory in Australia involved over eight hours of
ying time. The preliminary results can guide investigations and inform decision making. It is
important to realise that the information generated on-site is primarily for intelligence
purposes to help direct the police investigation or decision making at the scene. This does not
replace the need to conduct laboratory based conrmatory analyses to inform the judicial
process. ([84.2250] highlights this issue utilising the Bali bombings 2002 case study).
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Protocols at the scene of an explosion
[84.1050] Scenes relating to post-blast investigations are generally referred to as primary
scenes (where the explosion occurred) and secondary scenes (scenes that are associated with
the primary scene, eg, a mortuary, where the deceased from the blast are being examined; a
hospital where the victims are being treated, premises where devices were constructed and/or
explosives made, open areas where experiments/trials were conducted or vehicle/s used for
transport). This section focuses on the examination of primary scenes; however, a brief
overview is provided on considerations for processing secondary scenes ([84.1170] refers).
One essential aspect of attending explosive related scenes is that persons and items entering a
primary or secondary scene (or an analytical facility) must be demonstrably free of
explosives (Murray, 2012 Ch 18). If contamination with explosives occurs or the possibility
of contamination occurs at any stage of an investigation (be it scene, seizure, packaging,
transportation, storage or analysis) then evidence of explosive traces may hold little or no
weight in a court of law. Demonstrably free of explosives is a practical application of quality
assurance: demonstrably means tested, found to be negative and documented. Portable
analytical equipment and explosive detection dogs are useful for this purpose. It applies to
personnel, their clothing and footwear, their equipment, and their transportation, etc.
Contamination has caused many real problems in investigations and can be the starting point
for independent experts and counsel.
Paragraphs [84.1770] [84.1810] discuss procedures for contamination prevention and the
different types of control samples that can be collected to assist in demonstrating that surfaces
are free of explosives prior to scene entry and/or examination of items. The following sections
deal with this issue explicitly and implicitly and it is an essential aspect of training in this eld.
Primary scenes
[84.1060] There are general protocols that are considered when conducting a post-blast
scene examination. These protocols are outlined by forensic laboratories in their standard
procedures and also in numerous texts such as US Department of Justice (2000); NFPA 921
(2011); (Thurman) 2011 and Beveridge (2012). The examination plan will be dictated by the
individual circumstances of the incident. The key response and examination phases are covered
at [84.1070] [84.1130].
Emergency response and search and rescue
[84.1070] The rst phase of any response to an explosion involves the search and rescue
of the injured. The primary role of rst responders in this instance is humanitarian and scene
protection. Their training should emphasise minimal re suppression, no non-essential
personnel on-site and a marked corridor for emergency personnel. Post-blast scene examiners
can brief emergency personnel on key points of scene preservation; however, the rescue of
surviving victims takes priority. The recovery of the deceased is also a priority with respect to
the identication and reconciliation phases of the DVI process. The DVI process should be
conducted in coordination with the post-blast scene examination process.
In a major incident, once the injured have been removed and jurisdiction has been established,
there should be an initial brieng to establish the facts, including safety hazards and reports
from rst responders. The plan is then implemented and work assignments are set. The
post-blast scene examiner should consider the impact of this initial phase on the scene,
particularly with respect to the potential destruction or relocation of items of interest.
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Contamination prevention procedures
[84.1080] See [84.1050] and [84.1770] [84.1810].
Site safety and clearance
[84.1090] The scene should generally be declared safe by a bomb technician or other
appropriate personnel before others enter. This is known as the primary sweep. The purpose
of this is to ensure that there are no additional explosive devices, including booby traps, and to
render safe any that are located. Structural integrity must also be assessed by qualied
personnel such as structural engineers. Utilities personnel should attend as required to assess
gas and electricity safety issues. It is essential to consider and address chemical and biological
hazards, including toxic, corrosive, ammable or explosive vapours and body uids.
Scene appreciation phase
[84.1100] The rst phase of the scene examination typically involves the classication of
the post-blast scene as to whether the nature of the explosion is obvious or not (eg, an
explosion at a power station, a work place incident or a terrorist attack). Issues identied are
combined with information from the rst responders and witnesses in order to formulate the
most efficient and effective course of action. Required resources to achieve the planned
objectives are also considered during the appreciation phase. Potential physical evidence
observed at this stage is noted and protected.
Scene assessment phase
[84.1110] The scene must be secured as soon as possible by establishing boundaries and
ensuring that all non-essential personnel are kept out. The command centre can be kept fully
informed of developments inside the boundaries via regular briengs and possibly through the
use of specialised video technology. All authorised personnel (ie assisting with the examination
of the scene) entering the scene should be logged in and out. In order to ensure security and
preservation of the scene, the size of the scene must be determined. In order to do this, the
furthest most spread of debris is located and a 50 per cent buffer zone is generally added to
determine the placement of the outer cordon. Depending on the incident, the 50 per cent buffer
region can be searched and cleared of evidence as a priority so that the cordon can be
decreased. This is particularly important if the scene is located in a central business district as
it allows the impact on business closures and the movement of people to be minimised.
Scene examination phase
[84.1120] Typical post-blast evidence from IEDs consists of remnants of timers, power
sources, containers, tapes and wires; however, physical evidence can take many forms.
Materials damaged by the explosion are considered for collection and may include metal and
plastic fragments, clothing, adhesive tape, cardboard, wrapping paper, timer parts, battery
parts, wires, electronic parts, parts of radios and stereos, other potential containers, scorched
material, and shattered, deposited or penetrated material. Objects such as suitcases, other
baggage, and furniture are also prime sources of embedded fragments. Traces of explosive
residues and other forensic evidence are also collected for analysis and identication.
Record, Search and Collect
This aspect of scene examination includes the recording of the overall scene and then the
searching, recording and collection of primary fragmentation according to a pre-determined
search pattern. Search patterns typically are spiral, grid, strip or zone depending on the
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circumstances, including the size of the scene and available resources. Entry and exit points to
the seat of the blast are established and cleared of any debris. Remaining debris of interest
from the search areas is recorded and collected. The search areas can nally be swept, with the
sweepings collected.
All items/samples collected should be documented, packaged and stored in order to maintain
the integrity of the items. Paragraph [84.1080] addresses quality control measures for
consideration when processing a scene. In general, processes should be adopted in order to
minimise the potential for contamination, this includes:
Items/equipment taken on site should be demonstrably free of explosives.
Physical evidence/debris should be collected using clean, unused implements and
containers. Containers should be clean, air-tight and impermeable to vapours of
explosives and petroleum products. Proven examples are clean, unused paint cans,
mason jars and heat-sealed nylon bags.
The collection of material suspected of bearing explosive traces should not be
undertaken by anyone who recently has handled, or who habitually handles
explosives, including explosives ordnance disposal (EOD) or bomb squad officers. If
circumstances necessitate that such officers must collect exhibits, then the requirement
for them being demonstrably free of explosives by virtue of documented
precautions and screening is essential to minimise court challenges (refer to
[84.1080]).
Consideration to the preservation of other trace evidence types, including identication
material such as ngerprints and DNA on IED fragments.
Samples of soil and/or other sweepings can also be collected. This debris may be sifted on-site
using various sizes of screens or removed to a forensic laboratory for searching. When samples
of soil or like material are collected for residue examination, a control sample of the same
material should be taken from an area remote from likely explosive residue deposition. The
same applies to surfaces that are swabbed for trace explosive residues.
Fragments travelling at high velocity may penetrate animate and inanimate objects. Human and
animal victims, alive or dead, are sources of physical evidence which should be recovered at
hospital during treatment or on pathological examination (see [84.1170]).
Field portable instruments and explosive detection dogs
As discussed in [84.1010] (also [84.2630]) the scene examination phase can be assisted by the
use of portable explosive detection instruments and dogs trained to detect explosive residues
(Furton and Myers, 2001; Woods et al, 2004; Hallowell et al, 2012).
Damage assessment
Damage assessment includes observing and interpreting the shattering and/or pushing effects
of positive and negative blast pressure waves, impacts from primary and secondary
fragmentation and effects of heat and re (Strobel, 2012, Ch 5). The post-blast scene examiner
will interpret the damage to inform an opinion on the type of explosion ie mechanical or
chemical. If chemical, the probable type of chemical eg, vapourair; dustair or explosive
compound/mixture may be assessed. The examiner will also try to determine: the use of a
high or low explosive; approximate size of the main charge; type of container; where the
device was placed etc. If an explosive was involved, the nature of the damage close to the site
of the explosion plus any evidence of container fragmentation can permit a reasonable estimate
of whether a low or high explosive was involved. It is important to establish as soon as
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possible what objects were present before the blast and where they were located. This may
permit estimation of the quantity of explosive, location/placement of the device and assist
recognition of foreign material such as device fragments. Sorensen and McGill (2011) present
a review of blast scene damage observables, specically structural damage to commonly used
building materials, to inform opinions on size, type and position of the charge. Keane and
Esper (2009) also provide a discussion on the forensic investigation of blast damage to a
number of buildings in Britain.
Explosive residue collection
The examination phase includes the search and collection of unconsumed explosive materials
and residues. This phase also involves the collection of suitable environmental controls and
reference samples (refer to [84.1780] [84.1810]). Residues may be recovered by swabbing
objects which are suspected of bearing residues but cannot feasibly be removed, for example,
a blackened wall or pillar, or skin. Alternatively, and preferably, items are collected for
examination in the main laboratory.
Samples and swabs for explosive residue analysis are generally collected from close to the seat
of explosion. Samples/swabs can also be collected from surfaces that are facing the seat of
explosion where residues may have been deposited. If there has been a re, re ghting efforts
and/or a search and rescue operation, these may have affected the survival of residues. In these
instances, surfaces that are further away and/or above ground level are often a good source of
residues (refer to [84.2080] on the Bali Bombings case study).
If swabs are collected in the eld, they are collected utilising dry swabs or swabs wetted with
organic solvent, inorganic solvent or a mixture of solvents. Depending on the situation and the
surfaces, vacuuming may also be an alternative (eg, victims clothing or oors of secondary
premises). Further details in relation to residue collection procedures are provided in
[84.1390]. Commercial Explosive Residue Swab Kits are also advertised for sale by private
organisations. Explosive residue traces may also be sought through sampling of the air at the
seat of the explosion by drawing the air through an adsorbent material using a portable pump:
Wardleworth and Ancient (1983); Deak et al (1989). This is an effective method for recovering
residues of volatile explosives (eg, EGDN and NG from dynamite).
Kunz et al (2012) present a useful body of work addressing the chemical and physical fates of
trace amounts of explosives exposed to different environmental conditions. This information
can be used to inform explosive residue sampling and analysis plans and also the interpretation
of results. Abdul-Karim et al (2013) report on research to inform decisions on where residue
samples are best sought at post blast scenes based on the spatial distribution of RDX residues.
Analytical phase
[84.1130] This phase includes the reconstruction of the device and analysis of explosive
residues, identication materials (eg, ngerprints and DNA) and other physical, trace and
electronic evidence that may assist in answering the key investigation questions as outlined in
[84.970]. Paragraphs [84.1200] [84.1450] provide an overview of the common key aspects of
the analytical phase, including types of evidence, discipline capabilities and protocols for the
analysis of explosive residues.
Secondary scenes
[84.1170] Secondary scenes are often a source of key information and in some cases the
missing link in reconstructing the device and overall sequence of events. Secondary scenes can
include:
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(a) Morgues and hospitals
Residual evidence of the device and chemical residues may be recovered from the deceased
and/or injured at morgues and hospitals. The post-blast scene examiner should work closely
with the forensic pathologist or other medical practitioner to ensure that potential evidence is
recovered and that relevant questions are answered. Paragraph [84.1220] provides more details
in relation to the role of the forensic pathologist.
(b) Premises, vehicles, open areas
Locations where a device may have been stored, constructed or explosives manufactured can
be prime sources of evidence. These could also include premises, vehicles, boats etc that may
have been involved in the incident at some stage. Houses/premises where it is believed the
offenders may have constructed (or stored) a device should be examined for evidence of the
device, including explosive residues, and also evidence placing the offenders in these premises.
Likewise, vehicles that may have been used to transport the devices, explosives or persons
should also be examined. Locations (such as open areas) where persons of interest may have
undertaken trials with devices or explosives or hidden materials should also be examined. It is
vital that consideration be given to eliminating any potential cross-contamination of the
secondary scene from the primary scene. Steps that can be taken include personnel examining
the primary scene and equipment utilised in the primary scene, should not enter the secondary
scene. If this cannot be avoided, then appropriate precautions should be taken, including
personnel showering and donning new protective clothing and cleaning and testing previously
utilised equipment prior to entering the secondary scene.
Control swabs should also be taken from the equipment and personnel prior to entering the
scene. These precautions are taken to ensure that any evidence located and identied at the
secondary scene is the result of a true connection with the primary scene and not a result of
cross-contamination. Quality control measures are further discussed in [84.1770] [84.1820].
When processing secondary scenes, consideration should be given to investigative priorities.
An examination plan should be developed by the senior forensic examiner (eg, forensic
coordinator) in conjunction with the senior investigating officer prior to entry in order to meet
investigative priorities and ensure there are no missed opportunities.
A secondary scene may also be a clandestine laboratory where the explosives were or are being
manufactured/synthesised. These scenes are potentially hazardous and should be processed in
consultation with a forensic chemist or other appropriate hazardous materials response
personnel. Typical seizures may include: chemicals; improvised explosives; scientic
equipment; personal protective equipment, IED components; literature and experimental notes,
including recipes. Speers et al (2013) provide an excellent overview of procedures for the safe
and effective examination of clandestine explosive laboratories.
(c) Persons of interest
Samples for trace analysis and reference samples for identication purposes should be
collected from persons of interest. Procedures will be guided by the jurisdictional legislation
under which the person has been charged. A number of options exist for when a person can be
sampled for explosive residues and their clothing collected, however the key points are to
prevent the person from destroying potential evidence and ensure that the person cannot come
into contact with surfaces/persons potentially contaminated with explosives.
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Laboratory examination
Forensic disciplines
[84.1210] Once the eld examination has commenced and items have been recovered/
samples collected, the laboratory examination of these items/samples commences in order to
assist in answering the questions outlined in [84.970]. When exhibits from an explosive related
scene are received at a laboratory, the responsibility for contamination prevention (quality
assurance) transfers to the laboratory. Exhibits should be stored in a secure area and in a
manner that prevents the potential for contamination. Where possible, exhibits for trace
explosive residue analysis should be refrigerated prior to examination. This is due to the fact
that some explosive compounds are volatile and will volatilise or sublime over time (ie
transform into a gas/vapour).
A wide range of scientic and technical specialists can be involved in a post-blast
investigation, particularly when it comes to examining the recovered evidence. Whilst the
objective of the examination is determined in consultation with the criminal investigators, two
of the primary forensic objectives are: (1) to determine what the IED consisted of and (2) to
link the components to the bomb maker/s. The expertise required depends on the
circumstances and the nature of the evidence. It is important to emphasise the importance of a
team approach, with on-going communication between team members in the laboratory and the
eld.
It is important to discuss potential areas of an item or surface to be swabbed for explosive
residues, DNA, ngerprints and other potential trace evidence with the various scientic
specialists prior to examining items. This maximises the recovery of all potentially signicant
evidence. A general sequence of examinations by the various disciplines may include:
1. Visual examination (including naked eye and microscopy) to recover intact (or
partially consumed) explosive particles and fragments of interest. This is followed by
the collection of swabs/solvent washes on designated areas of the item for subsequent
explosive residue analysis (usually conducted by the chemist or crime scene officer
following consultation with relevant specialists).
2. Latent ngerprint processing by the ngerprint specialists. Depending on the surface,
a search may be conducted using oblique lighting prior to swabs being collected in
step 1 to assist in identifying suitable areas for explosive residue swabbing and
ngerprint recovery.
3. Swabbing for trace DNA by a biologist (or other suitably qualied member).
4. Device reconstruction with post-blast scene examiners, bomb technicians, and other
personnel with relevant expertise.
The aforementioned order of examinations may vary depending on the circumstances of the
incident under investigation.
Due to the extreme pressures and temperatures that surfaces in contact with and in close
proximity to a device are exposed to during an explosion (in addition to the re ghting and
rescue efforts), the identication and recovery of traditional forensic evidence, including
ngerprints and DNA, becomes more challenging. This section provides an overview of
examinations that can be conducted by the various scientic disciplines.
Identication materials
[84.1230] Identication materials, such as DNA, ngerprints and hair, are all potential
types of evidence that should be considered during a post-blast investigation. Examination of
these may assist in:
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identifying the person who constructed the IED; and
identifying those associated with the device and/or the components prior to the blast.
The examination of these evidence types are addressed in chapters throughout this series
(including Chapters 80 (DNA), 88 (bres and hair), 96 (ngerprints)), however the
examination of these materials in a post-blast context will be addressed in this section.
[84.1240] Fingerprints
Fingerprint experts often perform a vital role in post-blast scene examinations, whether
deployed to the eld or conducting examinations in the laboratory. Suitable surfaces are
selected and techniques are applied that would not necessarily be routinely utilised.
Notwithstanding the destructive impact of the explosion on identication material, ngerprints
can sometimes be identied on IED fragments. The most probable sources of ngerprints are
containers eg, bags, boxes, pipe fragments and adhesive tapes.
In Chapter 96 of this work, at paragraph [96.700], Comber et al, (2006) describe procedures to
recover and detect ngermarks on adhesive tape. Cited references include Bratton et al (1996)
which discusses a black powder method to process adhesive tapes and Scheimer et al (2005)
which discusses latent ngerprints on black electrical tape.
Boyle et al (2004) report on the use of cyanoacrylate (super glue) fuming to recover
ngerprints from metal and plastic pipe bomb fragments. The authors determined that the
process did not signicantly interfere with explosive residue recovery and analysis. The
fuming was conducted on-scene and latent print development was undertaken in the laboratory.
Jasuja et al (2007) studied the development of latent ngerprints on the adhesive side of tapes
using phase transfer catalyst and Rose Bengal dye.
The recovery of trace DNA and also explosive residues from areas where ngerprints are
observed is a consideration for forensic scientists in order to maximise the recovery of all
potential evidence. Whilst this recovery will generally only be attempted in the event of a poor
quality print (ie not suitable for identication purposes) and in the absence of other DNA or
trace explosive evidence, it is a decision that should be made following consultation with
relevant discipline experts. Research has been conducted into the development of techniques to
detect latent ngerprints and subsequently analyse the chemical compounds deposited within,
specically explosives. King (2012) reports on the recovery and identication of explosive
resides deposited in latent ngermarks following the application of different ngermark
detection methods. The research demonstrates that each ngermark detection method applied
in sequence is likely to reduce the amount of residue remaining. Emmons et al (2009) discuss
the use of Raman chemical imaging to detect and identify explosives in contaminated
ngerprints. Hazarika and Russell (2012) provide an overview of advances in ngerprinting
technology including in relation to identifying chemicals handled by a person and the identity
of that person. Verkouteren et al (2010) describe a method based on polarised light microscopy
and image analysis for automated mapping of RDX particles in ngerprints deposited using the
explosive C-4. Rowell et al (2012) describe the detection of nitro-organic and peroxide
explosives in latent ngermarks by direct analysis in real time-mass spectrometry (DART-MS)
and surface-assisted laser desorption/ionization-time of ight-mass spectrometry (SALDI-
TOF-MS). Banas et al (2012) report on the detection of microscopic particles in latent
ngerprints utilising synchrotron radiation-based Fourier transform infra-red micro-imaging.
Abdelhamid et al (2011) discuss the analysis of explosive residues in ngerprints using optical
catapulting-laser-induced breakdown spectroscopy (OC-LIBS). Verkouteren (2007) address the
recovery of explosive particles (namely RDX and PETN) in ngerprint residues. Phares et al
(2000) and Dorozhkin et al (2005) discuss the transfer of explosive residues through
ngerprints.
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[84.1250] DNA
Fragments recovered from IEDs should be tested for DNA in the same manner as other objects
suspected of bearing DNA. The heat generated by the explosion does not necessarily negate
the potential for positive results. This was demonstrated by Esslinger et al (2004) who reported
the recovery of DNA proles from subjects who had handled metal and plastic pipe bombs.
Post-blast fragments of the pipes were swabbed and analysed for DNA. Of the twenty pipe
bombs, four gave reportable results matching subjects DNA proles, and another eight also
matched but were below reportable levels. Zamir et al (2000) discuss the extraction and
analysis of DNA from adhesive tapes following processing for ngerprints.
Ramasamy et al (2011) report on the successful recovery of DNA and ngerprints from the
exterior and interior of a vehicle following the use of a render safe tool. The authors also report
on the successful recovery of DNA and ngerprints from glass and plastic surfaces of items
placed inside the vehicle at the time of the render safe procedure.
Hoffmann et al (2012) report on a study aimed at identifying persons who had handled an IED
through the post blast recovery of DNA from IED containers, in this case - backpacks. The
research was successful in recovering DNA from back packs containing smokeless powder
lled pipe bombs (galvanised steel and PVC) following deagration.
Bille et al (2009) evaluated the effects of cyanoacrylate fuming, time after recovery and
location of biological material on the recovery of DNA from pipe bombs containing black
powder substitutes. In summary, only a fraction of the initial DNA deposited was recovered
from post-blast pipe fragments. A signicant decrease in the amount of DNA recovered was
observed as time passed since the deagration (in this case from 1 week to 3 months).
Cyanoacrylate fuming did not have a signicant effect on the successful recovery and analysis
of DNA and greater quantities of DNA were recovered from the pipe nipples compared to the
end caps. The paper also includes a discussion on factors that may affect the success of DNA
typing.
These results emphasise the importance of careful handling of post-blast fragments to avoid
loss of such evidence. DNA analysis, and the ngerprint examination noted in the preceding
sub-paragraph underline the need for a considered and results-based protocol for the
examination of evidence by ngerprint experts, biologists and chemists to ensure that the work
of one discipline does not destroy what is potential evidence for another.
[84.1260] Hair
Hair attached to debris recovered during a post-blast scene examination can be a useful source
of evidence towards identifying people associated with the device pre-blast. Adhesive tapes are
commonly utilised in the construction of a device and are a prime source of hairs for
comparison to hair from a suspected bomb maker and also DNA if the roots of the hair are
present.
Hair can also be a source of trace explosive residues, particularly in the case of a bomb-maker
and/or suicide bomber (Efremenko et al, 2007; Oxley et al, 2007; Oxley et al, 2008; Bell et al,
2009; Oxley et al, 2009; Oxley et al, 2012).
Hair examination is discussed in Chapter 88 of this series.
Physical and trace evidence
[84.1270] Like any forensic investigation, all potential types of physical and trace
evidence should be considered during a post-blast investigation. Physical and trace evidence
commonly associated with post-blast examinations include:
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explosive residues, including control and reference samples;
metal, plastic, paper/cardboard or rubber (potentially used as a container);
adhesive tapes, glue;
monolament line, string;
bres, textiles;
surface coatings such as paint; and
electrical components timer, batteries, electronic parts, wire, connectors, switches,
detonator wires and fragments, fuse, and mobile phones.
Examination of these may assist in linking or excluding:
two or more devices or scenes;
a suspect to a device; and
identifying the construction, source and history of a device.
The examination of different types of trace evidence are addressed in chapters throughout this
series (including Chapter 88 (Fibres and Hairs) and Chapter 90 (Paint)) and by Strobel (2012
pp 142-144), however the examination of some of the materials in a post-blast context will be
addressed in this section.
Trace evidence from an explosion scene should be examined with a microscope, categorised,
reconstructed and analysed as required for identication. If necessary, as the investigation
proceeds, items from the scene may have to be compared to standard commercial products or
material seized from suspects (R v Reyat (1993) 80 CCC (3d) 210; 25 CR (4th) 125n
[84.1900]).
The size of fragmentation/debris is generally smaller the closer the original material is to the
explosive event (eg, closer to the device at the time of initiation). This is because the pressure
is greater when closest to the explosive event and decreases as the distance from the device
increases. This is the key reason why primary fragmentation (eg, container, power source etc)
is generally recovered as tiny pieces that are sometimes difficult to identify.
The range of materials that may be recovered post-blast is vast, but some are much more
common than others. Examples include: timers, batteries, switches, wires and electrical
connectors, some of which are illustrated by Thurman (2011). Illustration can also be achieved
simply by looking around most homes, shops and electronics stores. There is nothing unusual
about the components of IED initiation mechanisms. What is important is to be able to
recognise device components in post-blast debris and reconstruct the device. Industrial
products can be identied and tracked through thorough police work and consultation with
manufacturing industries and retailers. This investigative process supported by electronic data
processing, may lead to identication of customers.
Those involved in examining post-blast debris should be familiar with the potential
signicance of what they may view under a microscope. This is rather like triage. While the
intent may be to seek traces of explosive residues, recognition and understanding the
signicance of battery components or chemicals, electronic parts and burned switch
components may advance the investigation in other useful directions.
To be able to make this type of contribution requires the same 3P approach as lawyers take
to a trial: prepare, prepare, prepare. For the scientist and reconstruction expert alike, the how
to is: test, test, test. Any likely IED component as determined by experience, from literature
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or by searching the internet, can be acquired, taken apart, and then blown up under conditions
designed to maximise recovery. This process provides experience, establishes memory and
provides on-going photographic, documented, physical and chemical databases for future
reference.
A simple looking battery may consist of a painted metal container with interior plastic
containers within which are cylindrical batteries containing various components and chemicals.
The best time to study its anatomy and the chemical composition of its constituents is before
an explosion so that the components can be identied post-blast.
Electronic devices are complex instruments. The post-blast expert should work together with
the technical specialists in the reconstruction of the device. The specialists can assist in
identifying unknown components or assist in determining the electronic circuitry that would
have been utilised to construct the device.
Polymers are another common class of materials associated with IEDs. Examples are paint,
bres and textiles, plastic, glues, rope, monolament line and adhesive tapes. All can constitute
chemical and physical evidence and there is a lot of literature pertaining to their analysis.
Polymers can usually be identied by their infrared spectrum. In a comparison of polymeric
materials and other chemical evidence, the objective is to apply analytical methods which are
designed to detect signicant differences in composition whereby the samples can be
differentiated. For polymers, such additional methods typically include: pyrolysis gas
chromatographymass spectrometry (py GC/MS); scanning electron microscopy with energy
dispersive x-ray analysis (SEM/EDX); Raman spectroscopy; and micro x-ray uorescence
spectroscopy (XRF). These methods are described in several works including the following
chapters in this series: Chapter 88 (Fibres) and Chapter 90 (Paint). Was-Gubala and Krauss
(2004a) and Was-Gubala and Krauss (2004b) discuss damage observed to textiles and single
bres as a result of vapour cloud explosions, which may be signicant if determining whether
clothes/items have been associated with an explosion. Baker et al (2012, Ch 8 pp. 318-322)
also have discussed and illustrated explosive damage to fabric in the context of air disasters.
Was-Gubala (2009) provides a summary of research into the forensic examination of bres and
the interpretation of analytical results, including measurable effects of destructive processes
(including res and explosions) on bres.
Quirk et al (2009) discuss the evaluation of carbon and hydrogen stable isotope values of
plastic in order to determine whether fragments of plastic recovered post blast could be
associated with a common source and also with a specic pre-blast source. The specic
scenario evaluated in this work was post blast fragments from a two-way radio could be
associated with its undamaged pair. This was achieved when three or more post-blast
fragments were recovered.
IED components often are physically bound with adhesive tape. Tape usually survives an
explosion and can be compared to adhesive tapes in possession of a suspect [R v Reyat (1993)
80 CCC (3d) 210; 25 CR (4th) 125n [84.1900]). Dietz et al (2012) report on the application of
carbon isotope ratio measurements of PVC tape backings to discriminate and also associate
samples as originating from a common source. The carbon isotope values were generally
preserved during the explosion, allowing association of pre- and post- blast samples. Further,
adhesive tapes can carry signicant physical evidence such as ngerprints and DNA (Zamir et
al, 2000), and material such as bres, hairs and detritus adhering from where and from whom
the device was assembled.
Several authors have studied adhesive tapes, including Maynard et al (2001); Sakayanagi et al
(2003); Bradley et al (2006) and Goodpaster et al (2007). These papers provide a useful
general discussion of tape analysis and differentiation, both based on chemical composition
and the potential to perform physical matching/ts between ends of tape.
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Document examination
[84.1280] Documents such as personal effects ie identication documents, records, labels,
boxes, manuals and notes bearing handwriting, stencils, print etc. can be very useful evidence
in a forensic examination, including post-blast investigations (Blueschke and Kwasny, 1989).
Two case examples illustrate this. Garstang (2012 Ch 7 pp. 267-271) describes the treatment of
documents to preserve them after being water soaked. The method involved freeze drying and
coating with parylene. IR analysis techniques enabled writing in a burned area to be read
which indicated alterations to a maintenance document. The document contained the probable
cause of an air disaster (ie re caused by under-inated tyres).
In R v Reyat (1993) 80 CCC (3d) 210; 25 CR (4th) 125n ([84.1900]) the examination of a
handwritten stencil on a cardboard fragment recovered post-blast narrowed the number of
possible sources of the stereo housing the bomb to single digits out of 4000 produced in Japan
and Korea. The cardboard had originated from the box which contained the stereo. The box
markings pertained to shipping. A fragment of the operating manual indicated recent purchase.
Both were accepted by the court as important pieces of evidence.
Metallurgy
[84.1290] Damage
Explosives may leave very characteristic signatures in metal such that explosive damage can
be distinguished from impact damage or structural failure. Thus, metallurgical examination can
be a very productive approach to the investigation of suspected explosions, including in the
event of aircraft accidents when the primary question is Was there an explosion? rather than
What was the explosive? (Tardif and Sterling, 1967; Baker et al, 2012 Ch 8; Garstang, 2012
Ch 7). If damage to metal is identied as explosive related, then this can assist in identifying
device components (eg, containers) and suitable surfaces for further forensic examinations.
Examinations of metal plates that may have been utilised to direct force, and metal containers
including pipes, wires and other metal objects, can be aided by a metallurgist, particularly
during the reconstruction of the items.
Walsh et al (2003) conducted a study on the post-blast micro-structure and hardness of three
common metals used in pipe bombs to assist in developing a method for the investigation of
pipe bombs. The damage to the microstructure increased with increasing velocity of detonation
(VOD) and pressure generated by the explosive. The material hardness increased sharply and
then plateaued as the pressure and VOD increased. Gregory et al (2010) discuss the
characterisation of post-blast metal fragments, specically microstructural changes and
microhardness, and the potential to correlate the fragment damage with the type of explosive
ller and bomb design.
[84.1300] Toolmarks/serial number restoration
Metal is also a good source of toolmarks. Chapter 85 of this series describes toolmark
identication. Lang and Klees (2008) have studied toolmarks left by drill bits and determined
drill bit use indicators. They concluded that trace deposits of particulate matter or smears,
physical damage including chipping, abrasion and ssuring on the bit, and thermal effects were
primary indicators of drill use. They also determined that well dened tool marks were
produced on swarf shavings which could be matched to a particular drill bit. This is pertinent
to IEDs such as a pipe bomb in which a hole is drilled to permit insertion of a fuse. The noted
paper provides a good literature review of the topic. Tools such as wrenches used in pipe and
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end cap manipulation can leave toolmarks. Toolmarks on wires (and plastic coatings)
originating from cutting implements is also useful evidence in associating or excluding a
specic tool with a mark or associating a number of marks on different samples.
The restoration of serial numbers is also a discipline of value in a post-blast investigation. The
restoration of serial numbers from a damaged vehicle chassis during the investigation of the
Bali bombings (2002) clearly demonstrates the value of this discipline (refer to [84.2080]).
Pathology
[84.1325] There is advantage in a multidisciplinary approach to the examination of the
bodies and body parts of deceased persons after an explosion. The examination team(s) may
comprise one or more practitioners from each of the following disciplines:
DVI practitioner;
forensic pathologist;
forensic anthropologist;
crime scene examiner;
ngerprint expert;
forensic chemist; and
bomb technician.
The forensic pathologist and forensic anthropologist have complementary roles in examining
the human remains. The role of the forensic pathologist is one of a primary examiner, for the
purposes of identication and to assess any injuries that may be present. The forensic
anthropologist can assist the examination, particularly where bone is present, by identifying
disrupted, heat damaged and badly decomposed body parts for reconstruction and subsequent
identication of individuals.
The examination team also needs to include experienced photographers and scribes. Each team
must work to recognised quality assurance standards using consistent standard operating
procedures (SOPs).
Trauma to a body can provide some evidence about the nature of the explosion, for example:
presence and degree of injuries;
explosive chemical, biological and physical trace evidence.
Presence and degree of injuries
It is important to note that injuries caused by dispersed chemical explosions can present
differently to those that occur after a concentrated explosion. The longer burning effect that is
produced in a dispersed explosion causes greater thermal damage to the skin than that seen in
a concentrated explosion. However, the extreme incineration observed in some victims is
almost always caused by post-blast re, regardless of the type of explosion. Additionally,
disruption of the body and typical explosive (triad) injuries may also be observed in victims of
a dispersed explosion, but they are caused by the environment and are not a result of proximity
to the point of ignition. Blast injuries also occur after a dispersed explosion.
Six categories of injury resulting from a concentrated explosion have been dened by Marshall
(1988) as:
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1. complete disruption;
2. explosive injury;
3. injury by separate fragments;
4. injury by falling masonry;
5. burns; and
6. blast.
1. Complete disruption of a body is generally associated with direct contact with the
source of the explosion. The disruption may be localised to one of two regions of the
body for example, localised, complete disruption of the hands and lower parts of the
arms may imply that the source of the explosion was being held. Accordingly, body
parts assume great importance by implication of contact or very close proximity to the
source of explosion; this should be borne in mind when sampling for explosive
residues (see below).
2. The second category of injuries is Explosive Injury which consist of a triad of
penetrating (puncture) injuries, abrasions and bruises. This triad is typically seen in
victims who are close to the blast seat but not in contact.
In both Complete Disruption and Explosive Injury above, there is generally a
dirty appearance to the skin due to the forceful impregnation of smoke and explosive
residue.
3 and 4. There may be penetration of the body by fragments of debris from the explosives
source or surroundings. Similarly, dislodged masonry may collapse and cause
secondary injuries to the body.
5. Supercial ash burns can occur on the skin if the victim is very close to the
source, but they are usually not signicant. Most burning of victims is a consequence
of post-blast re, rather than from the explosion itself.
6. Air pressure changes consequent to an explosion can cause internal injuries, involving
organs and tissues where there is an interface between air and the tissue including:
lungs;
airways (bronchi);
ears;
sinuses; and
stomach and intestine.
Four categories of clinical blast injuries are also described in the general literature:
Primary injuries shockwave overpressure causing barotraumas;
Secondary injuries caused by primary (source) fragments or secondary
(environmental) fragments;
Tertiary high speed wind causing falling, tumbling; falling masonry; and
Quarternary burns; asphyxia caused by toxic fumes; and chemical, biological,
radiological and nuclear.
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The interpretation of injuries is important in reconstructing the incident, and placing the victim
at the scene. For example, the location on the body, the direction of penetrating injuries and
heat damage can be used to extrapolate the direction and proximity of the explosive source.
Recovery of explosive trace evidence
The body can be a very effective medium for stopping and retaining not only primary
fragmentation, but also explosive residues. Recovery of such pertinent physical evidence is
valuable to an investigation. Indeed, the mere existence of such foreign material on a body
assumes great signicance when the primary question is not What was the explosive? but
rather Did an explosion occur? as in an aircraft crash.
As indicated above, it is important not to neglect body parts when attempting to recover
explosive trace evidence. The evidence may be located on clothing and/or the surface of the
body (including in the hair), as well as in the depths of penetrating injuries.
Examination protocol for bodies and body parts
External examination
Careful recording of the location and direction of injuries, as well as the overall appearance of
the body or body part should be made, including photographic record, diagrams and text
description.
Laposata (1985) has described the protocols listed below for collecting trace evidence from
bombing victims.
The external and internal examinations of a body may include a number or all of the steps
below; however, these will be dictated by the specic requirements of the incident and
available resources.
(1) Radiography (plain lm x-rays and CT)
(a) dead body
(b) body parts and tissue fragments from the scene
(c) surgical specimens
(d) survivors (including direct magnication radiography)
(2) Recovery of explosive residues
(a) inspect for unconsumed or partially consumed explosives
(b) swab with appropriate solvents, include control swab
(c) collect ngernail scrapings
(d) sample scalp hair
(e) perform magnetic sweep
(3) Examination of clothing and body surfaces
(a) remove radio opaque (revealed by x-rays) evidence
(b) search for and remove radio lucent (not revealed by x-rays) evidence
(4) Package clothing.
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Internal examination
(1) remove radio opaque evidence;
(2) dissect wound tracks and remove radiolucent evidence;
(3) re-radiograph;
(4) full post-mortem examination if authorised.
Where possible, police and/or forensic scientists should accompany injured persons to hospital
and seize any materials recovered (likewise with the deceased at autopsy). All materials
removed must be appropriately packaged and submitted to the forensic laboratory via the
normal procedures for continuity of evidence. If a post-blast examiner cannot attend the
autopsy or hospital, the pathologist should consult the examiner prior to collection.
Background information
Depending on the circumstances, a forensic pathologist and anthropologist may have attended
the scene. If not, the following information should be made available prior to the autopsy:
(1) position of the body at the scene in relation to the centre of the explosion and large
objects at the scene;
(2) post-explosion alterations of the scene which could produce observed effects to a
body other than explosive-related trauma (re extinguishing chemicals, weather,
structural collapse, secondary re);
(3) suspected bomb type (undisguised, disguised, hidden; that is, an indication of the
possible nature of material from an improvised explosive device (including any
containers or casing in which the device may be placed) which could be found in or
on a body; and
(4) materials in the environment (for example, car interior, room furnishings; ie material
of known origin which might be found in or on the body).
The following literature, and references therein, provide further information on blast injuries
and forensic pathology of victims of explosions:
The (United States of America) Armed Forces Institute of Pathology (undated) has a
website with comprehensive information on pathology.
Kitulwatte and Pollanen (2012, Ch 19) Centers for Disease Control and Prevention
(2006);
NFPA 921 (2011, Ch 23 and Ch 21 p. 203); and
Marshall T. (1988) A pathologists view of terrorist violence. For Sci Int. 36; pp57-67.
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Analysis and identication of explosives
[84.1350] The heart of an IED is the explosive. Identication of the explosive is the task
of the forensic chemist. Chemists can work only on what they receive from investigators and
scene examiners. For this section, the assumption for post-blast analysis is that all relevant
exhibits have been seized, there are no contamination issues, examinations for ngerprints and
DNA have been considered and that the question now is what was the explosive?. It is also
assumed that the laboratory quality assurance issues discussed at [84.1750] are in place and
operational.
There is no universally accepted combination of methods applicable to all cases. Rather, the
forensic scientist selects the procedures and instruments which are most appropriate to the
exhibits presented and the circumstances of the case. Some techniques cannot be utilised in
isolation to identify an explosive or explosive mixture. For instance, portable detection
instruments such as IMS are generally used as screening techniques to produce results for
intelligence purposes or for the triaging of items. Any results that are required to be presented
in court should be conrmed using an analytical technique or combination of techniques back
in the laboratory.
Guidelines developed by the Technical Working Group for Fire and Explosives TWGFEX
(undated and 2007) for the forensic identication of intact (unconsumed) explosives and their
residues, provide an overview of the techniques that are regarded as presumptive and the
required combination of techniques to produce a conrmatory result for a range of explosive
types.
Three key factors that will determine what instrumentation will be employed are:
are the samples trace (ie not visible to the naked eye) or bulk (ie visible to the naked
eye)?;
are the results required for court purposes?;
is the purpose of the analysis to identify the material or to compare with other
samples to conrm common origin?; and
to what instruments does the chemist have access?
Examination of debris and analytical preparation
[84.1360] A owchart providing an overview of a generic analytical sequence for the
analysis of debris (including items and fragments) for explosive residues is shown in Figure 3.
The analytical sequence will vary based on available resources and the circumstances of each
case. As can be seen in Figure 3, the examination procedure will generally be based on the
following ve phases. An overview of each phase is provided in this section.
(1) vapour analysis;
(2) visual and microscopic examination of debris for bulk explosives;
(3) swabs and solvent extraction of debris for trace explosives;
(4) chemical and instrumental analysis; and
(5) reporting.
Details of analytical techniques are provided in Appendix A at the end of the chapter. The
application of these techniques is discussed in this section. Abbreviations are listed at the start
of the chapter.
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Figure 3 Generic analytical sequence for explosive residue analysis
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(I indicates techniques utilised for the analysis of inorganic compounds and O indicates
techniques utilised for the analysis of organic compounds).
Vapour analysis for volatile organics
[84.1370] Air from the seat of an explosion or from sealed containers of debris can be
analysed for the presence of explosive vapours. This is commonly known as headspace
analysis and is useful when analysing for volatile compounds such as TATP, EGDN and NG.
Due to the volatility of the compounds, it is important to collect an air sample or package the
debris in airtight containers as soon as practical otherwise these compounds may be lost to the
atmosphere.
In order to collect the air sample, a portable pump is sometimes used to sample the air from
around the seat of the explosion or from material suspected to have been in contact with an
explosive by drawing the air through a substance which adsorbs explosive vapours. The same
process is applied in the laboratory to heated debris in nylon bags, mason jars or unused paint
cans and is referred to as direct headspace sampling. The most commonly used adsorbents
are charcoal (Garner et al 1986) or Tenax (a proprietary resin) (Wardleworth and Ancient,
1983; Deak et al, 1989). Adsorbed explosives are recovered by solvent extraction.
Volatile organics can also be trapped directly onto an adsorbent material such as charcoal. This
form of passive headspace sampling is achieved by placing the adsorbent material in the
sealed container with the debris. The container can then be left to equilibrate at room
temperature or may be heated in order to volatilise the organic vapours that are subsequently
trapped on the adsorbent. Adsorbed explosives are recovered by solvent extraction.
Solid Phase Micro Extraction (SPME) is also available for passive headspace sampling. SPME
is based on the adsorption of the volatile organic onto a bre which consists of a stationary
phase on a ne length of fused silica. This can either be directly injected into an analytical
instrument such as a GC/MS or extracted with a solvent. Examples of its application are
discussed at [84.1610] and [84.1650].
Visual/microscopical examination for explosives and other trace
evidence
[84.1380] Visual and microscopical examination of debris requires meticulous attention to
detail combined with the knowledge and ability to recognise and recover pertinent evidence.
The efficiency and effectiveness of the examination also reects the extent to which materials
of high evidential potential have been selected for submission to the laboratory. The emphasis
is on searching for:
(1) trace evidence from explosives ie unconsumed or partially consumed explosives;
(2) device remains; and
(3) other forensic trace evidence.
All recovered materials should be recorded and photographed before analysis.
Residues from explosives may be recovered as recognisable particles of unreacted or partially
reacted explosives. These commonly are low explosives, including grains of propellant powder
and components of improvised chemical mixtures. Less commonly, traces of unreacted high
explosives, eg, dynamite, plastic explosives, slurries and emulsions, may be recovered.
Signicant quantities of unreacted high explosives can be recovered if the explosive low
orders ie the explosive is not fully converted to gaseous products.
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Particles of unreacted explosive or of crystalline residue which are physically recovered from
debris are examined microscopically and typically analysed by one or a combination of the
instrumental techniques outlined at [84.1410].
High explosives usually are wrapped in paper or plastic. Fragments which survive the
explosion may contain traces of impregnated explosives which can be extracted and identied.
Dynamite and some brands of emulsion explosives have paper wrappers. Slurry and emulsion
explosives are frequently packaged in plastic sausages, the ends of which are sealed with a
metal clip. Metal clips invariably survive an explosion and, if recognised, can provide an
immediate clue to the type of explosive used. Access to a reference collection of wrappers of
explosives is a useful resource for forensic laboratories.
The visual search also incorporates the search for any primary fragmentation that may assist
the reconstruction process. These fragments can also be examined for ngerprints, DNA and
trace explosive residues as required.
Swabs and solvent extraction of debris for trace explosives
[84.1390] If unreacted explosives or solid residues are not recovered during the
microscopical examination, then solvent extractions from surfaces of interest are conducted
(either by direct solvent washing or collection using a swab). Materials which have sustained
extensive damage, such as parts of a device, clothing, and blackened (as opposed to burned)
material have high potential for residue recovery by solvent extraction.
The objective is to maximise the extraction of explosives and minimise co-extracted
contaminants. The rst step, typically, is to collect extractions from materials such as metal
and glass which are less likely to produce interfering co-extracted compounds than, for
example, plastics and clothing. Surfaces are also selected based on their suspected location
relative to the device at time of detonation, with priority given to primary fragments that were
suspected of being part of the device.
Solvent selection depends both on the explosive sought and the material from which the
explosive is to be extracted. The solvent is applied either by swabbing or by direct solvent
washing. A minimum quantity of solvent is used. The solvent extract remaining after the
swabbing or washing is collected for clean-up procedures ([84.1400]) and subsequently
instrumental analysis ([84.1410]).
A general sequence of solvents for an unknown explosive is as follows:
(1) polar organic solvent for organic explosives (and some oils and waxes); and
(2) water for inorganic compounds.
Organic explosives are generally extracted with polar organic solvents such as methanol,
acetonitrile, acetone, or isopropanol. The sequence may also include a non-polar organic
solvent extraction for oils and waxes prior to use of the polar organic solvent if commercial
emulsions are suspected.
The non-polar organic solvent step is included because of the increasing market share of
emulsion explosives which contain oils and waxes which might not be readily soluble in some
polar organic solvents. Solvents such as iso-octane (Bender, Crump and Midkiff, 1993),
dichloromethane or pentane can be utilised for oils and waxes.
Inorganic components are extracted with ultra-high purity water (eg, de-ionised or MilliPore
water). These may be unreacted components of explosives such as ammonium or sodium
nitrate, or reaction products such as sodium chloride or potassium sulphate (Beveridge et al,
1975). Water also extracts non-explosive related inorganic compounds such as sodium chloride
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of natural origin, ammonium nitrate from fertilisers, and sodium bicarbonate and ammonium
dihydrogen phosphate from re extinguishers etc.
This procedure generally yields organic fractions, an inorganic fraction and an insoluble
fraction (Garner et al, 1986; Beveridge, 1992). Each fraction is analysed systematically (see
Figure 3 at [84.1360]).
An alternative method used in some laboratories is to extract with a 1:1 mixture of ethanol
(polar organic solvent) and water, which yields one solution and insoluble material.
Alternatives also include utilising one organic solvent (such as acetonitrile) that extracts both
the oils and waxes and the organic explosive, and water for the inorganic components,
resulting in two extracts for instrumental analysis. Some laboratories utilise dry swabs or
commercially available medi-wipes (in the eld and laboratory) that are extracted with suitable
organic and inorganic solvents. The increasing use of peroxide explosives has resulted in a
more specic extraction solvent, eg, acetonitrile.
Twibell et al (1982); Russell (1984); Warren et al (1999); Thompson et al (1999); Broome and
Todd (2009); Song-im et al (2012a); Song-im et al (2012b); Romolo et al (2013); De Tata et al
(2013) and others discuss various research on the recovery, extraction and clean-up of traces of
organic and inorganic explosive residues.
Clean-up procedures
[84.1400] The collected solvent extracts are sometimes subjected to a clean-up procedure
prior to instrumental analysis. There are two reasons to clean-up extracts of explosive residue.
One is to protect analytical instrumentation from substances which could impair performance
of columns and detectors; the other is to remove substances which could mask detection of
traces of explosives. In some circumstances, the chemist may decide not to conduct a clean-up
procedure. This may be the case if the extract appears to be relatively clean, the concentration
of the explosive is suspected to be low, or highly specic detection methods are utilised that do
not require the same level of clean-up (eg, MS/MS).
A common way to clean-up organic extracts is to place the extract on a vertical column of
polymer material and then pass a solvent or mixture of solvents through the column. The
explosive is retained on the column and the contaminants pass through. The explosive is
subsequently recovered from the column.
Inorganic extracts can be cleaned-up by centrifuging or ltering. Pre-washed membrane lters
should be used rather than paper lters, since the latter contain detectable quantities of ions
such as nitrate, chloride and sulphate which are among those sought in explosive residues.
Ammonium and nitrate ions can be destroyed by bacterial action, so solutions to be analysed
should not be left standing at room temperature for more than two to three days. Bacterial
action can be counteracted with chemicals such as phenol, methanol and borax. A portion is
retained in solution for analysis by methods which require liquid samples, for example, ion
chromatography and capillary electrophoresis.
A second portion of the solvent can be evaporated under air or nitrogen at room temperature in
order to analyse the remaining residue. This provides an alternative technique for the analysis
of the sample (eg, IR can be utilised to analyse the solid residue).
Twibell et al (1982); Lloyd (1985); Douse and Smith (1986); Tamiri and Zitrin (1986); Lloyd
and King (1990); Beveridge (1992); Song-im et al (2012a); Song-im et al (2012b); Romolo et
al (2013) and De Tata et al (2013) discuss options for different clean-up procedures.
Chemical and instrumental analysis
[84.1410] Developments in the sensitivity and selectivity of instrument detectors continue
to improve detection limits for explosives, but no one method can detect all components of all
Update: 73
84 - 17055
explosives. Scientists therefore have to analyse explosive residues systematically and
comprehensively. If particles of unreacted explosive are recognised and recovered, then the
protocol required for identication is relatively straightforward. For multi-component
explosives, like dynamite, several methods may have to be employed. If the question is What
brand of explosive is this? or Compare these explosives and determine if they could have
had a common origin then additives and minor components (such as trace elements) or
isotope ratios may also have to be determined.
There is no universally agreed upon method for the analysis of explosives. There are, however,
widely accepted criteria. An important one is that a single chromatographic analysis in which
the retention time (for TLC, retention factor) of an unknown compound matches that of a
standard does not by itself constitute identication. This applies to GC, LC, IC, CE and TLC.
However, if the detector on the chromatograph is a mass spectrometer, then identication may
be achieved. Techniques like IR, XRF, Raman, XRPD and SEM/EDX may provide
unambiguous identication of compounds and elements. Royds et al (2005) provide an
overview of analytical methods for explosive residue analysis, including advantages and
limitations associated with each. Yinon (2007, 1999) and Beveridge (2012) provide in-depth
discussions on the application of various techniques for the detection, analysis and
identication of explosives.
Examples of techniques that can be utilised for the analysis of bulk explosives and solvent
extracts are provided in the following sections. These are also represented in Figure 3 at
[84.1360]. Descriptions of each of the analytical techniques with regards to theory of operation
are provided in Appendix A. For the purpose of this section, instrumentation is grouped
according to fundamental principle of operation, ie chromatography, electrophoresis,
spectrometry or spectroscopy. The results from each of these techniques are generally
produced in the form of chromatograms (chromatography), electropherograms (electrophoresis),
and spectra (spectrometry and spectroscopy).Techniques include:
(1) Chemical colour tests and thin layer chromatography (TLC)
(2) Chromatography
(a) gas chromatography (GC)
(b) liquid chromatography (LC, commonly known as HPLC high performance
liquid chromatography)
(c) ion chromatography (IC)
(3) Electrophoresis
(a) capillary electrophoresis (CE)
(4) Spectrometry
(a) mass spectrometry (MS)
(b) ion mobility spectrometry (IMS)
(c) isotope ratio mass spectrometry (IRMS)
(5) Spectroscopy
(a) infrared spectroscopy (IR or FTIR Fourier Transform IR)
(b) Raman spectroscopy
(c) scanning electron microscopy / energy dispersive x-ray spectroscopy
(SEM/EDX)
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(d) x-ray uorescence spectroscopy (XRF) and
(e) x-ray powder diffraction spectroscopy (XRPD).
The US-based TWGFEX Laboratory Explosion Group (TWGFEX, 2007) has published
guideline tables which categorise analytical techniques for intact explosives and post-blast
residues into four groups.
1. Category 1 provides signicant structural and/or elemental information and is
sufficient for identication.
2. Category 2 provides limited structural or elemental information and requires one more
supporting technique for identication.
3. Category 3 provides a high degree of selectivity but requires two more supporting
techniques for identication.
4. Category 4 are useful but do not fall into categories 1, 2 or 3 and require three more
supporting techniques for identication.
Techniques that fall into Categories 1 and 2, include: IR, Raman, GC/MS, LC/MS, XRD and
EDX. The material being analysed will dictate whether the technique is regarded as a Category
1 or 2.
Techniques that fall into Category 3 include: GC, GC/CL (TEA), LC/CL (TEA), TLC,
IMS, and microscopy (stereobinocular or polarising).
Techniques that fall into Category 4 include: burning tests, colour tests and melting point
measurements.
The bottom line, however, is that while it is essential for forensic scientists to set standards for
themselves, it is the courts which determine whether the evidence is admissible. Like scientic
theories, analytical methods and protocols last for as long as they can withstand challenges
from counsel well briefed by independent experts who may testify and / or advise counsel. If
analytical methods and protocols withstand legal challenges, they are maintained. If they do
not, they are revised.
Bulk explosives
[84.1420] Particles of unreacted explosive or of crystalline residue which are physically
recovered from debris are examined microscopically and typically analysed by one or a
combination of the instrumental techniques: IR, Raman, XRPD, micro-XRF, or SEM/EDX.
Chemical spots tests, TLC, and burn tests can also be employed (generally prior to undertaking
instrumental analysis).
If the particles are a mixture of organic and inorganic compounds, components can be
separated by solvent extraction and individually identied. The procedures and analytical
methods are similar to those described below for trace residues except that clean-up is not
required.
Organic extracts
[84.1430] Materials extracted by organic solvents may contain explosives, non-explosive
additives and co-extracted contaminants. A high concentration of co-extracted material relative
to explosives usually necessitates clean-up procedures.
Update: 73
84 - 17057
Techniques available for the analysis of organic extracts include: IMS, chemical spot tests,
TLC, GC and LC with a suitable detector such as MS.
The availability of detonator-sensitive emulsion explosives, and the possibility of bulk ANFO
being used in large scale explosions, means that there should also be a screen for petroleum
oils and waxes. IR, GC/FID and GC/MS are suitable methods. Since oils and waxes are widely
used products, it is important to analyse relevant control/reference samples.
If nitrate esters, nitramines or nitro-compounds are identied, then the class of explosive is
established and specic additives may be sought.
Inorganic extracts
[84.1440]
Unevaporated extract
Inorganic solvent extracts are analysed for cations (positive ions) and anions (negative ions) by
ion chromatography. Since the ions are indicated by response time only, and since response
times can be affected by parameters such as concentration, further conrmation is required.
One simple method is to spike a second sample with the indicated ion and observe the
response. However, a second method is desirable. Capillary electrophoresis has been shown to
be a complementary method for anion conrmation (McCord et al, 1994). An alternative
method for conrming the presence of an ion would be to use the same analytical technique
(eg, IC or CE); however, analyse the samples a second time utilising a different analytical
column (ie different stationary phase/packing). This is also an option for GC and LC
techniques when analysing organic extracts.
Evaporated extract
Evaporation is typically achieved quickly on a steam bath or slowly at ambient temperature
using a stream of nitrogen gas.
(1) Crystalline residue: if the evaporated residue is solid, methods of analysis are drawn
from IR, Raman, SEM/EDX, micro-XRF, and XRPD.
Depending on the sample composition, these methods can provide denitive
identication. Spot tests may be used for screening if there is sufficient sample.
If the analysis of an evaporated extract indicates more than one compound, for
example, sodium nitrate and potassium chloride, these compounds might not have
been present in the residue prior to extraction; the ions might have been originally
associated as potassium nitrate and sodium chloride.
(2) Syrups: if the residue is a syrup, this could indicate residual sugar. Such samples are
unsuitable for analysis by XRPD. Refer to section 84.1600 for a summary of
analytical techniques for sugars.
Evaporating a sample and analysing the residue by IR, Raman, SEM/EDX, micro-XRF or
XRPD, provides non-chromatographic identication (see below) but if certain ions (ammonium,
nitrite, methyl ammonium, chlorate) are present in only low concentrations they can be lost
on evaporation (Reutter et al, 1983). If these ions are sought, the IC/CE protocol is most
appropriate.
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Insoluble material
[84.1450] Insoluble material in solvent extracts of explosive residues may include such
materials as unreacted aluminium from slurries, emulsions and improvised explosives; barium
sulphate from a limited number of dynamites and slurries (particularly those for seismic
application); microballoons from emulsions; manganese dioxide and zinc from battery cores;
and metallic oxides.
The methods used for the analysis of these materials can include: IR, Raman, SEM/EDX,
micro-XRF and XRPD (Beveridge, 1975; Beveridge and Lothian, 2004; Lim et al, 2007 and
Bender and Beveridge 2012, 2012).
Identication and Interpretation
[84.1510] Determination of the appropriateness of analytical techniques and the
signicance of the analytical results are primary responsibilities of a forensic scientist and are
the essence of reporting and expert testimony. That is, what do the results of the analyses
mean? This section focuses on issues pertaining to the positive identication of the major
classes of explosives typically found in IEDs. In criminal trials in common law jurisdictions,
identity and comparison of materials must be proved beyond a reasonable doubt.
The composition of post-blast residues will depend on the chemicals utilised in the main
charge and initiation systems, the efficiency of the explosion reaction, materials/chemicals
present in the environment at the time of the blast, and the treatment/handling of the items
containing the residues following the blast eg, exposure to the environment and/or other
examination conducted on the item prior to explosive residue analysis. Murray (2012) provides
an overview of key factors with respect to interpretation and determining the signicance of
analytical results. After a reminder that all personnel, working areas, equipment, and
instruments must be demonstrably free of explosives, he discusses the pertinent factors
inuencing interpretation and signicance, and which scientists should consider, to be as
follows:
are explosive residues present?
what are these materials and where do they occur?
what are the background levels?
how much is present?
how could material be present where it was found?
The analytical sequence, regardless of the type of explosive, will generally follow a common
path as detailed in Figure 3 at [84.1360], ie microscopy and analysis of any intact particles,
solvent extractions from swabs or washings and instrumental analysis. This section addresses
the post-blast identication of residues, however also encompasses the identication of intact
samples which will aid pre-blast association of samples for common origin or comparison of
post-blast to pre-blast recovered samples.
Propellants
[84.1520] Low explosives generally encompass propellant powders and inorganic
chemical mixtures initiated by ame when contained in a pipe or similar vessel (Oxley et al,
2001). Analysis of low explosives has been reviewed, illustrated and discussed by Bender and
Update: 73
84 - 17059
Beveridge (2012 Ch 11). The following sections discuss the identication of common
propellants, both pre- and post-blast, including black powders and their substitutes and
smokeless powders.
[84.1530] Black powder and black powder substitutes
Black powders classical composition is potassium nitrate: sulphur: charcoal (75:15:10).
Commercial products are manufactured in various size ranges and visually are black, shiny,
irregularly shaped grains. Potassium nitrate is easily identied by IR and Raman spectroscopy.
If extracted with water, the ions can be identied by IC and a complementary method such as
CE. Sulphur may also be identied by IR spectroscopy or by SEM/EDX. Bradley (2005)
discusses a method for the identication of elemental sulphur in explosives and explosive
residues utilising GC/MS. If an SEM/EDX is equipped with a low element detector, carbon
may be detected. If a sample is burned, some sulphur is converted to sulphate and thiocyanate
and carbon to carbonate. Both of these ions can be identied by IR or Raman or in solution by
IC and a complementary method (eg, CE).
Many black powder substitutes have appeared on the market with various components and
additives. Black powder substitutes generally consist of a carbonaceous organic fuel and
inorganic oxidisers such as KNO
3
and/or KClO
4
. The fuel source may include: charcoal,
sulphur, sodium benzoate, dicyandiamide, nitrobenzoic acid or ascorbic acid (Bottegal et al,
2010).
Analysis of intact powder
For certainty in identication of black powders, the morphology and the chemical composition,
including each component, should be determined. Table 1 provides an overview of components
of black powder and substitutes, together with the techniques that can be used for the analysis
of the different components of intact particles. All of these have been or can be used in IEDs,
particularly in pipe bombs.
Pyrodex and Triple Seven are common black powder substitutes which share the same
visual appearance and oxidisers (potassium nitrate, potassium perchlorate), however different
fuels. Pyrodex contains charcoal, sulphur, sodium benzoate and dicyandiamide (DCDA),
whereas Triple Seven has no sulphur but contains 3-nitrobenzoic acid (Routon et al, 2011).
The components of intact Pyrodex other than carbon can all be identied by IR, Raman and
XRPD (NB Of these techniques only Raman can identify the presence of carbon). SEM/EDX
identies Na, K, S and Cl, and may also identify C, N and O if equipped with a low element
detector. HPLC with a UV detector can indicate the presence of dicyanodiamide (DCDA) and
sodium benzoate (Bender, 1989a; Bender and Boyle, 2004), as can GC/MS. Nitrate and
perchlorate ions can be detected by ion chromatography and 3-nitrobenzoic acid can be
determined by GC/MS and FTIR (Bender and Boyle, 2004). In an alternative approach,
Dreifuss and Goodpaster (2004) applied reversed phase electron spray ionisation LC/MS
methods to identify nitrate, perchlorate, dicyanodiamide, and benzoic acid in Pyrodex and the
same compounds plus 3-nitrobenzoate in Triple Seven. The method also identied ascorbic
acid in intact powders. Klapec and Ng (2001) also discuss the use of CE for the detection of
sodium benzoate. Routon et al (2011) report on the derivitisation of the organic fuels in
Pyrodex and Triple Seven, with subsequent analysis by GC-MS. The method was successful in
the discrimination of Pyrodex and Triple Seven samples, both intact particles and post blast
residues.
Ascorbic acid has created some analytical difficulties because of its tendency to chemically
degrade. This property has led to applications directed at identifying degradation products of
ascorbic acid. Goodpaster and Keto (2004) have approached the problem by identifying
Expert Evidence
84 - 17060
ascorbic acid and degradation products by analysing trimethylsilyl derivatives by GC/MS.
Lang and Boyle (2007) applied the novel technique of IC/MS and successfully identied
diagnostic degradation products of ascorbic, though not the acid itself. In yet another approach
using older technology, McCord and co-workers applied IC complemented with CE to the
problem and reported that the methods permitted detection of both the inorganic oxidisers
(nitrate and perchlorate) and ascorbic acid (Bottegal et al, 2007). Bottegal et al (2010)
developed a gradient high-performance liquid chromatography/electrospray ionisation
quadrupole time-of-ight mass spectrometry (HPLC/ESI-QToFMS) method for the analysis of
the organic and inorganic components in black powder substitutes.
It follows that there are several approaches to the same end. Drawing from the noted literature,
Table 1 summarises the reported methods.
TABLE 1 Primary components and techniques for the analysis of intact particles
of black powder and black powder substitutes
Technique Black
Powder
Pyrodex Triple Seven Jim
Shockeys
Gold
IR,
Raman,
SEM/
EDX,
XRPD, IC,
CE
potassium
nitrate
potassium nitrate potassium nitrate potassium
nitrate
Raman,
SEM/EDX
sulphur sulphur - -
Raman,
SEM/EDX
charcoal charcoal charcoal -
IR, Raman
SEM/
EDX,
XRPD, IC,
CE
- potassium perchlorate potassium perchlorate potassium
perchlorate
GC/MS,
LC/MS IC,
CE,
IMS/MS
- - - ascorbic
acid
GC/MS,
LC/MS
- sodium benzoate sodium benzoate -
GC/MS,
LC/MS
- dicyanodiamide
(DCDA)
HN=C(NH
2
)NHCN
dicyanodiamide
(DCDA)
HN=C(NH
2
)NHCN
-
GC/MS,
LC/MS
- - 3- nitrobenzoic acid -
Update: 73
84 - 17061
Technique Black
Powder
Pyrodex Triple Seven Jim
Shockeys
Gold
HPLC/
ESI-
QToFMS
Ascorbate,
perchlo-
rate,
nitrate,
chlorate
anions
Analysis of black powder and black powder substitute post-blast residues
Table 2 summarises some of the available techniques for the analysis of major components of
post-blast residues (including anions and compounds) from pipe bombs containing black
powder and/or selected substitutes as detailed by [a] Bottegal et al (2007); [b] Lang and Boyle
(2007); [c] Dreifuss and Goodpaster (2004); [d] Bender and Boyle (2004); and [e] Bottegal et
al (2010). These data are a summary and representative only, and results will vary depending
on the conditions of the explosion.
TABLE 2 Techniques for the analysis of post-blast residues of black powder and
some black powder substitutes
Literature
Reference/
Technique
Black Powder Pyrodex Triple Seven Jim Shockeys
Gold
[a] IC/CE NO
3
-
, NO
2
-
,
SO
4
2-
, HS
-
,
HCO
3
-
, (Cl
-
)*
*
NO
3
-
, NO
2
-
,
Cl
-
, SO
4
2-
, HS
-
,
HCO
3
-
NO
3
-
, NO
2
-
,
Cl
-
, ClO
3
-
,
ClO
4
-
, HCO
3
-
NO
3
-
, NO
2
-
,
Cl
-
, ClO
4
-
,
HCO
3
-
,
ascorbate
(* contami-
nant)
[b] IC/MS NO
3
-
, NO
2
-
,
Cl
-
, ClO
3
-
,
ClO
4
-
, HCO
3
-
,
oxalate,
threonate
[c] LC/MS NO
3
-
, ClO
4
-
,
Cl
-
, CNS
-
,
benzoic acid,
DCDA
[d] XRPD K
2
SO
4
, KCl,
K
2
CO
3
KCl, K
2
CO
3
,
[d] HPLC Sodium
benzoate,
DCDA
Sodium
benzoate,
DCDA,3-
nitrobenzoic
acid
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Literature
Reference/
Technique
Black Powder Pyrodex Triple Seven Jim Shockeys
Gold
[e] HPLC/ESI-
QToFMS
Oxalate,
threonate,
nitrite,
chlorate,
nitrate,
perchlorate
Table 3 (see at [84.1630]) can also be utilised for an indication of typical inorganic reaction
products which may be relevant to components of different black powders. If intact or partially
consumed particles are recovered post-blast, then techniques represented in Table 1 would
generally be utilised for analysis.
[84.1540] Smokeless powders
Smokeless powders, which are widely available in bulk form in the United States of America
for hand loading, are commonly used as pipe bomb llers (Wolfe, 1991; National Research
Council, Committee on Smokeless and Black Powder, 1998; Kelly and Mothershead, 2001;
Oxley et al, 2001; Heramb and McCord, 2002 and Beveridge and Bender, 2012).They can
provide strong associative evidence if the brand can be determined. To do so requires a
combination of morphology and chemical composition including additives Powders are
manufactured in various forms which are designed for burning properties. Some more common
shapes are balls and discs which usually are double base powders, and tubes and rods which
usually are single base powders. Careful measurement of morphology is the rst step in
forensic examination. Size, shape, colour, surface appearance and texture can give a high
degree of discrimination. Recovered particles can be compared to reference particles. This is
followed by chemical analysis. Infrared spectroscopy should be used to conrm the presence
of nitrate esters and cellulose. The nitrate esters have characteristic peaks at 1648 cm
-1
,
1278 cm
-1
and 837 cm
-1
. The cellulose has characteristic peaks at 1004 cm
-1
, 1067 cm
-1
and
1159 cm
-1
.
To determine if the product is single or double base, an examination must be made for
nitroglycerine (NG). Appropriate methods range from TLC (Beveridge et al, 1975) to
instrumental methods including GC/MS, LC/CL, LC/MS and others (see below). These
techniques can also be utilised to identify the presence of other organic additives. Wissinger
BR McCord (2002) and Cascio et al (2004) refer to the analysis of smokeless powders using
HPLC.
In post-blast residues, the presence of the various components should be identied in the
solvent extracts (eg, NC and NG in the organic extract). In addition, high levels of nitrate ions
may be detected with IC and/or CE.
Identication of a powder as single or double base may suffice in minor investigations, but if
the purpose is to identify a manufacturer or to compare samples from a scene to powder in
possession of a suspect, then analysis and identication of the additives and their derivatives
(eg, DPA; N-nitrosodiphenylamine, N-NODPA; 2-nitropdiphenylamine, 2-NDPA; and
4-nitrodiphenylamine, 4-NDPA) should be undertaken. Additives can be extracted with an
organic solvent such as methylene chloride (ie dichloromethane) or chloroform and be
analysed with techniques including: TLC, FTIR, LC, GC, GC/MS, and CE. There is
considerable literature on the topic of additive residue analysis since the IED eld overlaps the
legitimate eld of propellants used in ammunition.
Update: 73
84 - 17063
Chemically, organic gunshot residue has the same composition as that of smokeless powders
used in an IED. The quantity of intact powder in the residue from an IED; however, is much
higher than in organic gunshot residue. Burleson et al (2009) report on a SPME technique to
extract organic gunshot residues (including DPA, EC and MC) from a single particle of
partially burnt smokeless powder. The samples were analysed utilising a GC-nitrogen
phosphorus detector (NPD).
Lopez et al (2013) also report on a method to estimate the age of gunpowder samples based on
the concentration of DPA and its derivatives (as determined by HPLC) over time.
One of the rst reported methods for the analysis for additives and their products was TLC
(Archer, 1975). McCrehan and Reardon (2002) of the United States of America National
Institute of Standards and Technology conducted a study with the purpose of determining the
state-of-the-art practice for forensic smokeless powder analyses. Reardon and McCrehan
(2001) also discuss a quantitative method for the extraction and analysis of powder additives.
The authors report that when the target analytes (NG, DPA, EC) were quantitatively recovered
by ultrasonic extraction and analysed with micellar CE (MEKC), compositional information
was obtained.
LC and CE are often the methods of choice, in part because they are operated at ambient
temperature which eliminates the problem of thermal degradation of additives which can be a
problem with GC analyses. McCrehan and Bedner (2006) used both methods to derive an LC
reference standard containing NG, DPA, N-nitrosodiphenylamine, and ethyl centralite.
McCrehan et al (2002) used CE to compare propellant powders using a propellant: stabiliser
ratio to compare organic gunshot residue to unred powder and to determine the extent to
which cartridges in a box could be associated.
In a different application, Hopper and McCord (2005) used capillary zone electrophoresis to
analyse inorganic ions in smokeless powders. IC was used as a complementary technique.
They analysed intact powders, residues from burning and residues from pipe bombs. They
concluded that in general, differences in relative and overall ionic concentration can be useful
in distinguishing between individual powders and between smokeless powders and inorganic
mixtures.
McCord and co-scientists have also researched the application of gradient reversed phase LC
for the analysis and comparison of smokeless powders using a UV detector (Wissinger and
McCord, 2002) and an MS detector (Mathis and McCord, 2004).
In one of the largest studies of smokeless powders, Rankin and Cottle (2004) combined HPLC
with a diode array detector (UV) and GC/MS to analyse over 300 samples. By application of
multivariate statistics they reported that for double base powders, the combination of NG, DPA
and 2,4 DNT concentrations was highly discriminating, and for single base powders, the ratio
of 2,4 DNT and methyl and ethyl centralite was discriminating.
Scherperel et al (2009) report on the use of nanoelectrospray ionisation mass spectrometry
(nESI-MS) for the characterisation of smokeless powders.
Joshi et al (2011) discuss the analysis of the headspace composition of smokeless powders
using SPME sampling and analysis by GC-MS, GC-ECD and IMS. A technique for the eld
detection of smokeless powders using an IMS detector is demonstrated through the study of 65
smokeless powders. Energetic materials and additives, including: diphenylamine, ethyl
centralite, methyl centralite, 2,4-DNT and NG (in the case of double base powder) were all
successfully detected.
Perre et al (2012) report on the application of capillary electrochromatography coupled to UV
and time of ight-mass spectrometry (TOF-MS) for the separation and identication of
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fourteen organic compounds commonly encountered as additives in smokeless powders. The
method shows potential in differentiating brands of smokeless powders.
Even if successful, Kelly and Mothershead (2001) note some potential complications in
identifying a brand, particularly:
manufacturer change of suppliers;
wholesale marketers may switch bulk products (powders may have different
compositions but identical ballistic properties);
cross contamination when a mixture of powders is utilised in an IED;
some products are identical blends of two or more powders; and
post-blast contamination.
Pyrotechnics
[84.1550]
Flash powders
Unreacted ash powder mixtures are relatively straightforward to analyse. Analytical schemes
have been published by Meyers (1978) and Midkiff (1989).
The post-blast residues may contain traces of unreacted powder and also reaction products. In
intact particles, chlorates are readily identied by IR, XRPD and Raman. The metal fuel can be
identied by XRF and/or SEM/EDX. Flash powders generally produce chlorides as the
reaction product. Sodium and potassium chloride are transparent in IR so cannot be used for
identication. XRPD and Raman are suitable, and IC/CE of an aqueous extract can show the
presence of chloride, sodium and/or potassium ions. The metal component is converted to
metal oxide which can be identied by XRPD and analysis by SEM/EDX will give a
qualitative analysis of the elements present.
Phillips (2001) reported that ash powders deagrated both unconned and conned in pipes
producing spherical particulate residues, the composition of which were characteristic of the
composition of the metal fuel. SEM/EDX was utilised for the analysis of the residues. Kosanke
et al (2003, 2006) subsequently reported similar ndings.
Other pyrotechnics
Pyrotechnics contain chemicals for specic effects, one being whistling reworks. Fung (1985)
has reported the use of such mixtures as the explosive component of pipe bombs. IR spectra of
solvent extracts of a white powder revealed compositions of potassium perchlorate and sodium
salicylate in one instance and potassium perchlorate and potassium benzoate in the other.
These mixtures were attributed to whistling reworks, one of which matched a known brand.
Brandsma and De Bruyn (2001) reported on the application of ion chromatography to screen
for oxidisers and use of spot tests, x-ray uorescence and SEM/EDX for conrmation. They
further reported an ion chromatography system for monovalent and divalent cations.
Vermeij et al (2009) examined the morphology and composition of post blast pyrotechnic
residues at different levels of connement. Three different ash powder compositions and a
black powder composition were evaluated, with residues analysed using SEM/EDX and XRD.
Although the level of connement was reported to have a minor effect on the morphology of
the residues, further work was recommended.
Update: 73
84 - 17065
Castro et al (2011) have also reported on the successful analysis of several conscated
reworks samples using Raman, SEM-EDS and FTIR. A comparison of the techniques for the
identication of the core components and also additives is included.
An advantage of IR, Raman and XRPD analysis of inorganic compounds isolated intact
without solvent extraction is that the anion and cation are linked in one compound. However,
in the event that intact particles are not recovered, solvent extractions should be conducted.
One disadvantage of this is that if there are multiple anions and cations eg, on analysis by CE
and IC, the original ion pairings cannot be determined with certainty.
Commercial explosives
[84.1560] To a chemist, dynamite is challenging, since its components range from volatile
organic compounds (EGDN and NG) and non-volatile organic compounds (eg, NC) through to
water-soluble inorganic components (AN, SN) to insoluble components (eg, barium sulphate,
fuels such as nutshells and pulp, and additives such as calcium carbonate (see [84.510]). These
components can be recovered from hand swabs or from post-blast debris by systematic
analysis. Earlier approaches were discussed and illustrated by Beveridge et al (1975) based on
successive solvent extraction and methods based on IR and TLC among others. Developments
over following decades particularly have enhanced analysis and identication of the organic
components by GC and LC with CL and MS detectors (Figure 3, [84.1360][84.1400];
[84.1410]; [84.1440][84.1450]; and [84.1970]).
As noted at [84.500][84.540], AN is a component of slurries, emulsions and blasting agents.
It is also a major component of ammonia dynamites. AN is employed in the noted products
as prills (solidied droplets typically around 1.5 to 2.0 millimetres in diameter) which can
readily be identied as AN from its characteristic infrared spectrum (Zitrin and Tamiri, 2012
Ch 16) and x-ray diffraction pattern. The same methods apply to solid post-blast residues.
There is also a characteristic colour test (orange colour with Nesslers reagent) (Amas and
Yallop, 1966) which can be applied to screen large quantities of residue. In residues recovered
as swabs, AN typically is sought as its constituent ammonium and nitrate ions. The primary
technique is IC complemented by another technique, eg, CE.
In emulsions, the AN, frequently in combination with sodium nitrate, is combined with various
oils and waxes, sensitisers and often aluminium. Analysis of emulsion explosives and their
post-blast residues generally has consisted of extraction with non-polar solvents for oils and
waxes, and with water for the nitrate salts, leaving residual solids. Analysis has been relatively
straightforward, drawing for example on: spot tests; IR; GC/FID; LC/UV; IC; SEM/EDX and
XRPD (Bender et al, 1993; Midkiff and Walters, 1993; Kishi et al, 1995; Lau et al, 1995;
Kumo-oka and Beveridge, 1997; Nakamura et al, 1997; Burns et al, 1998; De Tata et al, 2006;
and Reardon and Proudfoot, 2007). Overall, the papers show that it is possible to recover AN
and hydrocarbons from post-blast debris.
Research has been undertaken demonstrating the potential to distinguish AN samples,
including that of Benson et al (2009a) who describe the characterisation of AN using isotope
ratio mass spectrometry. The widespread use of AN as a fertiliser also makes it a prime
precursor for illegal explosives (National Research Council, Committee on Marketing,
Rendering Inert, and Licensing of Explosive Materials, 1998, Chs 4 and 5). The analysis and
identication of ammonium nitrate in improvised explosive mixtures is addressed at [84.1610].
Military explosives
[84.1570] Military explosives primarily are nitrated organic explosives such as RDX,
TNT, picric acid, PETN and tetryl. Dynamites based on NG and EGDN are too sensitive for
Expert Evidence
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most military applications. Methods of analysis for military explosives are well established;
typical methods involve GC and LC with CL or MS detectors. Bulk quantities can be analysed
by IR and TLC. Commercial and military explosives are designed to be efficient and as such, if
they high order, little, if any at all, will be recovered intact. If a device containing such high
explosives low orders, then intact particles may be recovered for analysis.
Intact particles of explosives such as RDX, TNT, PETN, and tetryl can generally be identied
utilising FTIR (Zitrin and Tamiri, 2012 Ch 16). When analysing post-blast residues, if any are
recovered, then the compounds can be identied by GC and LC connected to an MS or CL
detector. Highly volatile compounds are more suited to analysis by LC as opposed to GC as the
low operating temperature of the LC reduces the likeliness of thermal decomposition of these
labile compounds. TLC methods are also long established and can also be utilised for the
clean-up of extracts (Beveridge et al, 1975; Doyle 2012, Ch 13; Bladek et al, 1998).
Yinon et al (1994) discuss the analysis of high explosives, including: RDX, HMX, MATB,
DATB, TATB and tetryl utilising pyrolysis GC/MS. Molecular ions, decomposition products
and thermal fragmentation pathways are provided.
Yinon (1999) provides an overview of the degradation processes and products of various
explosives. These potential products for TNT, tetryl, RDX and nitrate ester explosives
including NG and PETN, should be considered during the interpretation of results if samples
have been exposed to various environmental conditions eg, water, sunlight, and microorganisms
(eg, in soil).
Basch et al (1986) discuss the recovery and identication of dinitrate and trinitrate esters of
pentaerythritol post explosions involving PETN. Tamiri and Zitrin (2012, Ch 15) provides a
concise discussion and illustration of complex rearrangement products in the MS of PETN.
Dinitrotoluene (DNT) and dinitrobenzene (DNB) have been discussed as two of the main
post-blast residues from TNT (Oxley et al, 2003).
Vogelsanger (2004) discusses the chemical stability, compatibility and shelf life of explosives.
Whilst this paper is written in the context of the storage of bulk explosives and associated
safety, it can be utilised to understand some of the decomposition products of some common
organic high explosives which may be encountered during the interpretation of results.
Lai et al (2010) address the identication of volatile taggants, including cyclohexanone and
DMNB, in plastic explosives (C-4, Semtex, and Detasheet).
The GC instrument section in Appendix A provides further references for the analysis of
organic high explosives using GC/MS.
Improvised explosive mixtures
[84.1580] Yeager (2012, Ch 12) has rigorously described the chemistry, characteristics,
detection and analysis of improvised explosives with accompanying emphasis on safety.
Crippen (2006) has published an extensive compendium of the components of improvised
explosive mixtures to aid rst responders. We note, however, that improvised explosive
mixtures should only be handled, sampled or disposed of by bomb technicians and/or forensic
chemists trained, equipped and aware of the deadly inherent dangers which such mixtures
pose. Further, interpretation of the signicance of chemical precursors lies with forensic
chemists.
The National Research Council, Committee on Marketing, Rendering Inert, and Licensing of
Explosive Materials (1998, 126-132, 147) has discussed and assessed chemicals most likely to
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be used in bomb-making. The categories were chemicals that could themselves be detonated,
precursors (oxidisers and fuels) that could physically be mixed, and chemicals which could be
reacted to produce explosive compounds. Some of these chemicals are discussed below.
Improvised low explosives typically are mechanical mixtures of fuels (eg, carbon-rich fuels
like sugar and metal powders like aluminium) and oxidisers (eg, nitrates, chlorates or
perchlorates) (National Research Council Committee on Marketing, Rendering Inert, and
Licensing of Explosive Materials, 1998, 126-132, 147). The residues can consist of unreacted
chemicals and products of the oxidation / reduction reaction (see Table 3). The samples are
analysed using the same approach as for other samples, including microscopy and subsequent
instrumental analysis (including FTIR, XRPD, Raman, XRF and SEM/EDX) of recovered
particles and solvent extractions.
The organic solvent extract would be analysed for carbonaceous fuels by GC/MS and/or
LC/MS. The aqueous extract is analysed using ion chromatography complemented by CE or
by evaporation and analysis of the solid residue as described previously. Insoluble material
such as metals and metal oxides are analysed by the same methods noted for physically
removed solids. Sulphur may also be identied by IR or by SEM/EDX. Bradley (2005)
discusses a method for the identication of elemental sulphur in explosives and explosive
residues utilising GC/MS.
Examples of analysis of components of improvised explosive mixtures are provided by
Wakeeld et al (2001) (TLC, FTIR, IC, SEM/EDX, CE, spot tests) and Beveridge and Lothian
(2004) (FTIR, IC, SEM/EDX, Polarising microscopy, GC/MS). Hutchinson et al (2007) have
described the application of a portable CE instrument to on-scene identication of inorganic
post-blast residues. Kuila et al (2006) discuss the analysis of a range of improvised low
explosives and their post-blast residues utilising IC and SEM/EDX. Lim et al (2007) have
described a protocol based on Raman spectroscopy and have illustrated its ability to determine
chemical components of explosive mixtures dissolved in water.
[84.1600] Fertiliser based improvised explosives
A major terrorist weapon is the large vehicle bomb also known as a vehicle borne
improvised explosive device (VBIED) (Sachtleben 2012, Ch 10). This device is a vehicle
bearing explosives. During the troubles in Northern Ireland, chloratesugar mixtures were
used; however, fertiliser bombs have become a more commonly used improvised mixture. Two
fertilisers typically used for this purpose are ammonium nitrate and urea nitrate. Chlorate and
perchlorate based devices continue to be used, with an increase observed in different regions
over the past decade (section 84.1630 refers).
Ammonium nitrate based improvised explosives
Improvised explosives made with ammonium nitrate fertiliser have been widely used in illegal
bombings. The Irish Republican Army used mixtures with sugar in large vehicle bombs in both
Ireland and the United Kingdom. Authorities tried to reduce the effectiveness of such mixtures
by mixing the ammonium nitrate with calcium carbonate to reduce its explosive sensitivity
(National Research Council, Committee on Marketing, Rendering Inert, and Licensing of
Explosive Materials, 1998, 103-106).
The analysis of solid post blast residues would be conducted by FTIR, Raman and XRPD.
Aqueous extracts would be analysed by IC and CE for ammonium and nitrate ions.
Phillips et al (2000) and Cullum et al (2000) have described the post-blast scenes and recovery
and analysis of residues from large bombs composed of AN / sugar and calcium ammonium
nitrate / sugar respectively. Brown et al (2004) describes the analysis of AN using SPME and
GC/MS.
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Residual sugar may be sought by derivatising the aqueous extract or its residue on evaporation
and analysing by GC/MS (Beveridge et al, 1983; Nowicki and Pauling, 1988). The presence of
residual sugars may also be indicated by IC (Walker et al, 2001) and by colour tests (eg,
Fehlings solution). Phillips et al (2000) provide excellent details of experimental conditions
both for analysis by IC of ammonium and nitrate ions and of sugars. They also fully describe
an LC/UV method for detection of sugars. The ammonium and nitrate ions were typically
recovered after the large bomb explosions but sucrose was not. Some explosions did yield
glucose.
The fuel oil component of improvised or commercial ANFO may be extracted with a suitable
organic solvent (eg, pentane or dichloromethane) and analysed by GC/FID and/or GC/MS. The
remaining powder would be analysed by FTIR or Raman and XRPD if necessary. Kuila et al
(2007) discuss the use of TLC for the detection of the constituents of the fuel oil used in
ANFO. Post-blast, the fuel oil component may be recovered by an organic solvent
swab/washing from the surface of interest. Alternatively, a charcoal strip can be added to the
packaging of debris and allowed to equilibrate (with or without heating) with the headspace.
The strip can then be removed and extracted with an organic solvent. The AN would be
recovered post-blast through the use of a water swab/wash of the surface of interest. AN is also
partially soluble in acetone.
Additional details in relation to the analysis and identication of ammonium nitrate based
commercial products are provided at [84.1560].
Urea nitrate (UNi) based improvised explosives
Urea nitrate (UNi) is a powerful improvised explosive derived from the fertiliser urea and
nitric acid. It was reportedly used in the World Trade Centre bombing in New York in 1993
and is reportedly used by suicide bombers in Israel (Almog et al, 2007). UNi can be identied
by its IR spectrum, but not in trace amounts.
Israeli scientists have published several papers on the detection and identication of UNi.
These were designed to overcome the tendency of UNi to hydrolyse in hot water to urea and
nitric acid, especially in trace quantities. Almog et al (2005) have described a eld test based
on the formation of a red pigment from the reaction of UNi with
p-dimethylaminocinnamaldehyde (P-DMAC). A similar reaction has been produced with
paradimethylamonobenzaldehyde to produce a yellow dye. The structures of the dyes have
been determined (Lemberger and Almog, 2007). Almog et al (2007) have reported an
analytical method in which UNi was extracted with hot acetone, cleaned up on a chromosorb
G-HP column and analysed by HPLC/MS using atmospheric pressure ionisation. UNi traces
thus recovered were identied by MS. However, under certain conditions, UNi can be formed
during the analytical process from urea nitrate salts and acids or acidic salts (Tamiri and Zitrin
2012, Ch 15 p. 655). Tamiri et al (2009) discuss initial research towards trace characterisation
of UNi post-blast, specically the extraction from solid mixtures to organic solvents using
Crown ethers and analysis by LC/MS. Almog et al (2013) further discuss the successful
analysis of urea nitrate post-blast by GC-MS.
Phillips et al (2000) have described the post-blast scene outcome of a large (545kg) urea nitrate
bomb.
As with other inorganic compounds of explosive signicance, in the event that intact particles
are not recovered and multiple anions and cations are identied in the solvent extract, the
original ion pairings cannot be determined with certainty. This means that if urea and nitrate
ions are detected in an aqueous extract, the conrmed association of these ions cannot be made
ie urea nitrate cannot generally be conclusively identied as the source compound. De Perre et
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al (2012) discuss the need for selective methods for the detection of UNi and AN. The authors
describe a method based on electrospray ionisation time-of-ight mass spectrometry for the
detection of UNi and AN
DePerre and McCord (2011) also discuss a method for the analysis of trace levels of urea
nitrate using liquid chromatography-UV/uorescence. The method detects the presence of the
urea nitrate ion pair, even in the presence of materials containing urea and other interferences.
[84.1630] Inorganic salt improvised mixtures
Inorganic salts typically of potassium and sodium which are oxidisers such as chlorates,
perchlorates, nitrates and permanganates, can be mixed with fuels such as sulphur, sugar and
other inorganic compounds, and powdered metals. The signicance of identifying ions
post-blast in the inorganic extracts needs to be interpreted in conjunction with appropriate
environmental controls collected during the investigation and other analytical results. This is
also of signicance for organic residues, particular with respect to sites suspected to be
contaminated with background levels of organic explosives (such as explosive ranges, quarries
and locations where land mines have been utilised). Understanding potential reaction products
is an important factor in piecing together what the explosive charge may have been. Table 3
shows typical inorganic reaction products for different chemical reactants (Beveridge et al,
1983; Beveridge and Lothian, 2004; and Lang and Boyle, 2008).
Methods listed in the cited literature, Table 3 and [84.1440] [84.1450] are appropriate for
inorganic ions.
Reaction products or unreacted
components
Possible original component
Chloride (Cl
) Chlorate (ClO
3
), perchlorate (ClO
4
)
Chlorate (ClO
3
) Perchlorate (ClO
4
), chlorate (ClO
3
)
Nitrite (NO
2
), nitrate (NO
3
) Nitrate (NO
3
)
Carbonate (CO
3
2
), bicarbonate (HCO
3
) Sucrose (C
12
H
22
O
11
), charcoal, ascorbic
acid
Metal oxide Al, Mg, Zn
Sulphate (SO
4
2
), thiosulphate (S
2
O
3
2
) Sulphur
[84.1640] Nitromethane
Nitromethane is an energetic material which is used as racing car fuel. It is listed as an
explosive on its own and has reportedly been used as an adjunct explosive in ammonium
nitrate improvised explosives. The noted reference short listed it as a likely to be used
explosive precursor chemical (National Research Council, Committee on Marketing,
Rendering Inert, and Licensing of Explosive Materials, 1998, 126-132, 147). Shekhar (2012)
provide a review of the explosive characteristics of nitromethane. Nakamura and Arai (2001)
reported a case involving nitromethane mixed with sawdust. Identication was based on
analysis by GC/MS (electron impact mode) and GC/CL of headspace samples.
[84.1650] Peroxide explosives
The literature with respect to the analysis of peroxide explosives has been reviewed by
Schulte-Ladbeck et al (2006) and further discussed by Yeager (2012) and Doyle (2012). TATP
TABLE 3 Post-blast products of chemical ractants
was rst reported in the forensic literature by Zitrin et al (1983) and by Evans et al (1986).
Tamiri et al (1998) have described evidence in three clandestine laboratories making TATP.
Crowson and Beardah (2001) developed an LC/MS method for trace analysis of HMTD. They
reported that LC separation is preferred to GC separation of thermally labile compounds like
HMTD. They interfaced an LC to a quadrupole MS with an atmospheric pressure chemical
ionisation interface in positive mode and achieved identication of HMTD at levels of
detection comparable to that of other explosives analysed by GC/CL and GC/MS. Widmer et al
(2002) then developed an LC/MS method for trace analysis of TATP. Xu et al (2004b) applied
HPLC/APCI-MS/MS to the analysis of TATP and HMTD and were able to achieve
identication of both peroxides in the same analytical run. The method was successfully
applied to post-blast identication of TATP. Tamiri and Zitrin discuss and illustrate mass
spectra of peroxide explosives (2012, Ch 15 pp 646-648; 657). Doyle (2012, Ch 13
pp 563-566) discuss practical issues in identifying TATP and HMTD, and present data
supporting the view that LC/MS/MS is the optimal technique.
The recovery of TATP is often a challenge due to its tendency to sublime (ie convert directly
from a solid to a gas). Muller et al (2004) addressed detection of TATP after an explosion.
They reported that recovery of TATP in the vapour phase was best achieved with SPME
followed by GC/MS. The authors reported successful use of the method for identication of 54
exhibits of post-blast samples of TATP over a 1 year period. Nakamura and Arai (2001)
reported the successful identication of TATP from post-explosion debris using GC/MS in
electron impact mode. Subsequently, Nakamura et al (2004) published analytical data on the
analysis of HMTD, TATP and a by-product of its synthesis, diacetone diperoxide (DADP) by
Raman and IR spectroscopy and by GC/ECD, GC/MS and HPLC/UV (photodiode array
detector). HMTD was also analysed by GC/CL.
Egan et al (2004) studied the GC/MS analysis of TATP and HMTD. They concluded that the
application of positive chemical ionisation allowed more denitive identication than electron
impact alone. They reported that ammonia was a better reagent gas for TATP while methane
was better for HMTD. Both SPME and evaporation of acetone solutions were useful
preparation techniques for each peroxide.
Buttigieg et al (2003) characterised TATP by nuclear magnetic resonance, Raman and IR. They
subsequently analysed it by IMS and by coupling the IMS to a mass spectrometer were able to
identify the species present in the IMS as TATP from a single peak at an m/z of 223 mass units.
Rasanen et al (2008) discuss the detection of TATP in the gas phase utilising aspiration IMS
and GC/MS. Armitt et al (2008) provide a discussion on the analysis and detection of TATP
and other organic peroxides, including degradation and decomposition products. Cotte-
Rodriguez et al (2008) discuss the in situ detection of peroxide explosives using desorption
electrospray ionisation and desorption atmospheric pressure chemical ionisation. Schulte-
Ladbeck et al (2003) also discuss a method for the recovery and analysis of TATP in the
ambient air.
Oxley et al (2008) discuss a study comparing Raman and infrared spectroscopy for the analysis
of TATP, HMTD and other peroxide-ring structures.
Burks and Hage (2009) present a review in developments in the detection of peroxide-based
explosives through to 2009, including luminescence methods; IR and Raman; MS and IMS;
and electrochemical methods.
Fan et al (2012) present a method for the rapid headspace detection of TATP using planar
solid-phase microextraction coupled to an IMS detector.
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A number of papers have also addressed the characterisation of peroxide explosive samples,
including TATP through the analysis of a range of derivatives, impurities and reaction and
degradation products (Maty et al, 2011; Haroune et al, 2011; Partridge et al, 2010; Fitzgerald
and Bilusich, 2011; Fitzgerald and Bilusich, 2012). These methods can assist with sample
identication, as well as provide indications of synthesis conditions, starting materials and
ultimately source association.
Unlike the peroxide based explosives (such as TATP and HMTD), the analysis and
identication of the hydrogen peroxide organic material mixtures are reliant upon the recovery
and analysis of the individual components of the original mixture. A number of papers discuss
the detection and analysis of hydrogen peroxide in pre- and post-blast samples (Bartick et al,
2001; Eliasson et al, 2007, 2008; Chen et al, 2010; Tarvin et al, 2010; Tarvin et al, 2011).
It follows that existing analytical instruments and methods can be used successfully to analyse
peroxide explosives, both unreacted and post-blast. In the former case, it is prudent not to
handle or store bulk material in a laboratory.
As with all explosives casework, laboratories must decide based on the literature and their own
tests which validated methods and instruments provide the best results under real-world
conditions and which will withstand modern day challenge in court.
Reporting
[84.1700] The scientist draws on a number of resources to assist in interpreting the
signicance of the analytical results. Primary sources are the literature, contacts with
manufacturers and regulatory agencies, conference attendance and professional visits.
Scientists engaged in explosive residue analysis obtain extensive technical information from
experiments on an explosives range by collecting and analysing residues of available
explosives on a variety of typical substrates. The usefulness and limitations of available
methods are also assessed by experimenting in the laboratory by applying traditional and novel
techniques to explosives, to substrates, to substrates plus explosives and nally to
post-explosion debris.
In each analysis performed, an unknown compound is compared to standards of explosive
compounds to determine whether it is an explosive. As discussed, some of the techniques that
are utilised are considered conrmatory while others are presumptive. The distinction between
these two types of tests must be made clear when reporting results.
If an explosive material is detected using a conrmatory technique, then the sample can be said
to contain explosive residues. That is, a compound in the sample has been identied as a
particular explosive.
The analytical results from any individual technique must be considered with reference to the
results from other tests conducted. For example, an XRF spectrum that shows the presence of
chlorine, potassium and aluminium must be considered alongside the CE or IC result for
example indicating the presence of perchlorate and potassium ions. In this example, it could be
reported that potassium and perchlorate ions were detected in the sample, along with
aluminium. These are the residues expected from an explosive mixture comprising potassium
perchlorate and aluminium akes, commonly referred to as ash powder.
In the event of recovering and analysing intact particles if a crystal was analysed by FTIR
and found to be potassium perchlorate, and aluminium akes were identied by XRF, it is
possible to report that an explosive mixture containing potassium perchlorate and aluminium
akes was identied.
If a presumptive test such as an IMS, eg, the Ionscan, returned a positive result that could not
be conrmed, the result should be reported with stated qualications. In this instance, the
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positive presumptive result could be due to a number of reasons including: the amount of
explosive material in the sample was so small that it could not be conrmed; the trace of
explosive present was removed and consumed during the IMS analysis; or the positive result
from the presumptive test was a false positive. These possibilities should be made clear in any
nal report generated. On the other hand, if a presumptive test returns a negative result,
consideration should be given to whether swabs were collected from an appropriate location (ie
containing residues) or the potential that an explosive or chemical compound may be present
that is not detectable by the presumptive test being utilised. Consideration should also be given
to whether any potential compounds may have been masked by other materials present on the
swab or in the solvent extract.
The presence of explosive residues in the environment must also be considered in interpreting
results. Organic explosives are not naturally found in the environment however some
environments may be contaminated with organic explosives (eg, explosive military ranges).
Many inorganic ions that are indicative of an explosive material or a component in an
explosive mixture can be found in the environment. As a result, environmental background
sampling and testing is often required to determine the presence and level of inorganic
compounds in the environment (refer to [84.1790]). Of particular concern is the use of
ammonium nitrate as a fertiliser. This means that ammonium and nitrate ions are often found in
soil. It is therefore imperative that adequate control soil samples are taken and analysed if the
presence of an ammonium nitrate based explosive is suspected. The levels of inorganic ions
found in swabs collected from the environment must be assessed before reaching a conclusion
with respect to the signicance of the presence of inorganic ions in scene samples.
Suitable controls (as discussed at [84.1780]) should also be collected, analysed and reported on
when positive results are being reported. This demonstrates that the surfaces that may have
come into contact with the item (eg, examiner or examination bench) were not a potential
source of contamination.
It must be remembered that not all explosive materials can be detected by all tests. The nal
report produced should clearly state what samples were analysed, techniques utilised,
explosive compounds or residues for which the samples were tested, analytical test results and
their signicance in the context of the investigation.
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QUALITY ASSURANCE
[84.1750] The term quality assurance (QA) encompasses a range of aspects relating to the
way in which scientists perform their examinations and report on their ndings. Accreditation,
standard operation procedures, instrument / method validations and calibrations, training,
OH&S, and the use of appropriate controls and reference materials all form part of a quality
assurance system.
Accreditation
[84.1760] Most forensic laboratories are accredited against internationally recognised
standards by a national organisation, for example the National Association of Testing
Authorities (NATA) in Australia, American Society of Crime Laboratory Directors/Laboratory
Accreditation Board (ASCLD/LAB) in the United States, the United Kingdom Accreditation
Service (UKAS) in the United Kingdom and the Canadian Standards Association in Canada.
ISO/IEC 17025:2005 species the general requirements for the laboratory to perform tests
and/or calibrations, including sampling. The Supplementary Requirements for Accreditation in
the Field of Forensic Science outline requirements specic to laboratories conducting and
reporting on forensic examinations. Accreditation works towards ensuring that laboratories are
operating according to their procedures and to a certain standard, ensuring that customers of
the laboratory receive quality results and opinions. Laboratories have a series of manuals that
outline the quality, occupational health and safety and training requirements for that facility. In
addition, standard operating procedures are generally in place for each examination type
conducted and instrument utilised.
Demonstrating that method performance characteristics meet the requirements of the intended
application is essential in forensic science and is achieved through method/procedure
validation. Various publications are available that provide detailed descriptions of the
performance characteristics that can be evaluated as part of a method validation (NATA, 2012;
NATA, 2009). Performance characteristics of a method include: measurement uncertainty,
accuracy, precision, robustness, ruggedness, linear range and limits of detection. The
performance characteristics evaluated during a validation will depend on the instrument/
procedure and its intended application. Understanding the performance of an instrument/
procedure is vital in determining the signicance of the results. Method validation is an
expectation placed on all forensic laboratories, and indeed any laboratory accredited against
the international standard ISO 17025.
Laboratories perform routine calibrations and checks of instruments and procedures to
demonstrate their performance over time. The frequency of the calibrations/checks will be
dependent on the instrument and procedure.
Challenges to the work of investigators and laboratory scientists can come through reports and
testimony of independent experts. Challenges can deal with methods and procedures,
signicance (foundation of opinion) and contamination issues. If challenges are upheld in court
this may lead to changes in standard procedures and quality manuals to ensure against
repetition.
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Contamination prevention
[84.1770] As mentioned at [84.1050], a fundamental aspect of all forensic examinations,
both in the eld and in the laboratory, is the need to minimise the potential for contamination
to occur. In a post-blast investigation, like any forensic examination, contamination can relate
to any potential evidence type present at trace levels that may be of signicance to the
investigation at hand, eg, ngerprints, DNA, hairs and bres. The key difference in a post-blast
investigation is the need to take additional precautions in relation to trace explosive residues.
Awareness of the dangers of contamination is the rst step towards ensuring that it does not
occur. Investigators and analysts alike must be able to assure a court with documentation that
explosive traces detected in debris could not have originated from contamination during
collection, transportation, analysis or storage. This assurance can only be given by rigid
adherence to standard operating procedures and documentation.
If the investigation results in a trial, one of the rst areas that counsel may examine is the
possibility of explosive traces (unrelated to the investigation at hand) being brought
unintentionally onto the scene by investigators or others.
Samples are collected from persons and items prior to entering a scene or prior to examining
an item for trace explosive residues. It is important to collect the control samples prior to the
person or equipment being exposed to the scene or item under examination. If the controls are
collected after accessing the scene, it becomes difficult to demonstrate whether the person was
contaminated from the scene or whether the person was a source of contamination to the scene.
The samples are collected in the form of a swab, whether it be for analysis on-site utilising a
screening instrument and/or a swab for future analysis in the laboratory. These swabs can be
referred to as pre-entry swabs. All personnel, equipment, apparatus and containers taken on
scene should be swabbed up until a point in the examination phase (either in the scene or the
laboratory) where swabs have been collected for trace explosive residues. All items should not
have been physically associated with any sources of explosives eg, bomb squad personnel
and equipment.
Swabs can be tested by portable detection equipment in order to provide a real time response
to those entering a scene. If a positive result is returned from a person, they should change
their protective clothing and re-test their clothing. In the case of equipment, items can be
cleaned down with appropriate solvents and re-tested until a negative result is returned. In the
case of consumables, these should be discarded, replaced and re-tested. Operators should be
aware of any limitations of the portable detection equipment being utilised particularly with
respect to the range of explosives that can be detected by the equipment. Working explosive
detection dogs can also be used for screening personnel and equipment. The same cautions
apply as with instruments.
Note: the logistics and practicality of collecting pre-entry swabs of all members, equipment
and items entering a primary post-blast scene often do not allow for such swabs to be collected
(eg, re-ghting and search and rescue operations are paramount and often occurring before
the arrival of the forensic scientist). In the likely event that pre-entry swabs are not collected,
consideration needs to be turned to potential sources of contamination under the circumstances
at hand (eg, entry to scene by a bomb technician prior to the collection of samples for
explosive residues analysis). Once considered, these issues can be addressed by the scientist as
to their potential impact on the scene and samples. It is often the case that the potential sources
of contamination would not have come in contact with the surfaces/items being swabbed/
sampled for explosive residues, hence can be excluded as potential sources of contamination.
The situation is less forgiving in the event of secondary scenes, whereby identifying explosive
traces at a secondary scene can often imply association with the primary scene. In this
situation, it is critical that pre-entry swabs are collected from personnel and equipment entering
secondary scenes where trace explosive residues are of interest.
QUALITY ASSURANCE [84.1770]
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The steps outlined above provide an example of precautions that can be taken, however each
case will present its own individual circumstances on which appropriate procedures will need
to be implemented.
In the case of a bomb technician who enters the scene to conduct an initial sweep, whether the
individual dons clean protective clothing or not, consideration should be given to the collection
of pre-entry swabs. Analysis of the swabs will identify the types of explosives the individual
was contaminated with, which may often be different to the explosive of interest in the case at
hand and will ultimately assist with the overall interpretation of the results. Upon exiting the
scene, the bomb technician must also document any contact with surfaces so that this
information can be used by forensic chemists in interpreting the signicance of positive results
for explosives residues.
Quality control procedures used at the United Kingdom Forensic Explosives Laboratory have
been detailed by Crowson et al (2001), Crowson et al (2007), Beardah et al (2007) and
Crowson and Cawthorne (2012). Beveridge (2012) contains several chapters (authored by
Doyle (Ch 13), Murray (Ch 18), Broome and Todd (Ch 6) and Strobel (Ch 5)) which discuss
contamination and its prevention.
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Control samples
[84.1780] As discussed at [84.1770], the key mechanism to demonstrate that contamination
has not occurred is the collection of control samples (eg, pre-entry swabs). Surfaces from
which control samples are collected will be dependent on the situation at hand. As mentioned
earlier, control samples should be collected from all surfaces that may come into contact with
a surface of interest with respect to trace explosive residues. For example, when examining a
post-blast scene, control samples can be collected from the protective clothing of those
entering the scene and their equipment.
In the laboratory context, Oxley et al (2003) have studied the spillage potential and retention
potential of several commonly encountered explosives. TNT, PETN, RDX, HMX and TATP in
powdered form showed similar spillage and adhesion to glass but plasticised forms of PETN
and RDX showed little potential. Such studies indicate the need for controls.
Controls can be collected from the protective clothing of the examiner, their equipment, the
examination bench and any other surface that the item being examined or the examiner may
come into contact with during the examination. These controls do not necessarily need to be
examined, but should be examined in the event of a positive result. In the event of a positive
result from a control, the type of explosive should be compared to that identied in the scene
samples. If the explosive type is the same, then it may not be possible to exclude the
person/equipment as being a source of contamination to the scene.
[84.1790] Environmental/background controls
Another type of control is environmental or background controls. These controls can be
collected pre-blast (eg, in the event that high risk areas / potential targets have been identied)
or post-blast from surfaces in the surrounding area, but outside of the inner blast site. It is also
a very important step to collect any samples/chemicals from the scene which could interfere
with analysis of residues from the explosion, eg, soil or dry chemical re extinguisher. Such
controls assist the forensic chemist in determining the signicance of any positive results that
may be obtained from scene samples. This is particularly important when inorganic compounds
of potential explosive signicance are identied as it is more likely that these may be naturally
present in the environment compared to organic explosives such as TNT or RDX. To aid
interpretation, several studies have been conducted and published. In most of the studies the
methods used are IC, CE and SEM/EDX. Unlike case work, one method was often considered
to be sufficient for the studies.
Examples include Crowson et al (1996) [London various sites]; Mount and Miller (2001)
[US 3 cities (IC)]; Walker et al (2001) [UK urban and rural (IC)]; Sykes and Salt (2004)
[UK urban and rural (IC, SEM/EDX)]; Cullum et al (2004) [UK various (IC)]; Kuila et al
(2006) [India (IC, SEM/EDX)] and Lahoda et al (2008) [US 28 cities (IC, CE)].
Reference to the environmental studies cited above shows the necessity for caution in
interpreting the signicance of nding such reaction products on exhibits from a post-blast
scene or on persons or property. The cited studies, other local studies and control samples from
the environment of the explosion greatly assist in the interpretation process.
[84.1800] Matrix/substrate controls
Controls can also include swabs/extractions from materials of the same or similar
substrate/matrix as that being examined for trace explosive residues. This also assists in
determining the signicance of any positive results, particularly in the event of inorganic
compounds. These controls demonstrate whether the compound may have been inherent in the
matrix of the surface being analysed. An example of this would be the swabbing or extraction
QUALITY ASSURANCE [84.1800]
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of a piece of clothing from a victim. If a positive result was obtained for high levels of nitrate,
it needs to be determined whether the nitrate originated from the fabric, in particular the dyes,
or whether it was foreign to the clothing.
Reference samples
[84.1810] It is frequently necessary to purchase samples for comparison purposes. Any
recognisable container material (be it a car, a stereo or a suitcase) and/or recognisable parts of
an IED (such as wires, electronic parts, adhesive tapes etc) can provide an immediate lead for
the investigators. Acquisition of a duplicate item for comparison and identication purposes
can help to advance the investigation on several fronts.
Reference samples of various explosives may also be obtained for comparison.
Since such reference samples may provide the foundation for expert opinion, consideration
should be given as to whether these are regarded as exhibits and treated accordingly or as
internal database samples for casework reference.
Analytical and quality control samples
[84.1820] In order to demonstrate the performance of a technique or instrument, quality
control or analytical standards are routinely analysed. Such standards assist in demonstrating
the performance of the instrument with respect to its ability to detect the components of
interest. In addition, system blanks are analysed in order to demonstrate that no carry over
from the previously measured or analysed sample has occurred. This is often conducted with
analytical techniques such as GC, LC, IC and CE.
Expert Evidence
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CASE STUDY FORENSIC CHEMISTRY IN A
COMPLEX PROSECUTION BASED ON
CIRCUMSTANTIAL EVIDENCE
[84.1900] R v Reyat (1993) 80 CCC (3d) 210; 25 CR (4th) 125n (SCC)
Introduction
[84.1910] On June 25 1985, a suitcase from a Canadian Pacic Airlines ight from
Vancouver to Tokyo exploded at Narita International Airport, Japan, shortly after the aircraft
landed. The suitcase was being transferred to an Air India ight bound for Bangkok. Two
baggage handlers were killed and two were seriously injured.
The investigation took several years to complete. The evidence ultimately led to the arrest of
the suspected bomb maker and his extradition from the United Kingdom to Canada to stand
trial for manslaughter and explosives offences. The evidence was largely circumstantial.
This case study focuses on the role of forensic chemistry in the investigation and illustrates
many of the materials, besides explosives, which have to be dealt with by forensic laboratories
in major explosives incidents.
Jurisdiction
[84.1920] Canada assumed jurisdiction for the criminal investigation, on the basis that an
act committed in Canada caused deaths in Japan.
Response teams
[84.1930] Task forces were immediately established in Japan and Canada, and
information ows were established via diplomatic channels and by face-to-face meetings.
Police liaison officers attached to foreign embassies performed a key communications role.
Within a few weeks of the explosion, Japanese investigators from the National Police Agency
and Chiba Prefecture visited Canada to update the Royal Canadian Mounted Police (RCMP)
task force on early progress in the investigation; a forensic chemist experienced in post-blast
analysis and a bomb squad officer attended the briengs as consultants to the RCMP task
force.
Canadian teams which subsequently visited Japan consisted of one or two investigators, a
forensic chemist and a police liaison officer with diplomatic status. Later in the investigation,
the head of the prosecution team also visited Japan in order to view all of the evidence held
there and to conduct preliminary interviews with potential witnesses.
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The scene
[84.1940] Immediately after the explosion, the scene the baggage transfer area at Narita
airport was secured and processed by Japanese scenes of crime personnel. It was gridded,
documented, photographed, sketched and charted. The collection team consisted of a collector,
a recorder and a retainer. Forensic chemists attended the scene as advisors.
Over 1600 individual items were recovered, and 152 bags of sweepings were subsequently
screened and searched over a three-week period to yield many more exhibits.
Forensic chemistry
[84.1950] The forensic chemistry contribution to the investigation followed the following
seven steps (Jardine, 2012 (Ch 20)
pre-lab;
forensic examinations;
initial forensic opinions to investigators;
consultation with prosecution;
organisation of testimony; and
testimony as expert witness.
1. Pre-lab
[84.1960] Damage at the scene was completely consistent with detonation of a high
explosive in a metal container, which Japanese forensic scientists quickly identied as a Sanyo
stereo tuner, model FMT 611K.
Water pipes had broken and ooded the scene, and two types of dry chemical re extinguisher
had added ammonium and sodium ions to the scene. Both events complicated residue analysis,
since many explosive residues are water soluble and many explosives formulations contain
ammonium and sodium nitrate.
Canadian scientist/investigator teams visited the scene, discussed the formulations of Canadian
explosives, and presented videos of test explosions and residue samples. All exhibits were
examined in order to identify and negotiate release of material for use as reference standards
for a search of the suspects residence and for comparison to material subsequently seized.
Relevant exhibits were requested through diplomatic channels by way of Notes Verbale. As the
investigation evolved, this process was repeated several times.
2. Forensic examinations
[84.1970] Japanese forensic scientists examined material from the scene in order to
reconstruct the device and identify the explosive. Standards of tuners, timers etc were
purchased in Canada based on the information received and were sent to Japan for further
comparison.
Canadian scientists concentrated on comparison of material from the scene to material seized
from the residence and workplace of the suspect. Every trace of material in every bag was
minutely examined with a microscope to assess its potential signicance. A team approach was
Expert Evidence
84 - 21052
used for analysis. The explosives industry was consulted about sourcing dynamite found in
possession of the suspect. Communication with post-blast explosive experts, investigators and
Japanese counterparts was continuous.
Analytical protocols were adjusted to deal with contamination of the scene by dry chemical re
extinguishers.
Residue of single base smokeless powder and fragments from an ether can were identied
early in the investigation. However, test explosions with smokeless powder and ether using
simulated tuners conrmed the conclusion from fragmentation and damage that the primary
explosive was a high explosive.
The high explosive was not identied until some ve years after the explosion. Dynamite
traces were identied on clothing exhibits, including victims clothing. This was achieved by a
modied clean-up procedure followed by analysis using the selective TEA detector. The
methods were GC/TEA conrmed by HPLC/TEA and GC/MS. Older methods such as
TLC, IR and GC/ECD were completely ineffective because contamination prevented detection
of the trace quantities of residual explosive: Beveridge (1993).
Physical evidence
Laboratory investigation of explosions typically involves much more than identication of
chemical residues. The most important physical evidence found at the scene and subsequently
associated with the suspect is listed below along with the analytical methods.
(1) Stereo tuner (Sanyo model FMT 611 K)
metal fragments : MIC, SEM/EDX
wire fragments : MIC, SEM/EDX (metal)
MIC, IR (insulation)
paper from manual : MIC
styrofoam packing : MIC, IR
cardboard (box) : MIC
(examination of stencils and
printing by Documents
Section)
adhesive tapes : MIC, IR, PGC;
SEM/EDX (pigments)
(2) Electronic timer (car alarm clock, 12 volts)
circuit board : MIC, IR
integrated circuit : MIC
wires : MIC, SEM/EDX (metal)
MIC, IR (insulation)
crystal oscillator : MIC, SEM/EDX (metal)
CASE STUDY FORENSIC CHEMISTRY IN A COMPLEX PROSECUTION BASED ON
CIRCUMSTANTIAL EVIDENCE [84.1970]
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MIC, IR (plastic components)
(3) Electronic relay (6 volts)
armature : MIC
wires : MIC
plastic spool : MIC, IR
adhesive tapes : MIC, IR
(4) Battery (12 volt lantern battery)
electrodes : MIC
casing : MIC, SEM/EDX (metal)
MIC, IR (coatings)
cell material : MIC, IR (cardboard, tar)
cell core : MIC, IR, SEM/EDX
(5) Ether can fragments : MIC, SEM/EDX (metal)
MIC, IR (coating)
(6) Detonator fragments (victims
body)
: MIC, SEM/EDX
(7) Explosives
Smokeless powder (victims
clothing)
: MIC, IR,TLC
Dynamite residue (clothing) : MIC, extraction, clean-up,
GC/TEA, HPLC/TEA,
GC/MS, SEM/EDX
Dynamite (suspects home) : MIC, extraction, GC/TEA,
IR, TLC, SEM/EDX
The tuner proved to be very signicant, since a suspect had purchased the same model a few
weeks prior to the explosion and was unable to account for it. Differences in paint,
composition and construction distinguished Japanese production from Korean. A Japanese
production run of over 2000 tuners was narrowed to the suspect purchasing one of the very
few tuners in the world (only ve) that could have housed the bomb in the opinion of the
judge. This was achieved by recovery of a small blackened piece of cardboard bearing a single
letter (M) which a document examiner was able to compare positively to a hand written
stencil which had been placed onto a limited number of tuner cardboard boxes at the Canadian
distribution centre. Wire comparison indicated that the tuner electronics had been removed
leaving only the control knob wires inside the metal casing. Recovery of traces of the
operations manual supported recency of purchase.
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Another valuable piece of physical evidence which survived the explosion was green adhesive
tape from the tuner cardboard box which was indistinguishable from green tape found in the
suspects home on another box. Attempts to purchase a standard for comparison showed that it
was not a readily available item.
3. Initial forensic opinions to investigators
[84.1980] Results of comparisons and initial forensic opinions were immediately relayed
to the investigators leading to follow-ups in Canada and Japan, further exhibit submissions and
further consultations. This inuenced the direction of the investigation by supporting or not
supporting on-going theories.
4. Forensic reports to investigators
[84.1990] Over 35 forensic chemistry reports were issued. Copies were sent by the
investigators to the prosecution and thence to the defence as required by provisions for full
disclosure.
Affidavits were produced for the extradition process through which the accused was returned
from the United Kingdom to Canada to face trial.
5. Consultation with prosecution
[84.2000] Initial consultations dealt with weight of evidence in the context of charging
questions, eg, the signicance of positive comparisons between exhibits seized from the
suspect and from the scene. Canadian and Japanese forensic ndings were correlated.
6. Organisation of testimony
[84.2010] One aspect of trial preparation which was particularly helpful involved
consolidating many different reports issued by the same examiner into a 51 page report.
Exhibits were listed in the sequence in which they were to be entered in evidence in chief:
tuner, timer, relay etc. The consolidated report included all forensic examinations and tests
conducted and fully detailed all measurements and opinions. Photographs and videotapes of
test explosions were also included. A copy was given to the defence to aid in following the
testimony and organising cross-examination.
Commercial products purchased for use as standards for comparison to material recovered
from the scene of the explosion and from the suspect, the examination of which formed the
foundation of an opinion, were entered as exhibits.
Keeping track of exhibits and analytical data was greatly assisted by having:
(1) a separate le for each exhibit; and
(2) summary les containing photocopies of all pertinent spectra and chromatograms for
each type of material.
7. Testimony as expert witness
[84.2020] The consolidated report, the summary les, and specic exhibit les were on
hand during testimony. By both Crown and defence following the consolidated report, it was
relatively easy to keep track of the many exhibits and examinations (Jardine, 2012 Ch 20).
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Evidence-in-chief
Evidence-in-chief followed the consolidated report.
The sequence was:
(1) observations at the scene;
(2) the results and forensic opinions of the examination of circa 100 of the thousands of
exhibits examined; and
(3) presentation of 68 photographs and six videotapes of tests (reasons, conclusions, and
residues).
One aspect of evidence-in-chief was to negate, by video taped test explosions and presentation
of damaged material, some conclusions expressed by a defence expert in an affidavit to the
extradition hearing in the United Kingdom that the explosion had been caused by a large
charge of a low explosive.
Cross examination
Defence counsel referred to the consolidated report throughout cross-examination, which
assisted everyone in following the testimony.
Trial
[84.2030] Many police and forensic witnesses from Canada and Japan testied in the nine
month trial.
It was proved that, in the month preceding the explosion, the accused purchased, acquired,
possessed or had access to the following nine items which were consistent with those used to
make the bomb that exploded at Narita airport:
(1) tuner;
(2) timer;
(3) relay;
(4) battery;
(5) ether can;
(6) single base smokeless powder;
(7) detonators;
(8) dynamite; and
(9) adhesive tapes.
Verdict
[84.2040] The trial was in the Supreme Court of British Columbia by judge alone. The
case against the accused was primarily based on circumstantial evidence. The judge drew upon
an Australian case to clarify the issues: Martin v Osborne (1936) 55 CLR 367 (HCA), a
prosecution under the Transport Regulation Act 1933 (Vic).
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In dealing with the physical evidence, Paris J wrote:
The combination of all the above circumstances disclosed by the physical evidence is
sufficient to satisfy me beyond a reasonable doubt of Reyats participation in the fabrication
of the bomb. None of the individual components of the bomb is tied to him uniquely,
although the tuner is nearly so. But their combination in the bomb is unique, and the
evidence demonstrates that during the period shortly before when the bomb must have been
fabricated Reyat obtained and was in possession of that unique combination of exactly
corresponding materials. According to the common course of human affairs that unique
combination of circumstances could not be fortuitous. The only reasonable inference is that
Reyat was involved in the fabrication of the bomb. The contrary cannot reasonably be
supposed.
Mr Reyat was convicted of manslaughter and sentenced to ten years in prison over and above
the three years spent in custody during extradition proceedings, trial preparation and the trial
itself. The verdict and sentence were upheld on appeal.
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CASE STUDY THE BALI BOMBINGS
(12 OCTOBER 2002)
[84.2080] The forensic response to the three bombings that occurred on the Indonesian
island of Bali on 12 October 2002 is utilised in this section as a case study to demonstrate the
requirement for a multi-disciplined approach to a post-blast investigation and also highlight
some of the challenges that scientists may encounter. The joint Bali bombing investigation and
victim identication process is known as Operation ALLIANCE, of which the forensic
response played a major role in its success.
The incident
[84.2090] Around 11.00pm on a busy Saturday night (12 October 2002) in the main
tourist area of Kuta on the Indonesian island of Bali, three explosive devices detonated within
minutes of each other. These bombings resulted in the death of 202 people and the injury of
more than 200 others. The rst explosion was a TNT based device concealed in a suicide vest
that was detonated inside Paddys Bar. Within moments of the rst explosion, a second larger
vehicle borne device, consisting of a chlorate, aluminium and sulphur mixture, was initiated
outside the Sari Club (across the road from Paddys Bar). A third device (containing TNT)
detonated approximately 10 km away, in the Denpasar suburb of Renon, on a roadside
approximately 100m from the boundary fence of the United States of America Consulate. This
third device was a relatively small improvised explosive device (IED) causing only slight
injury to one person. The forensic response to the third device is not discussed in depth in this
case study; however, a key development in the forensic response was the recovery of mobile
phone components which resulted in the identication of the mobile phone (including make
and model). This was the rst indication to the examiners and investigators that the devices
could have been initiated by mobile phones.
The response
[84.2100] At the time of the bombings, two Australian Federal Police (AFP) Forensic
Officers were travelling to Jakarta to deliver a workshop on major incident crime scene
management. The members were redirected to Bali, where they arrived on 13 October. This
small Australian presence grew relatively quickly as the AFP Commissioner met with the head
of the Indonesian National Police (INP) in Bali and signed an agreement to form a joint
Australian-Indonesian Police investigation and intelligence team. Investigators and forensic
officers from Australia (including: ve crime scene examiners, three post-blast chemists, two
ngerprint experts, one biologist and two bomb technicians) commenced deployment to Bali
on 15 October. Resources were sourced not only from the AFP, but from all Australian State
and Territory police jurisdictions. Experts rotated through the deployments on a 14-day cycle,
which continued for approximately six months. The forensic team also grew to include
logistics and exhibit officers, odontologists, pathologists, and additional biologists and
ngerprint experts to conduct the massive Disaster Victim Identication (DVI) process.
Representatives from numerous international law enforcement agencies also joined the joint
investigation, of which the AFP became the lead with respect to international assistance.
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The INP had jurisdiction for the investigation of the incident, and the international agencies
were there to support. A command centre was established at a local hotel, from which the AFP
investigation, intelligence, forensic and DVI teams operated. All responses were coordinated
from this central location. A clear command structure was established with a Forensic and DVI
Commander assigned to oversee the Australian/International forensic response. Team leaders
were assigned to the Forensic Response and the DVI teams. The Forensic and DVI
Commander reported twice daily to the Australian Investigation Commander and as signicant
advances occurred. Regular reporting was also occurring between the INP and AFP
investigation teams. Investigators from up to 10 countries joined the INP and AFP in the
investigation.
The scenes
[84.2110] Despite the Australian teams being off-shore, the scenes were examined
utilising the key principles of post-blast scene examination. Decisions were obviously made
based on the environment and conditions of the scene. The best part of the forensic
examination of the two main post-blast scenes continued for approximately seven days.
Following this, the scenes were attended to examine specic areas as required.
As with most post-blast scene examinations, the examination of the two main scenes could not
commence until the res had been extinguished and all victims had been rescued and the
deceased recovered. Due to the extreme res that followed the initial blasts in both Paddys
Bar and the Sari Club, the structural integrity of the buildings also had to be determined before
the examiners could conduct a full examination. Each of these priority tasks had a potential
impact on the recovery of forensic evidence and needed to be considered by the scientists
when conducting their examination ie:
1. res destroyed potential evidence, either by consuming items such as explosive
residues or burning/distorting items (eg, primary fragmentation) beyond recognition;
2. re ghting efforts (combined with a broken water main under the road which lled
the crater outside the Sari Club) may have washed evidence away, including explosive
residues, in particular water-soluble compounds such as nitrates and chlorates; and
3. the rescue and recovery phase and the DVI process (which was conducted in tandem
with the scene examination) may have resulted in the movement/potential destruction
of evidence.
Another factor that may have affected the recovery and identication of explosive residues was
the humidity in the environment on the island.
Paddys Bar
[84.2120] Paddys Bar was a two-storey building accommodating a popular bar/nightclub.
This is where the rst device was detonated on the evening of 12 October 2002.
[84.2130] Scene interpretation
The re that resulted from the initial explosion had burnt the majority of the structure, in
particular the upper oor which was completely burnt out. The apparent seat of the blast was
identied due to localised damage to the lower oor, including minor fragment and blast
damage to furniture and body spatter and connective tissue on the ceiling towards the rear of
the bar. The extent of the localised damage indicated that the actual explosion had not been a
large explosion and that the main explosive charge was relatively small (ie less than 10 kg).
Expert Evidence
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The absence of a crater indicated that the device was not placed on the ground, hence was
elevated at the time of detonation. Trajectory assisted in estimating that the device was
80120 cm above the ground at time of detonation.
Post-mortem Examination
The body parts of a young male were recovered from the Paddys Bar scene and examined at
the local mortuary. The body parts consisted of a head with associated neck and back skin aps
and a portion of upper left shoulder. Two legs, left and right, were present and were amputated
in the upper thigh region. Physical evidence was recovered from a number of the wound tracts
present on the body parts (see Physical Evidence)).
The under surface of the chin exhibited considerable disruption, which continued upwards onto
both cheeks. Triad-type injuries were noted on much of the skin surface. Blackening of the
skin margins was observed. The directionality of the wound tracts indicated an upward
trajectory of the fragmentation and blast.
The lower legs both exhibited triad-type injuries, large tunnelling injuries and skin blackening
on both upper calf regions. Small puncture injuries on the heel regions were also noted. The
front surface of the legs exhibited puncture injuries on the upper surface of the feet and a large
tunnelling injury at the level of the right knee. The directionality of these wound tracts
indicated a downwards trajectory of the fragment and blast.
[84.2140] Physical evidence
Limited physical evidence was recovered as a result of the scene examination inside Paddys
Bar; however, the few items that were recovered contributed signicantly towards ascertaining
what happened. During the search, small sections of tartan fragment were recovered (each no
bigger than a few cm in length). Due to the damage to the fabric, including shredding into
small fragments and torn/singed edges, it was apparent that the fabric had been in contact or
close proximity to the device at time of detonation. The distribution was centered in one corner
of the bar indicating that it was not uniformly surrounding the main charge. This fabric was
subsequently compared to bres recovered during autopsy from wound tracks on body parts of
the suspected suicide bomber, ultimately linking the fabric to the suspected suicide bomber.
In addition to the fabric, fragments of blast-affected metal (each approximately 4 x 4 cm in
size) were recovered inside the bar and also recovered from the victims and deceased. There
appeared to be blood and skin in some of the folds of the metal, suggesting that they were
travelling fast enough to pass through people. Some were embedded in ttings and furniture,
which was consistent with relatively high velocities. The distribution of the recovered
fragments was relatively wide (ie to most parts of the room) which indicated that the initial
distribution of the fragments may have been centered in/around the explosive charge. Analysis
of the metal fragments utilising x-ray uorescence spectroscopy (XRF) revealed that they
consisted of 100 per cent iron, with an outer protective layer of aluminium (~96 per cent) and
zinc (~6 per cent). It was later revealed that these metal fragments had originated from the
same source and had been added to the device worn by the suicide bomber to increase fatalities
and injuries in the club.
Fragments of grey plastic were recovered during the autopsy of some body parts. These were
very small indicating that they had been near the device at time of detonation, possibly serving
as the container for the device. Later analysis and comparison of these fragments with grey
polypropylene pipes (detailed during the confession by one of the bombers) revealed that the
plastic was physically and chemically similar to the plastic of the end caps of the reference
pipes purchased, but not the body of the pipe.
A battery clip (indicative of a battery serving as the power source) and black insulated mono
core copper wire (possibly originating from detonator lead wires) with apparent explosive
damage and bres attached were also recovered. TNT was identied on the wire.
CASE STUDY THE BALI BOMBINGS (12 OCTOBER 2002) [84.2140]
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[84.2150] Explosive residue analysis
Despite the odds appearing to be against the recovery of trace explosive residues (eg, re, re
ghting, humidity and the large rescue effort), a considered and meticulous approach to scene
examination resulted in the identication of the components utilised in the main explosive
charge. Swabs for analysis were collected from surfaces above ground level (including from
the ceiling above the suspected seat of explosion) and from fragments that were recovered
from behind a metal barrier that was surrounding a concrete pillar in the club. These swabs and
fragments had been protected in part from human traffic, re and re ghting efforts.
Initial analysis was conducted in the temporary laboratory (see [84.2250]) utilising an IMS
detector. Indications of TNT were reported on the copper wire, sections of the fabric and also
from swabs collected from the head of the suspected suicide bomber. These results were
reported to investigators the same day of collection. The samples were subsequently prioritised
for analysis back in the central laboratory in Canberra, Australia. The swabs were treated as
exhibits from the time of collection and their continuity maintained. The results for TNT were
conrmed utilising ion mobility spectrometry (IMS), gas chromatographychemiluminescence
(GC/CL) and gas chromatographymass spectrometry with negative chemical ionisation
(GC/nci-MS) within two weeks of collection. Positive results for TNT were obtained on only
ve of the hundreds of samples analysed in relation to the Paddys Bar explosion.
[84.2160] Device reconstruction
Based on the interpretation of the scene, the recovered evidence and laboratory analyses the
following device reconstruction was possible:
1. Initiation device: battery (power source) and copper wires
2. Explosive: TNT, approximately <10 kg
3. Container: grey plastic and tartan fabric
4. Metal fragments added as shrapnel
[84.2170] Identication material
Connective tissue and spatter marks were visible on the ceiling above where the device was
believed to have been detonated. Samples were collected for DNA analysis to identify people
sitting around a table (area of interest) and possibly interview those people (if alive). The
results demonstrated that the material had originated from one individual which led to the
initial suspicion of a suicide bomber. The DNA prole from the spatter was compared to the
DNA prole from two lower legs and a head being examined in the morgue. The DNA proles
from the spatter, limbs and head matched. The DNA prole was compared to a database in
order to seek the persons parents and conrm his/her identify.
No ngerprints or DNA were recovered from post-blast fragments recovered from the scene.
Sari Club
[84.2180] The Sari Club was a single storey building accommodating a popular
bar/nightclub. The large vehicle borne device exploded outside of this club following the
detonation of the rst device inside Paddys Bar across the road.
[84.2190] Scene interpretation
Whilst a re had burnt the majority of the Sari Club (in part due to the highly ammable
materials, including a thatched palm leaf roof) and the vehicles out the front were signicantly
damaged, the seat of the blast was identied by the large crater on the roadside. Pieces of metal
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were recovered that had originated from a vehicle that appeared to have been close to or
containing the device at time of initiation. Due to the size (approximately 34 metres wide and
0.51.0 metres deep) and location of the crater and the signicantly damaged vehicle parts, the
device was identied as probably being a large vehicle borne device. The damage in close
proximity to the crater indicated a possible high explosive; however, the longer range damage,
crater and subsequent re did not. Further investigations and analyses were required.
Post-mortem Examination
A large number of body parts were recovered from the Sari Club scene and examined at the
local mortuary. The majority of the human remains exhibited evidence of incineration and
advanced decomposition. Many of the body parts consisted of combinations of soft tissue,
muscle and bone fragments. Large sheets of skin, amputated lower and upper limbs and large
joints (hip, knee and shoulder) were recovered. Long bone shafts were often broken in the
mid-shaft region. Feet and lower legs frequently exhibited thermal damage.
The body parts were described, photographed and DNA samples were taken, when the remains
were considered viable, as part of the DVI process (see Identication Material).
[84.2200] Physical evidence
The Sari Club scene examination involved the massive crater and its surrounds. Surrounding
the crater were vehicles and twisted bits of metal. The metal and vehicles were examined to
determine their approximate proximity to the device at time of initiation. A chassis rail that
appeared to have been in close proximity to the device was examined for chassis and engine
numbers. These numbers had been led away; however, serial number restoration procedures
were employed by the INP to recover the chassis number. In addition, and more clearly, a
routine vehicle inspection number (a DPR number Denpasar number for passenger-carrying
vehicles) had been stamped on the chassis rail and had not been led down. This number was
the breakthrough for the INP in tracing the vehicle back to the responsible terrorists (Royds et
al, 2005). No other primary fragmentation was recovered during the search. This is most likely
due to the re destroying fragments and fragments being washed away during the re
ghting/burst water main.
[84.2210] Explosive residue analysis
Swabs for explosive residue analysis were collected from cracks in the bitumen around the
crater and from street signs, light posts, building roofs and gutters surrounding the blast site.
The areas above ground were targeted as these areas would have been exposed less to the
effects of the re, re ghting response and the heavy throughput of people during the rescue
and recovery phase. Samples of water were also collected from the water in the crater in case
any remaining residues had dissolved in this medium.
Of the swabs analysed in country, no positive results were obtained. Despite this, the solvent
swabs were sent back to Canberra for analysis. Prioritised samples were independently
analysed by two additional laboratories. Due to the size of the crater, it was believed that an
improvised explosive mixture had been utilised, as it is generally not likely that the required
amount of high explosive (to produce such a crater size) would be utilised primarily due to
availability. Laboratory analysis resulted in the identication of chlorate ions in six of the
hundreds of samples analysed in relation to the Sari Club bombing. The presence of chlorate
was conrmed in water extractions utilising both ion chromatography (IC) and capillary
electrophoresis (CE) techniques. Chlorate was conrmed on swabs/extracts collected from in
and around the crater and elevated surfaces of lamp posts. The early recovery and preservation
of the samples allowed this relatively reactive ion to be recovered and identied. Elevated
levels of chloride and potassium ions were also identied on the swabs. Chlorate and chloride
were not identied in the temporary laboratory in Indonesia as the IMS technique can not
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detect chlorates, combined with the fact that it was only present on a very small proportion of
the swabs. Scanning electron microscopy/energy dispersive x-ray detection (SEM/EDX) was
also utilised to identify the presence of chloride and potassium on a number of metal street
signs.
In order to determine the signicance of the identication of chlorate and elevated levels of
chloride ions, swabs were collected from surfaces in adjacent streets to determine whether
chlorate and chloride were common to the environment, and if so, at what concentration/level.
Chlorate was not identied in the surrounding environment and only trace levels of chloride
were detected, thus assisting the chemists in determining whether the chlorate and chloride
were foreign to the environment ie could have originated from the main explosive charge.
[84.2220] Device reconstruction
As no primary fragmentation was recovered (except for the vehicle parts), the device
reconstruction based on scene examination and laboratory analysis consisted of:
1. Initiation device: unknown
2. Explosive: chlorate based improvised mixture
3. Container: vehicle
[84.2230] Identication material
The identication of the suicide bomber in relation to the Sari Club bombing was made
utilising DNA from recovered body parts at the scene. These parts were collected as part of the
DVI process, which highlights the importance of the DVI process in also potentially
identifying suicide bombers.
Secondary scenes
[84.2240] As the police investigation progressed, vehicles and premises of interest were
identied. The post-blast scene examiners and chemists were tasked with processing over 25
secondary scenes over the next 6 months. Approximately four months after the blasts, a team
of scientists were called to an address. Like all the others, the premises were clean and did not
show any visible signs of device construction or explosive manufacturing. Despite this, the
same protocols of wearing protective clothing and collecting control samples from all members
entering were conducted. Royds et al (2005) refer to the successful processing of this particular
address. It was here that two pieces of evidence that were vital in connecting the premises to
the bombings were recovered. This evidence included: two particles of explosive mixture (each
less than 1 mm in diameter) recovered by the examiner through the vacuuming of the oor.
These particles consisted of potassium chlorate, aluminium and sulphur and were only
recovered after days of searching the collected debris under a microscope. The potassium
chlorate was conrmed utilising Fourier transform infrared spectroscopy (FTIR), and the
aluminium and sulphur conrmed utilising SEM/EDX and XRF. PETN, TNT, and tetryl were
conrmed in solvent extractions from the oor vacummings and also solvent swabs from
surfaces in the premises. These were conrmed utilising GC/CL and GC/nci-MS. Chlorate and
chloride ions were also detected in these samples utilising CE.
The second piece of evidence was the development of a footprint using ninhydrin of one of the
bombers on a newspaper in the house, hence linking the bomber to the premises.
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Other aspects
[84.2250] Another aspect to the post-blast investigation that was occurring in Australia
during the initial stages was the collection of clothing of victims and witnesses who were
returning to Australia. The clothing was collected from people at airports and hospitals for
explosive residue analysis in the central laboratory in Canberra, Australia. TNT was detected
on the clothing from six people before samples were collected from the primary scene for
forensic analysis. The timely preliminary results were quickly fed back to the investigators in
country.
In response to the bombings, two forensic chemists were deployed to Bali to work as part of
the post-blast examination team. Whilst the chemists assisted with scene examinations and
collected samples for explosive residue analysis, the major successes of the chemists were in
relation to the analysis of samples in a temporary laboratory that was established in a local
hotel room in close proximity to the investigation forward command post. The laboratory was
utilised for approximately three months to analyse samples from both the primary and
secondary scenes. A microscope, a range of chemical colour tests, and portable IMS and IR
equipment were utilised for the analysis of samples.
Prior to utilising the laboratory for examining items, the room was cleaned and control samples
were taken from the various surfaces in the room (including: tiled oor, benches, chairs,
phones and light switches). These samples were analysed utilising an IMS that was operating
in the room and solvent swabs were also collected for future laboratory analysis. Members
entering the room were required to don protective clothing at the front door and collect a
control sample from themselves prior to commencing examinations.
Portable instruments were utilised to screen and prioritise the approximately 2000 exhibits that
were submitted to the AFPs central laboratory in Canberra, Australia. High priority samples
were also analysed by two independent laboratories (one in Australia and one overseas). Due
to the effective prioritisation of samples utilising the temporary laboratory in Bali,
conrmatory results from the central laboratory in Australia became available within two
weeks of the bombing. For completeness, the full examination of all the exhibits took over ve
months, with two scientists conducting the analysis, interpretation and reporting.
Legal outcomes
[84.2260] A number of Indonesians were convicted for their parts in the bombings. Some
have been executed.
Summary
[84.2270] Royds et al (2005) provide a descriptive overview of the actual events of
12 October. The key facets are described below and have been derived from a combination of
information from confessions from the accused and the results from the forensic investigation:
1. Paddys Bar
a) main explosive charge TNT
b) initiating explosive detonator
c) size of charge approximately 1 to 10 kg
d) container 5 lengths of PVC pipe, 50 mm diameter, sewn into a tartan lined
black vest
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84 - 22057
e) position between 80-120 cm above the oor at the back of the Bar
f) shrapnel tiny fragments of metal
g) initiation command: suicide bomber
2. Sari Club
a) main explosive charge improvised mixture of potassium chlorate
(~900 kg), aluminium (~150 kg) and sulphur (~75 kg)
b) initiating explosive TNT (~25 kg) (booster) + PETN (detonating cord)
c) size of charge approximately 1 tonne; however believed to have low
ordered
d) container 12 four-drawer plastic ling cabinets (containing main explosive
charge) connected by detonating cord (PETN) in the back of a white
Mitsubishi L300 van
e) position roadside, outside Sari Club
f) initiation command: suicide bomber. There was also evidence of back-up
remote and delay initiation systems
3. United States of America Consulate
a) main explosive charge TNT
b) initiating explosive detonator
c) size of charge approximately 1 kg
d) container unknown
e) position roadside/on gutter, ~100 m from the boundary fence of the United
States of America Consulate
f) initiation remotely by mobile phone
Acknowledgments
[84.2280] The authors wish to acknowledge the efforts of all those who worked tirelessly
on the Bali bombing investigation (2002), in particular the INP and the Australian forensic
scientists and investigators. The authors also wish to thank Dr Alanah Buck and Dr Clive Cook
for their contribution to the Pathology Section at [84.1325].
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APPENDIX A: ANALYTICAL TECHNIQUES FOR
THE ANALYSIS OF EXPLOSIVES
[84.2310] Instruments utilised in laboratories performing explosive residue analysis are
briey discussed in this appendix. Literature references providing further detailed descriptions
of each technique are provided.
The classical non-instrumental methods of analysis are chemical colour tests (spot tests) and
TLC. These, along with IR and XRPD were the principal methods of the 1970s, and remain
effective for the identication of bulk samples (Beveridge et al, 1975). However, the
application and interpretation of the results of TLC analyses and colour tests were among
several issues raised in challenges in the United Kingdom Court of Appeal in the late 1980s
and early 1990s to some convictions in bombings in the United Kingdom attributed to the Irish
Republican Army in the mid-1970s. Several convictions were overturned (Schurr, 1993;
Scaplehorn, 1993) and a judicial enquiry was held (May, 1992). In consequence, explosives
analysis methodology and interpretation was put under a microscope and lessons were learned.
Another review of explosives work was conducted in the 1990s in the United States of
America (USDOJ/OIG Special Report, 1997). This report also resulted in signicant changes
in quality assurance and both laboratories involved in these reviews have long since been
recognised as world leaders.
Several advances in instrumentation applications were made through the 1980s and into the
1990s such as routine application of GC, HPLC, IC, MS and SEM/EDX for the analysis of
explosives. These methods signicantly improved detection limits for the detection and
identication of trace explosive residues (Beveridge, 1992; Yinon and Zitrin, 1993). The turn
of the century (2000) saw a strong focus on the miniaturisation of traditional laboratory-based
analytical techniques to allow for on-site (eld) rapid screening and analysis of samples.
A brief description of each technique is provided, along with references containing in-depth
discussions and information for readers who wish for more detail. Research and development
is on-going in relation to the application and/or development of new techniques for the analysis
of explosives. Whilst some of the research is touched on, this section does not address new and
emerging techniques for the analysis of explosives rather it is limited to published literature
up to early-2013.
Non instrumental techniques Chemical colour tests (spot tests) and
thin layer chromatography
[84.2320] Chemical spot tests or colour tests involve either applying chemical reagents to
samples of explosive or burning them and observing the colour produced. The rst scheme for
the systematic analysis of explosives was based on spot tests (Amas and Yallop, 1966 and
1969). Many of the tests were not specic and most have been replaced by more denitive
instrumental analyses.
The value and limitations of the Griess test for nitrate esters, and other spot tests used in the
Birmingham Six Pub Bombing Case in the United Kingdom have been critiqued (Scaplehorn,
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1993). In particular, although nitroglycerine does give a positive Griess test, the test is not
specic for nitroglycerine whereby other nitrate esters such as nitrocellulose and PETN react
similarly.
If there is sufficient residual material to be examined for explosive residue, colour testing still
can be a useful screening method. If sample size is limited, then destructive tests such as
colour tests are generally not utilised. Indeed colour testing is frequently used for screening at
explosives scenes in Israel (Almog, 2006). Royds et al (2005) provide a summary of some of
the colour tests available for screening explosives.
Thin Layer Chromatography (TLC) involves a solution of explosive or residue being spotted
onto a thin layer of silica gel or alumina on a plate. The plate is placed into a solvent mixture
in a tank. The solvent migrates through the layer carrying the components of the explosive
sample with it. With appropriate solvent selection, components of the sample migrate at
different rates, and can be visualised as coloured spots by exposure to specic chemical
reagents sprayed onto the plate (Doyle 2012, Ch 13 pp. 554-557; McCord et al, 2012, Ch 14
pp. 601-603).
It is standard practice to analyse known explosives on the same plate as unknown samples in
order to compare the retention factor (Rf: the ratio of the distance travelled by the component
to the distance travelled by the solvent front) and the developed colour.
TLC has long been a mainstay of explosive residue analysis (Jenkins and Yallop, 1970; Douse,
1982). It is still a screening technique utilised in some laboratories around the world; however,
it is no longer acceptable as a stand-alone method of analysis (Zitrin, 1986; May, 1992).
Conrmation acceptable to the courts is normally achieved by instrumental analysis such as
GC/MS (described below) (Zitrin, 1986). Sharma (2005) discuss research utilising a range of
techniques, including TLC, for the characterisation and identication of explosives and their
residues.
Quality issues pertaining to TLC, namely: contamination, reference standards, interpretation
and documentation have been described by Doyle (2012, Ch 13 pp. 556-557).
Chromatography
[84.2330] McCord et al (2012 Ch 14) provides a useful discussion on the application of
chromatography for the analysis and identication of organic explosives, including TLC, GC,
HPLC, IC and CE techniques. Each of these techniques (except TLC) involves the injection of
a sample onto a column and the use of the retention time (ie time taken to pass through the
column) to identify the components of interest.
Gas chromatography (GC)
[84.2340] A sample of the mixture to be analysed is injected into the injection port of the
GC. The injection port needs to be hot enough to immediately vaporise the sample. The sample
is then swept onto the head of the column by the mobile gas phase.
Splitless injection mode can be used where the entire sample goes onto the column, or split
mode in which only part of the sample goes onto the column, the remainder being vented to
the atmosphere. Split injections can be used in situations where the sample is too large or
concentrated to run through the column.
The gas mobile phase ows from a source past the injector and carries the injected mixture
through a long capillary column whose inside walls are thinly coated with a waxy stationary
phase. The components of the mixture separate and elute one after another from the end of the
column.
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The movement of mixture components along the column will depend on their volatilities and
interaction with the stationary phase. The stronger the affinity (attraction) the components have
with the particular stationary phase, the more time they will spend on the column and hence
the longer the retention time. This is a major factor controlling the rate of movement of a
substance through a column.
Because volatility is such an important factor in GC, the chromatographic column is contained
in an oven. For very volatile compounds the oven may be operated at 30-40C; for relatively
non-volatile substances, temperatures of 200-350C may be needed. For GC analysis, the
column may be operated at one xed temperature (isothermally) or over a temperature range
(temperature programming).
Detected components are recorded as peaks on a plot (the gas chromatogram). The area of each
peak corresponds to the amount/quantity of the represented component. The time it takes the
components to pass through the column indicates the identity of the component. The time at
which the peak maximum occurs is referred to as the retention time; different compounds have
characteristic retention times which can be used to assist in identication. Components cannot
be identied solely by GC, hence the need for combined techniques such as GC/MS to conrm
the identity of substances.
The analytical column inside the GC oven provides the sample separation. Whilst a wide range
of analytical columns are available (eg, of varying length, width and stationary phase) forensic
laboratories tend to select an analytical column that will suit the range of materials that they
routinely analyse. A common column type may consist of a capillary column, 15 or 30 metres
in length, with a non-polar to medium polarity stationary phase. Selection of a stationary phase
should generally be based on the polarity of the sample. A very general rule is like dissolves
like. Column polarity has the greatest effect on how the column separates the compounds of
interest as the sample interacts with the stationary phase. A polar component (eg, an alcohol
such as ethanol) will tend to stick to a polar stationary phase but not to a non-polar one.
Non-polar compounds such as propane (LPG) will be held more strongly by non-polar
stationary phases.
The inside diameter of the capillary column has an effect on the columns resolving power and
its capacity or concentration range. In general, the larger the inside diameter of the column, the
larger the sample capacity is. However, the larger the inside diameter, the lower the resolution
is and the higher the ow rate necessary to achieve good performance.
The phase or lm thickness will primarily affect the retentive character and the capacity of the
column. Increasing the lm thickness will cause an increase in the retention of the compounds
being analysed. Thick lm columns are primarily used for extremely volatile compounds. The
thicker phases will retain components longer, allowing them to interact longer with the
stationary phase, thereby increasing the separation of closely eluting compounds.
The effect of the column length on a separation becomes less important as column length
increases. Resolution is a function of the square root of the column length. For example if you
want to double the separation between two peaks without changing the stationary phase, inside
diameter, lm thickness or GC conditions, it would take a four-fold increase in the column
length. In general, the longer the column, the better the separation of mixture components.
Detection
[84.2350] The components emerging from the GC column can be monitored by various
detectors, including those described below. Yinon (1999) provides an overview of the theory of
operation of GC/ECD, GC/FID, GC/CL and GC/MS instruments. Tebbett (1992) also provides
a discussion of gas chromatography in forensic science.
APPENDIX A: ANALYTICAL TECHNIQUES FOR THE ANALYSIS OF EXPLOSIVES [84.2350]
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84 - 23053
[84.2360] Flame ionisation detectors (FID)
Components emerging from the GC column are burned continuously in the ame of the FID
after being mixed with hydrogen and air. Ions and electrons formed when emerging organics
burn in the ame are detected electronically. The ow of current is monitored, amplied and
passed to the recording system.
This detector is insensitive to non-combustible gases such as H
2
O, CO
2
, SO
2
and NO
X
. The
ame ionisation detector is a useful general detector for the analysis of most organic samples,
including samples that are contaminated with water and oxides of nitrogen and sulphur. It is
widely used for GC analysis of compounds such as gasoline, but it is not selective for
explosives. As the detector is not specic for explosives, it is often difficult to identify the
presence of explosive compounds in samples containing complex mixtures. As a result,
selective detectors (such as MS) are often preferred. FID was superseded rstly by ECD and
later by CL and MS detectors. However, the increasing market share of slurry and emulsion
explosives, which do not contain nitrated organic compounds, but do contain oils and waxes,
has again required its application to residue analysis since the FID responds to oils and waxes
whereas ECD and TEA do not.
[84.2370] Electron capture detectors (ECD)
In the ECD, radiation from a source such as nickel-63 (Ni63) ionises part of the carrier gas,
producing a standing current in the electrode gap. As components that have signicant
electrophilic substituents (eg, halogens) enter the gap, they capture electrons resulting in a
decrease in the current in the electrode gap. This change in current is amplied and results in
the representation of a peak. The ECD has better sensitivity than the FID for electrophilic
compounds (including organic explosive compounds containing nitro-groups), and very poor
sensitivity for other components, permitting the selective detection of electrophilic components.
The ECD is a valuable back-up for explosive residue identication; however it is important
that the detector is only exposed to very clean samples as it is easily contaminated. In routine
analyses of real world explosive residue samples, ECD largely has been replaced by CL or
MS detectors, however there are some groups that still utilise and research the technique
(Collin et al, 2006; Calderara et al, 2003; Walsh, 2001).
[84.2380] Chemiluminescent detectors (CL)
Chemiluminescent detectors are selective for nitro- and nitroso-compounds and have a
sensitivity similar to the ECD (Douse, 1983; Fine et al, 1984). Nitro- or nitroso-compounds are
broken down by heat to form nitrogen monoxide (NO) by catalytic action. The NO is
converted by reaction with ozone to form excited NO
2
, which emits light in a specic
wavelength range in the infrared spectrum. The detector contains a lter which allows only
light of this narrow wavelength range to pass and produce a signal. Thus, only compounds
with -NO or -NO
2
should respond. Because it is based on light emission, the technique is
referred to as chemiluminescent detection. A commercially available CL detector is the
Thermal Energy Analyser (TEA).
The GC/CL (GC/TEA) combination is a useful screening technique for nitrated organic
explosives due it its selective nature for these types of compounds; however, it does not detect
emulsion explosives, ANFO or peroxide explosives. The TEA detectors selective lack of
response to co-extracted compounds which are not nitrated is its major advantage over the FID
and ECD due to the production of chromatograms with few interfering peaks and at
baselines. This same selectivity can also be considered a disadvantage as it is unable to detect
non-nitrated explosive compounds. A eld portable version of GC/CL is available under the
proprietary name of EGIS.
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[84.2390] Mass spectrometers (MS)
GC/MS used for the identication of explosives has been extensively reviewed by Yinon
(1991). Yinon and Zitrin (1981 and 1993) have described the basic techniques in their two
books on the analysis of explosives. Application of GC/MS to explosive residue analysis has
been further discussed by Zitrin (1986), Tamiri and Zitrin (1986), Tamiri et al (1993), Sigman
et al (2001), Calderara et al (2004), Perr et al (2005), Sharma et al (2005) and Tamiri and
Zitrin 2012, Ch 15.
Yinon (1999) and Tamiri and Zitrin (2012, Ch 15) provide an overview of the identication of
explosives utilising MS. Yinon (1999) also provides an overview of the principles of operation
of the different types of MS detectors, including: magnetic sector; time-of-ight (TOF);
quadrupole; ion trap; and tandem MS/MS. New applications of MS enhancing the detection
and identication of explosives are constantly under development, for example techniques such
as GC/MS/MS offer improved selectivity for the identication of target compounds,
particularly when co-eluting compounds mask the compounds of interest (Yinon, 2003; Perr et
al, 2005; Collin et al, 2009). Desorption electrospray ionization (DESI) is another MS
ionisation technique for the detection and identication of explosives (Sokol et al, 2011).
A summary of the theory of operation of the MS technique is provided here.
As each component of the mixture elutes from the end of the GC column, it appears in the ion
source of the mass spectrometer. The components are normally ionised either by an electron
beam (Electron Ionisation; EI) or by a reagent gas (Chemical Ionisation; CI).
After ions have been formed either by EI or CI, they are examined for mass and abundance by
the analyser part of the mass spectrometer, generally a quadrupole. The quadrupole uses
electric elds to separate ions according to mass-to-charge ratios (m/z). These molecular and
fragment ions compose the mass spectrum.
[NB: An ion of mass (m) having a single positive charge (z = 1) has a mass-to-charge ratio of
m/z = m/1 = m.]
The mass spectrometer scans continuously over a mass range. As the mixture is injected onto
the chromatographic column, repetitive scanning occurs over a preset mass range (eg,
50-500 mass units) at a preset interval (eg, every 0.5 seconds). Thus, one scan follows another
right throughout the chromatogram and hundreds of mass spectra may be recorded in a routine
GC/MS run.
The computer adds up all the ion peaks in each mass spectrum to give a total ion current for
the mass spectrum. These total ion currents are plotted along a x-axis (time for elution) and a
y-axis (amount of total ion current) to give a total ion current chromatogram (TIC) showing the
elution of all the components of a mixture. If reference materials are available, then the TIC
can be examined at a particular retention time and the mass spectrum of the peak of interest
obtained for comparison. An alternative is to conduct extracted ion monitoring (EIM) from the
TIC to highlight the presence or absence of compounds of interest by extracting the known
ions relating to the compound of interest. This results in a chromatogram containing peaks
representing only compounds of interest (if they have been detected).
After obtaining a mass spectrum from an eluting component, the next step is to try to identify
the component either through the skill/experience of the scientist or by comparison to reference
spectra either stored in an existing spectral database or obtained as a result of the analysis of a
reference material.
A library of spectra, such as that published by the National Institute of Standards and
Technology (NIST) assembled from an archive of >80,000 mass spectra, can be utilised to
identify peaks of interest. The computer uses search software to provide a shortlist of the best
matches between the library spectra and the one measured.
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Selected ion monitoring
Selected Ion Monitoring (SIM) is a technique that can signicantly increase the detectable
levels of organic compounds by looking at very specic masses only. This results in
sensitivities that are 100x greater than levels attainable in Full Scan (TIC) mode, where the MS
scans over an entire mass range. The disadvantage of SIM is that the entire mass spectral data
are not available.
When setting up a method for SIM, ions must be chosen for the analytes of interest. The
following may assist:
choose characteristic or unique ions as the molecular ions;
select the most abundant ions;
choose ions that will not be confused with ions from other compounds that may
co-elute; and
sensitivities are greater when fewer ions are selected, however more ions allow for an
increased specicity.
Electron ionisation (EI)
The EI ion source works on the principle of electron ionisation, whereby a heated lament
produces a beam of electrons. The high energy electrons interact with the vaporised sample
molecules eluting from the GC column. The molecules are fragmented into ions characteristic
of the original molecule as a result of this interaction. The ions are measured by the m/z
analyser.
Chemical ionisation (CI)
Chemical Ionisation (CI) uses an inner ionisation source different from that of Electron
Ionisation (EI).
When a reagent gas such as methane or ammonia is introduced into the ion chamber of the
source, it is bombarded with the electron beam, thereby producing reagent gas ions. By
producing a higher source pressure (than EI) in the CI ion chamber, reactions occur between
the neutral analyte and ions of the reagent gas. The reaction can involve a transfer of an
electron, proton, or other charged species.
In Positive CI mode, usually the positive sample ions are detected, eg, MH
+
; in Negative CI
mode, negative ions are detected, eg, M
-
.
Negative CI involves the capture of an electron by an electronegative sample, such as a
halogenated or oxygenated compound, to produce M- ions. A gas is required in the ionisation
source to slow down the fast-moving electrons so that they can be captured.
The fragmentation of the sample molecule utilising CI is at a lower energy and hence more
gentle than direct electron impact. This has the advantage over EI of producing fewer
fragment ions, in a simpler pattern, and usually results in a molecular ion. This permits the
molecular weight of the molecule, and hence its probable identity to be determined. CI is thus
sometimes the favoured method of ionisation for nitrated organic molecules. The ionisation
may be positive or negative; the mode is usually abbreviated as PICI and NICI respectively.
CI spectra are normally simpler than EI spectra as they only contain abundant quasimolecular
ions and few fragment ions. It is advantageous to run both CI and EI spectra on the same
compound to obtain complementary information.
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High performance liquid chromatography (HPLC)
[84.2420] Various scientic literature provide overviews of the analysis of organic
explosives using LC (Minet et al, 2001; Xu et al, 2004a and 2004b; Paull et al, 2004; Mathis
and McCord, 2005b; Gaurav et al, 2007a and 2007b; Oehrle, 2008; Song and Bartness, 2009
and Zitrin and Tamiri, 2012 Ch 15). The eld has also been reviewed in depth by Lloyd
(1991). Yinon (2003) provides a comprehensive overview of the analysis of explosives by
LC/MS, including theory of operation of electrospray ionisation (ESI) and atmospheric
pressure chemical ionisation (APCI).
HPLC: Partition chromatography
[84.2430] The solute (dissolved explosive) is injected onto the analytical column where it
is divided (partitioned) between two immiscible liquid phases, one stationary (the column
packing) and one mobile (pumped through the column). The amount of solute which dissolves
in the two liquid phases depends on the chemical nature of the phases and the solute. If the
nature of the solute is known, the composition and polarity of the phases can be
selected/adjusted to optimise separation.
If the composition of the mobile phase (eluent) remains unchanged throughout the analysis, the
procedure is called isocratic elution. If the composition of the mobile phase is varied, the
procedure is called gradient elution. HPLC is conducted at a xed temperature (usually close
to room temperature).
The separation procedure is called normal phase or reversed phase depending on the
relative polarity of the liquid phases:
(1) Normal phase chromatography: the stationary phase is polar and the mobile phase is
non-polar.
(2) Reversed phase chromatography: the stationary phase is non-polar and the mobile
phase is polar.
Liquid chromatography has two advantages over GC: analysis at a xed low temperature
which minimises thermal decomposition (which is important for energetic compounds), and
the ability to separate high molecular weight compounds which cannot be separated by GC. A
disadvantage is that HPLC typically requires some 20 times more sample and often exhibits
less resolution.
Detectors
[84.2440] Detectors used for HPLC analysis of explosives include: UV, CL (TEA), and
MS.
(1) UV detector
A UV detector detects the reduction of intensity of the UV light as the light is absorbed by the
molecules passing through. A UV detector is quite sensitive, and is effective with analysis of
relatively pure samples. A diode array UV detector also records the UV spectrum which
complements the chromatography retention time data (Paull et al, 2004). The lack of selectivity
can be a problem in residue analysis since the response to co-extracted compounds may
swamp traces of explosive. However, this property does provide a useful means of
monitoring the effectiveness of clean-up procedures.
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The UV detector can also be used to analyse inorganic ions (Bender, 1989; Skelly, 1982).
(2) CL (TEA) detector
The CL detector operates as described previously for GC, except that the mobile phase is
trapped out in a cold trap placed before the detector. Since water would form ice and block
the system, the CL detector cannot be used for aqueous reversed phase systems (Fine et al,
1984). The selectivity of the detector is a signicant advantage over the UV detector for
detection of explosive residues.
(3) MS detector
The use of MS with LC provides a very stable and suitable system for analysis of explosives
residues. Developments in HPLC/MS and HPLC MS/MS technology in the 2000s are making
these techniques methods of choice in laboratories specialising in explosives analysis (Yinon
and Zhao, 2001; Xu et al, 2004a and 2004b).
Ion chromatography (IC)
[84.2500] Ion chromatography is very widely used in protocols for analysis of inorganic
explosives and their residues (Reutter et al, 1983; McCord et al, 1994; Doyle et al, 2000;
Miller et al, 2001; Klassen et al, 2002; Dicinoski et al, 2006; Johns et al, 2008; McCord et al,
2012, Ch 14 pp 604-607). IC is generally used for the analysis of unevaporated aqueous
extracts. An advantage over evaporation techniques is that it detects ions such as ammonium
and chlorate which, if present in only trace quantities, can be lost by the evaporation process.
IC is a variation of liquid chromatography in which molecules are separated on an ion
exchange column. The column packing contains charged groups and the mobile phase contains
oppositely charged species which associate with the column packing. When a sample is passed
through the column, neutral molecules and ions with the same charge as the column packing
pass through uninterrupted, but ions with the opposite charge (the same as the mobile phase)
will associate with the column packing along with ions from the mobile phase. Weakly
associated ions pass through the column more rapidly than strongly associated ions and
separation is thus achieved. As the ions leave the column, they are detected by a conductivity
detector. This detector generates a series of chromatographic peaks corresponding to the
different times in which components of the analyte mixture emerge from the column. The
concentration of the ion is proportional to the response from the detector, and the associated
chromatographic peak area.
Chemically suppressed IC (conductivity detection)
In chemical suppression, a second column removes highly conducting ions from the mobile
phase before it reaches the detector. In the case of anion (negative ion) separation, cations
(positive ions eg, sodium) in the mobile phase are replaced with H+, thereby converting the
mobile phase from a highly conducting solution of base to a weakly conducting solution of
acid. Conversely, separated sample anions (negative ions eg, nitrate) are converted to highly
conducting strong acids which are readily detected by conductivity. That is, optimal conditions
for detection are established by highly conducting sample ions in a weakly conducting mobile
phase. Anions which do not form strong acids by this process are difficult to detect by this
method. The column must be regenerated to remove accumulated ions.
Non-suppressed IC (conductivity detection)
In non-suppressed IC, an eluent of low conductivity is normally used. The background is
higher and hence sensitivity is lower than suppressed IC.
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UV detection
Many inorganic ions absorb in the UV range and thus can be detected. A UV detector is
effective for several ions found in explosives (Skelly, 1982).
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84 - 23059
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Electrophoresis: Capillary electrophoresis (CE)
[84.2510] Capillary electrophoresis is frequently utilised as a complementary technique
for IC. CE involves separating charged species on the basis of ion conductance (movement)
created by an applied electric eld (McCord et al, 1994; Sarazin et al, 2010; Mc Cord et al,
2012, Ch 14, pp 608-614). Tagliaro et al (2008) provide a review of the applications of CE in
forensic science, including for the analysis of explosives. Pumera (2008, 2006) provides an
overview of research in the eld of microchip and conventional CE for analysis of explosives.
Hutchinson et al (2007) discuss the identication of inorganic improvised explosive mixtures
by analysis of post-blast residues using a portable CE. Lewis et al, 2013 also provide a review
on the development of portable CE systems.Capillary zone electrophoresis (CZE), otherwise
referred to as capillary electrophoresis (CE), involves the separation of ions of interest (either
anions such as nitrate and chlorates or cations such as ammonium or potassium) using a
capillary column lled with a buffer solution. The application of a voltage to the column
results in the movement of the ions. This movement is referred to as the electro-osmotic ow
(EOF). The movement results in the separation of the ions. The speed at which an ion will
move through a capillary is determined by its charge, size and the EOF of the system.
Neutral compounds (such as organic explosives) may be separated using a variation of CE
known as Micellar Electrokinetic Chromatography (MEKC), where a surfactant (detergent-like
solution) is added to the buffer to form micelles (spherical arrangement of molecules in an
aqueous solution). Neutral compounds interact with the micelles and a partition is set up
between the buffer and the micelle. Different neutral species will spend different amounts of
time in the micelle and the buffer, resulting in separation.
Detection of analytes after CE separation is usually through the use of a diode array. Other
types of detectors that can be utilised include mass spectrometry, conductivity and
amperemetry.
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84 - 24051
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Spectrometry
[84.2520] Three techniques for explosives analysis that operate based on the principle of
spectrometry are addressed in this section, namely: mass spectrometry, ion mobility
spectrometry and isotope ratio mass spectrometry.
Mass spectrometry (MS)
[84.2530] Refer to [84.1410] for details on mass spectrometers and their application to the
analysis of explosives.
Ion mobility spectrometry (IMS)
[84.2540] IMS is a widely used screening technique for a range of organic explosives and
the inorganic nitrate ion. It is very fast and sensitive, but is prone to contamination by dirty
samples. An object to be screened is swabbed and the swab inserted into the instrument where
it is heated to volatilise any explosive traces. If present, they are carried into a chamber where
they are ionised by a radioactive source and carried into a column where they are separated in
a drift tube under the effect of a weak electrical eld. The ions are separated based on their ion
mass, size and shape and detected in the sequence of their mobility. The principles underlying
the operation of the IMS technique have been reviewed in detail by Ewing et al (2001).
IMS is the most widely used technology for the eld detection of trace levels of explosives and
other contraband materials (Eiceman and Stone, 2004). Keller et al (2006) discuss the
application of IMS for the analysis of post-blast samples. Yinon (1999) also discusses the
application of IMS for the detection of explosives.
IMS analysers can detect and identify trace amounts of up to fty explosives (Ewing et al,
2001); however, only a limited number can be programmed into the detection algorithm at any
given time. Examples of explosives that can be detected include NG, RDX, DNT, PETN, TNT,
HMX, and tetryl, as well as nitrate-based explosives such as ANFO. Whilst IMS is able to
detect these organic explosives, the technique cannot be utilised for the analysis of typical
inorganic oxidiser/fuel type explosive mixtures including chlorate and perchlorate based
mixtures. The technique can be optimised for the detection of other types of explosives, such
as TATP (Moore, 2004); however, this often decreases the sensitivity of the technique to the
other compounds of interest. Various sampling and pre-concentration devices can also be used
for sample collection and preparation (Guerra-Diaz et al, 2010 provide one example).
Isotope ratio mass spectrometry (IRMS)
[84.2550] Isotope ratio mass spectrometers (IRMS) are specialised mass spectrometers
that produce precise and accurate measurements of variations in the natural isotopic abundance
of light stable isotopes. Isotopes are atoms of an element that differ in the number of neutrons
present in their nuclei, ie have different mass numbers. All but 12 elements exist as isotopes.
The isotopes of the following elements may be measured by IRMS: carbon (isotopes:
13
C and
12
C, not
14
C), oxygen (isotopes:
16
O,
17
O, and
18
O), hydrogen (isotopes:
1
H,
2
H, but not
3
H),
nitrogen (isotopes:
14
N and
15
N) and sulphur (isotopes:
32
S,
33
S,
34
S, and
36
S). Chlorine (Cl),
Silicon (Si) and Selenium (Se) isotopes are less frequently analysed.
Two of the main characteristics differentiating IRMS instruments from conventional organic
mass spectrometers previously discussed are:
Update: 73
84 - 25051
1 sample peaks are converted to a representative analyte gas (eg, CO
2
for carbon, N
2
for
nitrogen, CO for oxygen and H
2
for hydrogen) following elution from a GC column
as opposed to passing directly to a MS detector; and
2 they do not scan a mass range for characteristic fragment ions in order to provide
structural information on the sample being analysed (Meier-Augenstein, 1999),
instead they have a magnetic sector eld MS with high sensitivity which collects the
respective ion currents simultaneously in an array of Faraday cups (Hilkert et al,
1999).
Although it is possible to identify the explosive present using the techniques outlined in this
appendix, it is generally not possible to distinguish one source of the same explosive from
another. IRMS shows the potential to be able to distinguish one source of the same explosive
from another due to the use of different starting materials, manufacturing processes, storage
conditions and other factors that may affect the isotope ratios of the compounds. Nissenbaum
(1975); McGuire et al (1995); Wakelin (2000, 2001); Beardah (2002); Lott et al (2002);
Phillips et al (2003); Benson et al (2006); Motzer et al (2006); Pierrini et al (2007); Lock and
Meier-Augstein (2008); Benson et al (2009a and 2009b); Gentile et al (2009); Nic Daeid et al
(2010); Benson et al (2010) and Barnette et al (2011) provide comprehensive summaries of the
forensic applications of IRMS, including for the analysis of explosives.
Expert Evidence
84 - 25052
Spectroscopy
[84.2560] Primary spectroscopic methods utilised for the analysis of organic and
inorganic explosives are infrared and Raman. Additional spectroscopic techniques are utilised
for the elemental analysis of explosives and these are addressed at [84.2590].
Infrared spectroscopy (IR)
[84.2570] IR is an excellent method for the identication of relatively pure components of
explosives and their residues. IR is primarily utilised for the analysis and identication of
intact particles of organic or inorganic explosives. During the analysis of a sample, IR light is
passed through the sample. This light is in the same energy range as molecular vibrations,
hence some of the light is absorbed at specic wavelengths as determined by the arrangement
of atoms in the sample molecules ie the chemical structure of the compound. The result is an
infrared spectrum which can be interpreted and/or compared to spectra of reference materials
stored in a database to identify the compound.
Two types of instrument are in common use, with the older dispersive instruments now
giving way to the faster and more sophisticated Fourier Transform Infrared Spectrometers
(FTIR). During FTIR analysis, a broad band of infrared light is passed through the sample.
Some specic wavelengths of the infrared radiation are absorbed by the chemical bonds of the
substance. The wavelengths of IR radiation absorbed are indicative for a particular chemical
bond and its immediate chemical environment. Infrared spectroscopy is a non-destructive
technique.
The application of IR to explosives and their residues has been reviewed by Beveridge (1992),
Yinon and Zitrin (1993) and Yinon (1999) and illustrated by Chasen and Norwitz (1972) and
Tamiri and Zitrin (2012, Ch 15). Smith (1996) and Banas et al (2009) also are useful references
for the operation of the technique.
Raman spectroscopy
[84.2580] Raman spectroscopy is an instrumental technique that analyses the bonds within
a substance, either organic or inorganic in nature (solid, liquid or gas), to provide information
about its chemical composition. Raman spectroscopy involves illuminating a sample with
intense monochromatic light, and analysing the change in frequency of the scattered light to
give a Raman spectrum of the sample. The particular combination of the bands present in the
Raman spectrum of the unknown sample is used for its identication by means of comparison
with characteristic band patterns of reference materials stored in a database. Raman spectra can
be obtained non-invasively through transparent/translucent barriers such as plastics, glass,
polymer laminates and protective clearcoats on paint. This non-invasive sampling is important
especially in the analysis of sealed, potentially dangerous unknown substances such as those
retrieved from clandestine laboratories. Raman spectroscopy is a non-destructive technique.
Turrel and Corsett (1996) and Smith et al (2001) serve as useful references for the Raman
technique. Pitt et al (2005) discuss advances in the application of new Raman instrumentation,
including Raman-near eld optical systems and Raman-SEM combinations. One of the areas
discussed is the analysis of explosives. Nagli et al (2008) discuss the analysis of explosives,
including UN, TATP, RDX, TNT and PETN, utilising Raman cross-sections. Moore et al
(2009) and Mass et al (2012) discuss the detection of explosives using portable Raman
instruments. Ali et al (2009a and 2009b) discuss the use of confocal Raman microscopy for the
in-situ detection of explosive particles on clothing (including particles of PETN, TNT and
AN). Eliasson et al (2007, 2008) discuss the detection of concealed sugar and hydrogen
Update: 73
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peroxide solutions utilising spatially offset Raman spectroscopy (SORS). Gaft et al (2008)
discuss the use of a Raman system for the eld detection and identication of small amounts of
explosives on surfaces up to distances of 30 metres. Lim et al (2007) have applied Raman
spectroscopy to low explosive chemical mixtures. Journal references discussing other Raman
based techniques include the following: surface-enhanced Raman spectroscopy (SERS)
(Wackerbarth et al, 2010; Chou et al, 2012), and stand-off Raman spectroscopy (Zachhuber et
al, 2011; Moros et al, 2013).
Expert Evidence
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Elemental analysis
[84.2590] Elemental analysis is an important aspect of the analysis of chemical mixtures,
explosive compounds, post-blast residues and a range of related materials. The primary
techniques utilised for the analysis of explosives are based on x-ray spectroscopy.
Scanning electron microscopy/energy dispersive x-ray
spectroscopy (SEM/EDX or SEM/EDS)
[84.2600] A scanning electron microscope (SEM) is a type of microscope that uses an
electron beam rather than visible light (which is used in an optical microscope) to produce
highly resolved, linearly magnied images with large depth of eld. The SEM operates by
focusing a beam of high energy electrons on a sample. The point of focus of this electron beam
is systematically scanned over the sample. The electrons interact with the sample to produce
several kinds of measurable emissions, the most commonly analysed emissions being
secondary electrons (SE), backscattered electrons (BSE), photons (ie light) and x-rays.
The different emission signals are measured by dedicated detectors attached to the SEM. The
x-rays released from the beam-sample interaction are analysed by an energy dispersive
spectrometer (EDS) which is used to identify the elements present in the sample as well as
their relative quantities. The technique is most useful for the analysis of bulk or
particulates/crystals of inorganic explosives. SEM/EDX also permits rapid and sensitive
determination of metal composition. The process is rapid and non-destructive. The
combination of IR with elemental analysis by SEM/EDX permits identication of many
inorganic components of explosives. Goodhew et al (2001) and Goldstein et al (2003) serve as
a good source of information in relation to the theory of operation of SEM/EDX.
Micro x-ray uorescence spectroscopy (XRF)
[84.2610] During the analysis of a sample utilising x-ray uorescence spectroscopy
(XRF), x-rays generated by an x-ray tube are used to excite the sample. The x-rays knock an
electron out of an inner orbital causing an electron from a higher energy orbital to fall back to
a lower energy orbital. Energy is released in the form of an x-ray with a discrete amount of
energy. This x-ray uorescence is indicative of the atom from which it was generated. Thus, by
using XRF an elemental prole of the sample can be obtained. X-ray uorescence
spectroscopy (XRF) can be used to analyse bulk explosives or crystalline/particulate inorganic
explosives. XRF also permits rapid and sensitive determination of metal composition. X-rays
produced by elements with an atomic mass lower than sodium are too weak to be detected.
Thus, elements below sodium cannot be detected in this manner. XRF is a non-destructive
technique. Janssens et al (2001) serves as a useful reference for microscopic x-ray uorescence
analysis.
X-ray powder diffraction (XRPD)
[84.2620] XRPD is a traditional method of analysis for crystalline compounds. It is useful
for the identication of relatively pure substances and has applications both to components of
explosives and to residues (Beveridge et al, 1975; Yinon and Zitrin, 1981). The sample is
ground into a powder and placed in an x-ray beam. The crystals cause the beam to diffract into
characteristic patterns that are related to the structure of the crystal. The patterns can be
compared to extensive libraries of standards to assist with identication.
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Kotrly (2006) provides an overview of the applications of XRD for the analysis of explosives
and post-blast residues.
Expert Evidence
84 - 27052
Portable explosive detection instruments
[84.2630] Signicant advances in the miniaturisation of traditional analytical
instrumentation for use in the eld have been achieved over the last decade. These
achievements have resulted in the delivery of a new capability for use in the transport security,
rst responder, law enforcement and military communities for the onsite detection and analysis
of threat materials. A range of techniques are commercially available and utilised by
laboratories around the world for on-site screening and analysis of items for explosive
residues. Techniques include: ion mobility spectrometry (IMS); gas chromatography coupled
with IMS (GC/IMS); gas chromatography coupled with mass spectrometry (GC/MS); gas
chromatography coupled with a thermal energy analyser detector (GC/TEA); gas
chromatography coupled with a surface acoustic wave detector (GC/SAW); ion chromatography
(IC); CE; FTIR spectroscopy and Raman spectroscopy. Reviews of currently available portable
explosive detection instruments are provided by Hannum and Parmeter (1998), Rhykerd et al
(1999), Theisen et al (2005), and McMahon (2007). Applications are discussed and illustrated
by Benson et al (2012, Ch 17). See also [84.2250]
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