30134551 Investigation of Explosions E Evidence

84Investigation of explosions

by

Alexander D Beveridge BSc, LLB, MBA, PhD, FCIC.

Sarah J Benson BSc PhD

Update: 7384 - 1© 2013 THOMSON REUTERS

Author information

Alexander (Sandy) Beveridge is a consultant forensic chemist and lawyer inVancouver, BC, Canada. He spent over 30 years in the Forensic Science Service ofthe Royal Canadian Mounted Police, heading the Chemistry Sections in the Edmontonand Vancouver Laboratories. He is a graduate of the Universities of Glasgow (BSc,PhD), Alberta (MBA) and British Columbia (LLB). He has held chemistry researchfellowships 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, Taylorand Francis Group, Boca Raton, FL 2012) which reflects his long-term interest in thisfield. He has extensive case work experience in domestic and internationalinvestigations of explosions, has testified many times as an expert witness and enjoyshis more recent legal perspective of the field.

Sarah Benson works with the Forensics portfolio of the Australian Federal Police.Sarah currently holds the title of Coordinator Criminalistics, where she leads andmanages the Chemical Criminalistics, Document Sciences and Firearms Identificationand Armoury Teams. Sarah joined the AFP in January 2000 upon graduation from theUniversity of Technology, Sydney (UTS) with a Bachelor of Science (Honours) inApplied Chemistry – Forensic Science.

Sarah has gained significant experience in the field of forensic investigation ofexplosions, in both the field and laboratory. Sarah’s experience has been drawnthrough deployments to Indonesia and the Philippines to assist local authorities withthe examination of post-blast scenes and the subsequent laboratory support in thesematters. Sarah has also played a key role domestically in Australia in developingguidelines for the examination of secondary scenes in relation to explosive incidents.Sarah also has a keen interest in research and development in the ChemicalCriminalistics field, in particular the field of explosives, which was highlighted throughher PhD thesis titled Introduction of Isotope Ratio Mass Spectrometry (IRMS) for theForensic Analysis of Explosives (through the UTS).

We are delighted to announce that the Panel of Advisers of the National Instituteof Forensic Science awarded the 2010 Best Chapter in a Publication in theForensic Sciences to this Chapter.

EXPERT EVIDENCE

Expert Evidence84 - 2© 2013 THOMSON REUTERS

INTRODUCTION .............................................................................................................. [84.10]EXPLOSIONS ...............................................................................................................................Classification of explosions ............................................................................................... [84.100]

Mechanical .................................................................................................................... [84.110]Nuclear.......................................................................................................................... [84.120]Chemical ....................................................................................................................... [84.130]

Propagation ....................................................................................................................... [84.160]Deflagration................................................................................................................... [84.170]Detonation..................................................................................................................... [84.180]

Order.................................................................................................................................. [84.200]Effects ................................................................................................................................ [84.220]

Pressure........................................................................................................................ [84.230]Fragmentation............................................................................................................... [84.240]Thermal ......................................................................................................................... [84.250]

EXPLOSIVES................................................................................................................................Classification 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 classifications................................................................................................ [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]

TABLE OF CONTENTS


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]

Identification 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 identification 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]Identification 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]

Paddy’s Bar............................................................................................................ [84.2120]Scene interpretation .......................................................................................... [84.2130]Physical evidence ............................................................................................. [84.2140]Explosive residue analysis ................................................................................ [84.2150]Device reconstruction........................................................................................ [84.2160]Identification material ........................................................................................ [84.2170]

Sari Club ................................................................................................................ [84.2180]Scene interpretation .......................................................................................... [84.2190]Physical evidence ............................................................................................. [84.2200]Explosive residue analysis ................................................................................ [84.2210]Device reconstruction........................................................................................ [84.2220]Identification 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 OFEXPLOSIVES........................................................................................................... [84.2310]

Non-instrumental techniques – Chemical colour tests (spot tests) and thin layerchromatography ..................................................................................................... [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 fluorescence spectroscopy (XRF) ........................................................... [84.2610]X-ray powder diffraction (XRPD) ................................................................................ [84.2620]

TABLE OF CONTENTS


Portable explosive detection instruments........................................................................ [84.2630]BIBLIOGRAPHY

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INSTRUMENTS/TECHNIQUES


Instruments/techniquesCE....................................................capillary electrophoresisCI .....................................................chemical ionisationCL....................................................chemiluminescenceECD .................................................electron capture detectorEDX.................................................energy dispersive x-ray spectroscopyEI .....................................................electron impact ionisationFID...................................................flame ionisation detectorFTIR ................................................Fourier transform infrared spectroscopyGC....................................................gas chromatographyHPLC...............................................high performance liquid chromatographyIC .....................................................ion chromatographyIMS..................................................ion mobility spectrometryIR .....................................................infrared spectroscopyMEKC..............................................micellar electrokinetic chromatographyMIC..................................................microscopical examinationMS ...................................................mass spectrometryPGC .................................................pyrolysis gas chromatographyPMDE..............................................pendant mercury dropping electrodeSEM.................................................scanning electron microscopySFC..................................................supercritical fluid chromatographyTEA® ..............................................thermal energy analyser (chemiluminescent detector)TLC..................................................thin layer chromatographyUV ...................................................ultravioletXRPD ..............................................x-ray powder diffraction

ABBREVIATIONS

ExplosivesAN ...................................................ammonium nitrateANFO ..............................................ammonium nitrate / fuel oilBlack powder ..................................potassium nitrate/sulphur/charcoalDADP ..............................................diacetone diperoxideDATB...............................................1,3-diamino-2,4,6-trinitrobenzeneDCDA..............................................dicyanodiamideDNT.................................................dinitrotolueneDPA .................................................diphenylamineEC....................................................ethyl centraliteEGDN..............................................ethylene glycol dinitrateHMTD .............................................hexamethylene triperoxide diamineHMX................................................“high melting explosive”; octahydro-1,3,5,7-tetranitro-1,3,

5,7-tetrazocine; cyclotetramethylene tetranitramineMATB..............................................1-mono-amino-2,4,6-trinitrobenzene; picramide; 2,4,6-

trinitroanilineMC...................................................methyl centraliteMMAN ............................................mono methyl ammonium nitrateNC....................................................nitrocelluloseNG ...................................................nitroglycerine; 1,2,3–propanetriol trinitratePETN ...............................................pentaerythritol tetranitrateRDX.................................................1,3,5–trinitrohexahydro–S–triazine; cyclotrimethylene

trinitramineSemtex .............................................RDX and PETNTATB ...............................................1,3,5-triamino-2,4,6-trinitrobenzeneTATP................................................triacetone triperoxideTNT .................................................2,4,6–trinitrotoluene

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OrganisationsAFP..................................................Australian Federal PoliceASCLD/LAB...................................American Society of Crime Laboratory Directors/

Laboratory Accreditation BoardATF..................................................Alcohol, Tobacco and Firearms; Bureau of Alcohol,

Tobacco, Firearms and Explosives (a branch of the USTreasury 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 PoliceNATA...............................................National Association of Testing AuthoritiesNRIPS..............................................National Research Institute for Police Science (Japan)NFPA ...............................................National Fire Protection Association (United States of

America)RCMP..............................................Royal Canadian Mounted PoliceUKAS ..............................................United Kingdom Accreditation Service

ORGANISATIONS


OtherBLEVE ............................................boiling liquid expanding vapour explosionDVI ..................................................disaster victim identificationIED ..................................................improvised explosive deviceOH&S..............................................occupational health and safetyPBX .................................................polymer bonded explosivesSPME...............................................solid phase micro extractionVBIED.............................................vehicle-borne improvised explosive deviceVOD ................................................velocity of detonation

EXPERT EVIDENCE



INTRODUCTION[84.10] A useful definition of the term “explosion” is provided in the publication NFPA921 (2011, 921-13):

The sudden conversion of potential energy (chemical or mechanical) into kinetic energywith the production of and release of gases under pressure, or the release of gases underpressure. These high pressure gases then do mechanical work such as moving, changing orshattering nearby materials.

An explosion may occur naturally (eg, the eruption of a volcano), accidentally (eg, themechanical 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 improvisedexplosive devices (IED). The effects of the mechanical work will always be observed and mayaid commercial, military or illegal applications. This chapter addresses primarily the illegal useof explosives and the forensic investigation of such events. A systematic approach to theinvestigation of explosions can recover much useful evidence from a post-blast scene. Themost effective investigations of major incidents are often conducted by multi-disciplinaryteams 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, fingerprintexperts and metallurgists.

When an explosion occurs, a series of underlying questions are asked by the investigatingauthorities, 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 thatdirectly assist in providing answers to the aforementioned questions. Overviews are providedon:

(1) the nature and classification of explosions and explosives;

(2) the post-blast investigative process including:

• post-blast scene examination protocols, including recognition and recoveryof pertinent physical and trace evidence at the scene of an explosion;

• scientific disciplines/specialists that may be involved;

• laboratory analysis protocols for recovered items, with an emphasis on theanalysis and identification of explosive residues;


• interpretation and reporting of results; and

(3) case studies highlighting the key phases of a forensic post-blast investigation.

[84.10] EXPERT EVIDENCE



EXPLOSIONSClassification 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 theproperties and classification of common explosives and explosions.

Mechanical

[84.110] A mechanical explosion is often the result of container failure, for example, therupture of a steam boiler under excessive pressure. In the event of a mechanical explosion, nochemical reaction occurs.

A particularly dramatic example of a mechanical explosion is a boiling liquid expandingvapour explosion (BLEVE) in which a liquid under pressure above its boiling point is releasedby the failure of the container and almost instantly vaporises. BLEVEs can be produced fromobjects as small as butane cigarette lighters and aerosol cans to containers as large as railwaytank cars. If the liquid is flammable, then a fire almost invariably results. Mechanicalexplosions are not covered further in this chapter. A useful discussion of the topic may befound in NFPA 921 (2011, Ch 21).

Nuclear

[84.120] Nuclear explosions involve splitting the nucleus of atoms (referred to as“fission”), as occurs in an atomic bomb. Alternatively, nuclear explosions involve thecombination of atomic nuclei (referred to as “fusion”), as occurs in the sun and hydrogenbombs. Nuclear explosions are not covered in this chapter; however, useful discussions ofthese 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 anexplosive compound or a mixture of compounds. These rearrangements produce more stablechemical compounds (primarily gases) through reactions which give off heat (exothermic) anddo work (move things). The reactions are generally oxidation / reduction processes (ie achemical change where one reactant loses electrons (oxidation) and another gains electrons(reduction). Chemical explosions may be initiated by shock, friction, heat and flame. The focusof this chapter will be on the forensic investigation of events resulting from chemicalexplosions.





Propagation of Chemical Explosions

[84.160] Propagation of the chemical reaction proceeds by one of two mechanisms:deflagration or detonation.

Deflagration

[84.170] Deflagration is very rapid burning in which the flame front travels through theunreacted explosive at a speed less than the speed of sound (ie less than 1000 metres persecond). Explosives which typically react by deflagration are called “low” explosives. They arecharacterised by a relatively slow rate of pressure increase (also referred to as velocity ofdetonation (VOD)) and normally have to be confined in order to explode – that is, to releasegases violently into the environment by container rupture.

Detonation

[84.180] Detonation is a chain reaction in which a shock wave travels through theunreacted explosive at very high pressures and temperatures and faster than the speed ofsound. The shockwave compresses and heats the particles of the main charge (eg, ammoniumnitrate/fuel oil (ANFO) mixture) to a temperature above its decomposition temperature. As aresult, the explosive compound or mixture undergoes an exothermic chemical decomposition(ie material is rapidly converted into reaction products and produces heat) just behind the wavefront in the chemical reaction zone. This process accelerates the shockwave due to the largeamounts of heat and gas generated – referred to as the heat of explosion. This raises theinternal pressure which adds to the high pressures at the front of the wave. The pressure andtemperature in the detonation zone can exceed several hundred thousand atmospheres and3000°C (Mohanty, 2012; Akhavan, 2011). Figure 1 illustrates this detonation process.

Figure 1 – Diagram illustrating an “instantaneous” time lapse of the detonationprocess (adapted from Mohanty, 2012)

Explosives which are initiated by detonation are called “high” explosives. High explosives donot need to be confined to explode. When such a solid or liquid explodes, the volume canincrease 10,000 to 15,000 times and the gases can expand between 1500 and 9000 metres persecond (referred to as the VOD). Detonation can be achieved by burning to detonation or by an

EXPLOSIONS [84.180]


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 thanthe velocity of sound, deflagration is said to occur.




Order

[84.200] Explosions may be classified by resultant damage as “low order” or “high order”.If the rate of deflagration reaches between 1000 and 1800 metres per second, the reaction maybe classed as a “low order” detonation. If the rate increases to 5000 metres per second, thedetonation 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 largeobjects being pushed short distances – for example, a fuel/air explosion in a house causeswindow 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 thesurroundings and produces small fragments of material which travel considerable distances athigh velocity.

Fuel/air mixtures, in which the fuel is typically hydrocarbon(s) and the oxidiser is oxygen, canonly 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 isreferred to as “rich”. The proportion of the fuel to air must be in the correct range for theparticular fuel type to result in an explosion. Near the limits, such mixtures produce “loworder” 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 byvolume in air and for acetylene/air the range is approximately 2.5 to 82 per cent by volume inair. With respect to these two fuel types, it would generally be easier to create an explosivemixture utilising acetylene as opposed to gasoline, due to the wide range in which acetylene ispotentially explosive (ie 2.5 to 82 per cent).

Confusingly, the term “low order” is also used to describe a “misfire” or partial detonation ofa high explosive and “high order” can be used to indicate detonation at maximum possiblevelocity.

EXPLOSIONS [84.200]





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 reflection, focusing andshielding of the shockwave and structural fires. The physics of explosions has been describedin 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 ispositive in nature and is referred to as the overpressure (or the positive phase). There is also aless strong “returning” (or negative) phase caused by filling of the partial vacuum produced bythe gases rushing outwards (Mohanty, 2012).

Pressure is measured as force per unit area. There are several different scales. The standard unitis 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 structuresare:

windows broken : 3–7 kPa

concrete walls, unreinforced : 14–20 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 referredto as primary fragments. These primary fragments can produce extensive damage and injuriesand can also generate secondary fragments from surrounding surfaces/objects. Primaryfragments (and sometimes secondary fragments) may bear explosive residues and the damagealone 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 anexplosion.

Shrapnel refers to items or material included in the device construction specifically for thepurpose of causing maximum damage, injuries and/or fatalities. Shrapnel can be in the form ofmetal items inserted into the container (such as nails, bolts, screws) or actually form part of the

EXPLOSIONS [84.240]


device container itself such as a hand grenade. The metal casing of a hand grenade is designedto break apart at the weakest points upon explosion, ultimately generating small pieces ofprimary fragmentation which act as shrapnel.

Thermal

[84.250] The high temperature of an explosion reaction can ignite the surroundings. Thisis particularly true of deflagrating explosives which react at a lower temperature than highexplosives but for a longer time. Detonating explosives can cause a delayed fire by initiatingsmouldering. This frequently occurs with car bombs.

Fire can destroy evidence, but fire suppression can also be a problem not only because manyexplosive residues are water soluble and the saturation with water may wash vital evidenceaway, but also because chemical fire extinguisher powders may contain ions (charged atoms orcompounds) which occur in residues from particular types of explosives. These ions includesodium [Na+], ammonium [NH4

+] and bicarbonate [HCO3-]. Therefore, it is important to

educate fire departments of the need for minimum suppression at explosion scenes and forscientists to be aware of fire suppression methods and chemicals used at the scene.




EXPLOSIVESClassification of Explosives

[84.300] Explosives can be classified using a number of properties eg, rate of reaction,chemical composition, or their end use/application. A common way to classify explosives is bythe rate of reaction – that is as low (generally deflagrating) or high (detonating) explosives.

Low explosives

[84.320] Low explosives burn rapidly when ignited by flame or spark, and if confined, canexplode to rupture and fragment the container (for example, pipe bombs). The reaction fronttypically moves through the unreacted explosive at less than the speed of sound (ie1000 metres/second). Examples are propellant powders (including pistol, rifle and shotgunsmokeless powders, and traditional black gunpowder), improvised chemical mixtures (forexample, chlorate/sugar) and pyrotechnic compositions (for example, fireworks). However,some of these examples, when confined and initiated with a detonator, can react by detonation(Oxley et al, 2001; Bender and Beveridge, 2012).

The low explosives classification also includes dispersed explosive mixtures such as fuel/airand dust/air mixtures which typically deflagrate; that is, there is a definable flame front whichpropagates the explosion.

The effects of the mechanical work from low explosives are pushing rather than shattering ofsurrounding objects/surfaces.

High explosives

[84.330] In high explosives, the reaction front moves through the unreacted explosive atgreater than the speed of sound. High explosives may be subdivided into primary andsecondary explosives.

Primary high explosives

Primary high explosives are extremely sensitive and may be initiated (ie detonated) by heat, aswell as by shock and friction without confinement. Detonation velocities are generally between3500 and 5500 metres per second. The principal commercial use is in detonators. Examples arelead styphnate (lead trinitroresorcinate) and lead azide in commercial detonators and mercuryfulminate and triacetone triperoxide (TATP) in improvised detonators. Primary explosives aregenerally 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 confinement when initiated by shock from aprimary explosive (eg, detonator). Their detonation velocities are generally between 5500 and9000 metres per second. Examples include commercial dynamites, slurries, emulsions,


detonating cords, and military and plastic explosives (Hopler, 2012). Specific explosivecompounds include EGDN, NG, TNT, tetryl, RDX, HMX and PETN.

The detonation of high explosives is characterised by high pressures and a very rapid rate ofpressure rise which shatters the surroundings.

Blasting agents

[84.340] The term “blasting agent” refers to explosives (such as ammonium nitrate / fueloil mixtures (ANFO)) that are utilised for commercial applications such as mining anddemolition. These explosives are commercially manufactured and sold in bulk quantities. Theyare occasionally referred to as “tertiary explosives” because they cannot normally be detonatedwith a detonator and in common applications require detonation with secondary highexplosives which act as boosters (refer to Figure 2).




Initiation of Explosives

[84.370] Commercial and military explosives are initiated by detonators, fuses andboosters. These are discussed in the following sections. Improvised explosive devices maysimilarly be initiated, but more commonly employ improvised initiation systems such as ahomemade detonator containing TATP or HMTD.

The explosive initiation train

[84.380] The explosive initiation train assists in explaining chemical explosions and theclassification of explosives. Figure 2 illustrates a schematic three-step explosive train for anexplosive main charge such as blasting agent.

A primary high explosive in a detonator (eg, lead azide or styphnate) is classically detonatedby flame or a hot wire which then initiates a small quantity of a secondary high explosive alsoinside the detonator (eg, PETN). This in turn initiates a booster typically containing tetryl or amixture of TNT and PETN. The high velocity shock wave of the booster then detonates themain charge (eg, a blasting agent such as an ANFO mixture). A secondary explosive likedynamite 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 anexplosive main charge (eg a blasting agent)

Detonators, Fuses and Boosters

[84.390] Low explosives, such as propellant powders and improvised chemical mixturesconfined in a pipe bomb, are normally initiated by flame from a fuse such as commercial(“safety”) fuse which utilises a burning black powder core. Such fuse is used for blasting andfor model rockets (hobby fuse). Igniter cord is a less common form of fuse and consists of acentral wire covered in a pyrotechnic composition and contained in a plastic jacket. Burnedfuse usually can be recovered from post-blast debris.

Flame can also be produced by mixing certain chemicals whose reaction is so intense thatflames are produced (hypergolic mixtures). These mixtures can be used as silent delaymechanisms whereby the mixing of the chemicals is delayed.

Flame can also be generated electrically by a “squib”. Another source of electrically generatedheat energy is a glowing filament (“hot wire”).

Detonator shells are made from metals such as aluminium, steel or copper. The shell fragmentscan 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 theproperties of the detonator. These wires are referred to as lead or leg wires and are oftenrecovered post-blast. The wires are typically made from copper or tinned copper.

EXPLOSIVES [84.390]


Test explosions to build databases and liaison with industry can greatly aid identification ofdetonator components in post-blast debris. A commonly used primary explosive component islead azide (or less commonly, lead styphnate mixed with lead azide) which may leave acharacteristic 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 residuefrom 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 toinclude 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 wallswith a mixture of the high explosive HMX and aluminium (Al) powder. The tube is oftencolour-coded and may consist of a number of co-extruded layers. It can be initiated by adetonator, detonating cord or high intensity electrical spark provided by proprietary initiatingdevices. When initiated, the HMX/Al mixture generates a shock wave by a dust explosionwhich 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 frompost-blast debris.

Electronic detonators contain an electronic delay circuit housed in the detonator shell incontrast to the traditional pyrotechnic delay element used in non-electric and delay electricdetonators. Electronic detonators are fitted with electrical lead wires. Chemicals in a wiredmetal tube (such as aluminium) are heated by the application of electricity which causes themto react and in turn initiate a primary high explosive (such as lead azide or styphnate). Thisinitiation detonates a charge inside the detonator (usually consisting of a secondary highexplosive 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 delaycircuit to function the detonator and in this respect electronic detonators offer a high degree ofsecurity against illegal use.

Detonators are not usually sufficiently powerful to initiate blasting agents such as ANFO, forthis purpose boosters are used. Boosters may be specifically designed for the purpose (forexample, cast boosters) or may simply be a cartridge of a commercial high explosive. Castboosters 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 systemsoperate in the same manner as commercial ones but may have different specifications andcolour codings.

Illustrations and greater detail on these topics may be found in Thurman (2011).




Chemistry of explosives

[84.400] An understanding of the chemistry of explosives assists in the reconstruction ofevents. Detailed information on explosive compositions, chemistry, structural formulae, etcmay 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 andthe US Army Armament Research and Development Command) (Vols 1 to 10); Akhavan(2011); Thurman (2011) and Beveridge (2012).

Chemical classifications

[84.410] When classified according to chemistry, explosive compounds and chemicalmixtures can be categorised as:

(1) inorganic nitrates containing the nitrate ion [NO3-], for example ammonium nitrate

(NH4NO3);

(2) nitrate esters containing the structure C-O-NO2, for example ethylene glycol dinitrate(EGDN), and nitroglycerine (NG) (principal ingredients of dynamites) andpentaerythritol tetranitrate (PETN);

(3) nitramines containing the structure C-N-NO2, for example cyclotrimethylenetrinitramine (RDX) and tetryl;

(4) nitro–aromatic compounds containing the structure C-NO2, where the carbon is partof a benzene ring, for example 2,4,6 trinitrotoluene (TNT);

(5) nitro–aliphatic compounds containing the structure C-NO2, where the carbon is notpart of a benzene ring, for example nitromethane;

(6) perchlorates and chlorates containing the ClO4- and ClO3

- ions respectively, forexample potassium perchlorate (KClO4);

(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). Thefuel may be a finely powdered metal (for example aluminium or magnesium);sulphur; charcoal; sugar; ascorbic acid (vitamin D) or other organic compound such asdiesel fuel.

Oxygen balance

[84.420] Organic compounds are based on carbon, in which carbon is bonded to some orall of the hydrogen, oxygen and nitrogen. The primary products of combustion are carbondioxide and water. A certain amount of oxygen is required in the formulation of an explosivecompound to convert the carbon and hydrogen (ie fuel elements) to carbon dioxide and waterrespectively. The surplus or deficit of oxygen in an explosive’s formula is expressed as apercentage. The expression “oxygen balance” is used to describe the percentage of oxygen inan explosive’s formula that is required to convert all of the carbon and hydrogen. The chemicalcomposition of the post-blast products will depend on the amount of oxygen present. Aperfectly balanced explosive compound has an oxygen balance of zero. For example, the twoexplosive oils in dynamite, nitroglycerine (NG) and ethylene glycol dinitrate (EGDN), have a

EXPLOSIVES [84.420]


positive oxygen balance, whereas the primary explosive chemicals in military explosives(including 2,4,6 trinitrotoluene (TNT), pentaerythritol tetranitrate (PETN) andcyclotrimethylene trinitramine (RDX)) have a negative oxygen balance. If not enough oxygenis available (ie negative oxygen balance), then items recovered post-blast may exhibitsignificantly more carbon deposits arising from the unconverted carbon.

Chemical reactions

[84.430] In organic explosive compounds (such as NG, PETN, RDX and TNT), thechemical reaction which takes place is internal combustion between oxygen, carbon andhydrogen in the same molecule (compound). The carbon and hydrogen are normally separatedfrom the oxygen by a “buffer” element such as nitrogen. It is essential for intramolecularcombustion 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

C3H5(ONO2)3 → 3CO2 + 2.5H20 + 1.5N2 + 0.25O2

Trinitrotoluene (TNT, aromatic nitrate) – negative oxygen balance

2(C7H5(NO3)2 → 7CO2 + 5H2O + 3N2 + 7C

In explosives mixtures containing inorganic compounds, the reactive oxygen (oxidiser) isusually in one compound and the fuel (most frequently containing carbon and hydrogen) inanother. The efficiency of such explosives depends on whether the correct proportions of theoxidiser and the fuel are utilised and how intimately these are mixed. Examples include blackpowder and ammonium nitrate/fuel oil (Mohanty, 2012). Black powder’s efficiency issomewhat impaired by two of the reaction products being solids (ie K2SO4 and K2CO3) ratherthan just gases.

Black powder

8C + 3S + 10KNO3 → 3K2SO4 + 2K2CO3 + 6CO2

ANFO

3NH4NO3 + “CH2”* → CO2 + 3N2 + 7H2O

* generic fuel oil

(Mohanty, 2012).

Product formulations

[84.460] The principal chemical composition of a range of explosive products (under thesub-headings: propellants, pyrotechnics, commercial, military and improvised explosives) arediscussed in this section. [84.390] refers to detonators, fuses and boosters that can be utilised



+ 5N2

for the initiation of the aforementioned products. Additional details on generic formulations arelisted 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 ina ratio of 75:15:10) has been used for over 2000 years as a propellant, but has long beensuperseded commercially by smokeless powders based on nitrocellulose (NC). Refer to[84.1530] for details on black powder and their substitutes, including composition andidentification. [84.1540] provides details on techniques for the identification of components ofsmokeless powders.

Smokeless powders are manufactured worldwide and are utilised as propellants for rifle andhandgun ammunition. Smokeless powders are relatively easy to purchase in bulk due to theirlegitimate use by sportsmen who reload shells for competitive target shooting and hunting.Smokeless powders are nitrocellulose based and divided into three classes by the chemicalcomposition of their primary energetic ingredient(s):

• single base powder (NC) (widely used in rifle ammunition);

• double base powder (NC and NG) (widely used in handgun and shotgun ammunition);and

• triple base powder (NC, NG and nitroguanidine [HN = C(NH2) NH(NO2)]) ([US]National Research Council, Committee on Smokeless and Black Powder, 1998).Triple base powders are used in large calibre munitions and are rarely if everencountered in IEDs.

In addition to the energetic components, additives are incorporated to control the burn rate andflash characteristics. The additives are incorporated at different stages of the manufacturedepending 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 forseveral stabilisers.

• Plasticisers which assist in making the NC pliable and improve the gelatinisingproperties and hygroscopic properties. Ethyl centralite, phthalates (such as dibutylphthalate) and 2,4-DNT are commonly used plasticisers (Joshi et al, 2011).

• Additives are incorporated into the powder depending on the required combustion rateand formulation. Additives include: flash suppressants (reduce muzzle flash),deterrents and opacifiers (usually added as a surface coating, modulate burn rate ofthe individual grain and enhance the burn reproducibility and efficiency) and dyes(assist in visual identification) (Perre et al, 2012).The surface coating may include: 2,4dinitrotoluene (2,4 DNT), carbon, or potassium sulphate.

Pyrotechnics

[84.480] Pyrotechnic compositions are specifically designed to produce a lot of energywhich is used to produce:

• a flame or glow (ie a matchstick), or

EXPLOSIVES [84.480]


• smoke and light if combined with other volatile substances (ie fireworks), or

• large quantities of gas (eg, firework rockets and bangers) (Akhavan, 2011).

Pyrotechnic materials contain a fuel and an oxidiser, together with required additives toachieve the desired outcome (ie generation of heat, delay, smoke, light and/or noise). Akhavan(2011) describes the different applications and pyrotechnic compositions. Conkling andMocella (2011) present a comprehensive reference on the chemistry of pyrotechnics.

Flash powders

Flash powders are dangerous low explosive mixtures of chlorate oxidiser and aluminium ormagnesium powder. They have military applications as explosive simulators and like anychemical mixture may be used as a pipe bomb filler. Loud bangs and brilliant flashes inpyrotechnic displays usually are produced by flash powders. Klapötke et al (2013) discuss flashcompositions, specifically the sensitivity and explosive power of binary flash compositionscontaining aluminium and (per)chlorate oxidisers.

Other pyrotechnics

Black powder provides the “lift” for aerial pyrotechnic displays and when confined willexplode. 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 identification of pyrotechnic mixtures.

Commercial explosives (including blasting agents, slurries andemulsions)

[84.500] Commercial explosives are relatively safe to use and relatively simple andinexpensive to manufacture. Commercial manufacturers around the world review, modify anddevelop new explosive formulations on an on-going basis to ensure that that the mostcost-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 analysisand identification of commercial explosives. This section provides an overview of a range ofcommercial explosives, including those categorised as blasting agents, slurries and emulsions.

[84.510] Dynamite

Dynamite was developed in the 1860–1870s and formulations have changed little. The name isderived from the Greek word “dynamis” meaning “power”. Dynamites have a long history, buttheir production is falling in the face of rising production of AN based emulsions. The basiccomponents of dynamite are nitroglycerine, inorganic nitrates and carbonaceous fuels. What isconventionally known as “nitroglycerine” in dynamite is actually two compounds: ethyleneglycol dinitrate (EGDN) and nitroglycerine (NG, glycerol trinitrate). The EGDN reduces therisk of freezing (as NG freezes at approximately minus 13°C). Due to its high volatility, EGDNmay be readily detected by instrumental explosive sniffers and dogs. Dynamites which containnitrocellulose are called “gelatins”. Most dynamites are gelatins, and also contain sodiumnitrate (SN) to enhance the oxygen balance. The “ammonia” dynamites contain ammoniumnitrate (AN). Typical fuels are wood pulp, coconut husks and gums. Some dynamites alsocontain inert materials such as barium sulphate which can aid propagation of the explosion inseismic applications. Dynamites are initiated by shock from a detonator.



[84.520] Blasting agents

ANFO is a blasting agent developed in the 1950s and is made from ammonium nitrate and fueloil. Traditionally, bulk slurries and blasting agents are initiated by a booster, which is initiatedby a detonator. In later developments, “cap-sensitive” slurries were produced that could beinitiated with a detonator. These are packaged in plastic containers about the same size assticks of dynamite.

In 2011, 99% of the metric tonnage of industrial explosives sold for consumption in the UnitedStates of America were ammonium nitrate based blasting agents and oxidisers. 71% was usedin 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 the1950s. Typical formulations also incorporate additives including chemical sensitisers (eg,monomethyl ammonium nitrate (MMAN) or EGDN), or physical sensitisers (eg, air bubbles orglass microspheres). Commercial use of slurries has declined in the face of competition fromthe newer water-in-oil emulsion explosives ([84.540]).

[84.540] Emulsions

The newest development in commercial blasting explosives, which occurred in the 1960s and1970s, is emulsion explosives. These are water-in-oil emulsions that consist of an internalphase of a concentrated oxidising salt (typically a solution of ammonium nitrate and sodiumnitrate in water); an external phase of oils, waxes and surfactants; and glass microballoons orgas bubble void sensitisers to help propagate the explosion (Hopler, 2012). Cap-sensitiveemulsions have made very significant inroads into the dynamite market (ie products that can beinitiated utilising a detonator alone).

Military explosives (including plastic explosives)

[84.570] Military explosives are manufactured for use in artillery shells, missile warheadsand demolition charges. Military explosives are stable, ie resistant to impact, shock, andmoisture. They usually need to be capable of being stored for long periods of time withoutsignificant deterioration. All characteristics of military explosives must be completelyunderstood prior to use; including: power (amount of work conducted by the explosivecharge); sensitivity (relative ease to initiate/detonate); brisance (shattering effect);hygroscopicity (absorption of moisture from the air) and toxicity. Military organisations aroundthe world review, modify and develop new explosives on an on-going basis to ensure that thatthe most effective and safe products are deployed for use.

The most common military high explosives are trinitrotoluene (TNT), tetryl, pentaerythritoltetranitrate (PETN), cyclotrimethylene trinitramine (RDX) and cyclotetramethylenetetranitramine (HMX) (Hopler, 2012). “RDX” and “HMX” are British acronyms for “ResearchDepartment Explosive” and “High Melting Explosive” respectively. TNT is used fordemolition and is a component, along with HMX, of the explosive “octol”. PETN is ademolition 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 ofAmerica’s military also uses a product which although called “military dynamite” contains nonitroglycerine. Rather it contains RDX, TNT, lubricating oil and starch. Composition B (anRDX and TNT mix) is also commonly utilised by military organisations in their artilleryrounds and other munitions.

EXPLOSIVES [84.570]


Plastic explosives are formulated with waxes and oils which make them mouldable. Thus theycan be packed to fill an irregular cavity, or can be moulded into a shape which will concentratethe maximum force of the blast onto a specific area (“shaped charges”). Also, such explosivescan readily be disguised.

Polymer bonded explosives (PBX) were originally developed in order to reduce the sensitivityof 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 embeddedin 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 increasingdespite higher production costs compared to melt cast explosives.

Whilst melt cast explosives are commonly employed in low cost, mass-produced munitionssuch as artillery and mortar rounds, PBXs are now used widely in high cost, low throughputmunitions where the relative cost of the warhead is small relative to the overall cost of themissile or munition. (NB. The technique of casting is used for loading explosives intocontainers. The process involves melting the composition (eg, TNT) and pouring it into acontainer and allowing it to solidify (Akhavan, 2011)).

[84.1570] discusses the analysis and identification of military explosives.

Improvised explosives

[84.600] In stark contrast to commercial and military explosives, improvised explosivesgenerally have no legitimate uses and their characteristics tend to be unpredictable (ie withregards sensitivity, power and stability). Terrorists, criminals and enthusiasts employ a range ofchemicals in making improvised explosives that can cause damage, destruction, fatalities,injuries and general fear amongst the population. The reason for choosing a particularexplosive 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/orcharcoal) with a strong oxidiser (eg, ammonium nitrate, sodium or potassium chlorate orpotassium perchlorate) or by synthesis of chemicals to form an explosive product such asorganic 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, andLicensing of Explosive Materials, 1998, 126-132, 147; Yeager, 2012). Peroxide explosives arebeing used increasingly in terrorist attacks, including the London bombings of 2005 (Broomeand Todd, 2012). Their synthesis is relatively straightforward, requiring hydrogen peroxide asa necessary ingredient. There are several peroxide explosives, but the most common aretriacetone triperoxide (TATP) which is synthesised from acetone and hydrogen peroxide, andhexamethylenetriperoxide diamine (HMTD) which is synthesised from hydrogen peroxide andhexamine. Recipes to make improvised explosives of this type are readily available on the



internet. Due to the ready availability of recipes and starting materials, and the limited skillrequired to make improvised explosives, they are of concern to the law enforcementcommunity.

Also of increasing concern are the hydrogen peroxide organic mixtures (sometimes referred toas HPOM or concentrated hydrogen peroxide explosives (CHPX), which can be made bymixing hydrogen peroxide with an organic material such as flour or pepper. Such mixtures arementioned in trial transcripts of the attempted London bombings on 21 July 2005 and havebeen discussed by Broome and Todd (2012) and Yeager (2012). These mixtures vary inappearance and consistency. Once again, due to the availability of materials and the ease ofmanufacture, these mixtures are of concern to law enforcement and other agencies around theworld. As new explosives continue to emerge, scientists undertake research to characterise andevaluate the materials to inform procedures and methods.

Improvised explosives, whether they be oxidiser/fuel mixtures or discrete chemical compoundssuch as TATP, are generally manufactured and employed by criminals, terrorists, or enthusiasts(eg, for experimental or nuisance purposes). [84.1580] discusses the analysis and identificationof improvised explosive mixtures.

EXPLOSIVES [84.600]





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 chargewith a means of initiation. Low explosives must be contained, and containers are often usedwith 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, boththrough the provision of evidence to inform a judicial process or intelligence to direct aninvestigation or prevent the occurrence of future events. Each of the IED components is apotential source of trace chemical, biological and physical evidence which can be related tobomb 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 andchemical mixtures. Metal or plastic pipes are commonly used (“pipe bombs”). Containers forhigh explosives are used for concealment and / or fragmentation and range from baggagethrough to stereos (radios) to vehicles. Bulk explosives, typically improvised explosivemixtures, are most frequently used in vehicles – known as “large vehicle bombs” or“vehicle-borne explosives”.






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 orelectronic timer. These, by a mechanical action or electrical impulse, complete an electricalcircuit from a battery to a detonator (or to another initiation source such as a “hot wire”) inorder 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 thecontainer and then react with an appropriate chemical mixture inside the device to produce aflame. The flame 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, atrip 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 ofpressure change on a barometer or altimeter is another form of physical action which cancomplete a circuit.

Command initiation

[84.760] The bomber can initiate a device by remote control action; for example, by usinga mobile telephone to provide the electrical impulse necessary to complete a circuit and initiatea detonator.

Commercial blasting equipment would also fall into this category. Two systems in common useare the traditional electrical detonator and a non-electrical shock tube system ([84.390]).

IMPROVISED EXPLOSIVE DEVICES [84.760]




PRE-BLAST INVESTIGATION[84.900] Whilst the focus of this chapter is on post-blast investigations, it is important tonote the role of forensic scientists in support of proactive investigations to prevent illegal useof explosives.

During the course of an investigation, investigators may recover images, notes, manuals oractual items such as chemicals or device components. These may also be referred to in phonecalls that have been intercepted by police. Investigators draw upon relevant scientificdisciplines to provide advice to assist in identifying whether potentially illegal activities areunderway (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 ofexplosives?

• 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 ofthe recovery of suspected device components.





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 dolittle more than play “catch up” as the investigation unfolds. Preplanning on the part ofinvestigative agencies largely dictates whether the investigation runs the investigators orvice-versa.

Command and control

[84.960] Good communication, command and control within and between the investigationand forensic teams are vital to the success of a post-blast investigation. A command centre isestablished to coordinate communication and activities of those involved in the investigationand to ensure logistical support. Internal information flow must be clearly established throughteam briefings and interaction with all involved groups. Media protocols must be clearlyestablished and followed – normally through one spokesperson.

Jurisdiction should be established immediately – one person should assume immediate controlof the scene and the investigation (such as a senior investigating officer). This is particularlycritical when more than one agency is involved or in a multi-jurisdictional investigation, forexample, in a suspected aircraft bombing, or when a bomb manufactured in one country blowsup in another ([84.1900] R v Reyat (1993) 80 CCC (3d) 210; 25 CR (4th) 125n), or wheninternational assistance is provided ([84.2080] on the Bali Bombings).





Police criminal investigation

[84.970] The head of the investigation (eg, the senior investigating officer) requires goodinvestigative expertise rather than expertise in bombs and explosives – for which he or shemust rely on a team of specialists. Ideally, there will be a pre-planned strategy in place, forexample, calling upon the assistance of trained response teams comprising post-blast expertsand other scientific experts as required by the circumstances. The success of suchinvestigations relies on the early engagement of the most appropriate specialists. The roles ofsome of these specialists are described in this section.

The purpose of a police investigation is generally to identify, charge and prosecute anoffender/s who had the means, motivation and opportunity to commit the crime. The policeinvestigation seeks answers to the following essential questions (Vermette, 2012 s. 4.2.) andutilises the team of specialists to assist in providing them. The extent to which these questionsare investigated and answered will usually depend on the scale and profile of the incident. Inmajor 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 bombtechnician 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 specific 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]


• 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 identified as a result of the investigation?

The investigative/police team assists with securing the scene, identifying and interviewingwitnesses, assessing the neighbourhood, doing background checks on the victim/target andpursuing leads on suspects; that is, conduct a normal police investigation.




Forensic investigation

[84.980] Many specialist scientific disciplines may contribute to the forensic investigation.The roles of a number of core disciplines are summarised in the following sections. Examplesof 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 onthe scene of an air disaster; Foster (2012, Ch 9) who has described the expertise employed atthe scene of a gas explosion in a building and Strobel (2012, Ch 5) who has described the roleof 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 onthe scale of the incident, available resources and jurisdiction. In addition to the team leader (orcoordinator), team members will include post-blast scene examiners and other scientific andtechnical specialists as required. Scientific and technical specialists may include: forensicchemists; fingerprint 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 smallerjurisdictions, 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 largeincidents, logistic and exhibit management support will also be a consideration.

A detailed overview of the various specialists that may be engaged during an investigation isprovided at [84.1210] – [84.1300]. The roles of the post-blast scene examiner and forensicchemist in the field are outlined in the next section.

Post-blast scene examiner

[84.1000] A post-blast scene examiner performs or oversees the performance of thefollowing 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.



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 portableinstruments;

• ensuring that appropriate samples are submitted to the laboratory for priority analysis;and

• collection of other items of potential significance, eg, metal fragments, fabric, fibres,paint and plastics

As mentioned, one of the valuable roles that a chemist can play at a scene is the on-siteanalysis of items/samples utilising field portable instruments for screening for residues oridentifying recovered chemicals. An additional resource for consideration that falls under thiscategory is the use of explosive detection canines. These are handled by specialist handlers andnot the forensic chemist.

Portable explosive detection instruments offer a number of advantages in the investigation ofexplosive-related incidents. Such instruments enable analyses to be conducted close to apost-blast scene and result in the provision of real-time results to investigators and sceneexaminers. The use of portable instruments at or near the scene can also increase the efficiencyof analyses back at the main laboratory through initial sample screening and prioritisation. Inpost-blast examinations, portable instrumentation can significantly decrease the time in whichpreliminary results are available, particularly if there is significant transportation of exhibitsrequired. For example, the Australian Federal Police (AFP) have used portable instrumentationto provide preliminary results for investigations in Indonesia and the Philippines, wheretransportation of exhibits to the central laboratory in Australia involved over eight hours offlying time. The preliminary results can guide investigations and inform decision making. It isimportant 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 notreplace the need to conduct laboratory based confirmatory analyses to inform the judicialprocess. ([84.2250] highlights this issue utilising the Bali bombings 2002 case study).




Protocols at the scene of an explosion

[84.1050] Scenes relating to post-blast investigations are generally referred to as primaryscenes (where the explosion occurred) and secondary scenes (scenes that are associated withthe primary scene, eg, a mortuary, where the deceased from the blast are being examined; ahospital where the victims are being treated, premises where devices were constructed and/orexplosives made, open areas where experiments/trials were conducted or vehicle/s used fortransport). This section focuses on the examination of primary scenes; however, a briefoverview 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 aprimary or secondary scene (or an analytical facility) must be “demonstrably free ofexplosives” (Murray, 2012 Ch 18). If contamination with explosives occurs – or the possibilityof 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 noweight in a court of law. “Demonstrably free of explosives” is a practical application of qualityassurance: “demonstrably” means tested, found to be negative and documented. Portableanalytical equipment and explosive detection dogs are useful for this purpose. It applies topersonnel, their clothing and footwear, their equipment, and their transportation, etc.Contamination has caused many real problems in investigations and can be the starting pointfor independent experts and counsel.

Paragraphs [84.1770] – [84.1810] discuss procedures for contamination prevention and thedifferent types of control samples that can be collected to assist in demonstrating that surfacesare free of explosives prior to scene entry and/or examination of items. The following sectionsdeal with this issue explicitly and implicitly and it is an essential aspect of training in this field.

Primary scenes

[84.1060] There are general protocols that are considered when conducting a post-blastscene examination. These protocols are outlined by forensic laboratories in their standardprocedures 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 theindividual circumstances of the incident. The key response and examination phases are coveredat [84.1070] – [84.1130].

Emergency response and search and rescue

[84.1070] The first phase of any response to an explosion involves the search and rescueof the injured. The primary role of first responders in this instance is humanitarian and sceneprotection. Their training should emphasise minimal fire suppression, no non-essentialpersonnel on-site and a marked corridor for emergency personnel. Post-blast scene examinerscan brief emergency personnel on key points of scene preservation; however, the rescue ofsurviving victims takes priority. The recovery of the deceased is also a priority with respect tothe identification and reconciliation phases of the DVI process. The DVI process should beconducted 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 briefing to establish the facts, including safety hazards and reportsfrom first responders. The plan is then implemented and work assignments are set. Thepost-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.



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 otherappropriate personnel before others enter. This is known as the “primary sweep”. The purposeof this is to ensure that there are no additional explosive devices, including booby traps, and torender safe any that are located. Structural integrity must also be assessed by qualifiedpersonnel such as structural engineers. Utilities personnel should attend as required to assessgas and electricity safety issues. It is essential to consider and address chemical and biologicalhazards, including toxic, corrosive, flammable or explosive vapours and body fluids.

Scene appreciation phase

[84.1100] The first phase of the scene examination typically involves the classification ofthe post-blast scene as to whether the nature of the explosion is obvious or not (eg, anexplosion at a power station, a work place incident or a terrorist attack). Issues identified arecombined with information from the first responders and witnesses in order to formulate themost efficient and effective course of action. Required resources to achieve the plannedobjectives are also considered during the appreciation phase. Potential physical evidenceobserved at this stage is noted and protected.

Scene assessment phase

[84.1110] The scene must be secured as soon as possible by establishing boundaries andensuring that all non-essential personnel are kept out. The command centre can be kept fullyinformed of developments inside the boundaries via regular briefings and possibly through theuse of specialised video technology. All authorised personnel (ie assisting with the examinationof the scene) entering the scene should be logged in and out. In order to ensure security andpreservation of the scene, the size of the scene must be determined. In order to do this, thefurthest most spread of debris is located and a 50 per cent buffer zone is generally added todetermine the placement of the outer cordon. Depending on the incident, the 50 per cent bufferregion can be searched and cleared of evidence as a priority so that the cordon can bedecreased. This is particularly important if the scene is located in a central business district asit 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, powersources, containers, tapes and wires; however, physical evidence can take many forms.Materials damaged by the explosion are considered for collection and may include metal andplastic fragments, clothing, adhesive tape, cardboard, wrapping paper, timer parts, batteryparts, wires, electronic parts, parts of radios and stereos, other potential containers, scorchedmaterial, and shattered, deposited or penetrated material. Objects such as suitcases, otherbaggage, and furniture are also prime sources of embedded fragments. Traces of explosiveresidues and other forensic evidence are also collected for analysis and identification.

Record, Search and Collect

This aspect of scene examination includes the recording of the overall scene and then thesearching, recording and collection of primary fragmentation according to a pre-determinedsearch pattern. Search patterns typically are spiral, grid, strip or zone depending on the



circumstances, including the size of the scene and available resources. Entry and exit points tothe seat of the blast are established and cleared of any debris. Remaining debris of interestfrom the search areas is recorded and collected. The search areas can finally be swept, with thesweepings collected.

All items/samples collected should be documented, packaged and stored in order to maintainthe integrity of the items. Paragraph [84.1080] addresses quality control measures forconsideration when processing a scene. In general, processes should be adopted in order tominimise 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 andcontainers. Containers should be clean, air-tight and impermeable to vapours ofexplosives 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 beundertaken by anyone who recently has handled, or who habitually handlesexplosives, including explosives ordnance disposal (EOD) or bomb squad officers. Ifcircumstances necessitate that such officers must collect exhibits, then the requirementfor them being “demonstrably free of explosives” by virtue of documentedprecautions and screening is essential to minimise court challenges (refer to[84.1080]).

• Consideration to the preservation of other trace evidence types, including identificationmaterial such as fingerprints and DNA on IED fragments.

Samples of soil and/or other sweepings can also be collected. This debris may be sifted on-siteusing various sizes of screens or removed to a forensic laboratory for searching. When samplesof soil or like material are collected for residue examination, a control sample of the samematerial should be taken from an area remote from likely explosive residue deposition. Thesame applies to surfaces that are swabbed for trace explosive residues.

Fragments travelling at high velocity may penetrate animate and inanimate objects. Human andanimal victims, alive or dead, are sources of physical evidence which should be recovered athospital 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 theuse 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 effectsof positive and negative blast pressure waves, impacts from primary and secondaryfragmentation and effects of heat and fire (Strobel, 2012, Ch 5). The post-blast scene examinerwill interpret the damage to inform an opinion on the type of explosion ie mechanical orchemical. If chemical, the probable type of chemical eg, vapour–air; dust–air or explosivecompound/mixture – may be assessed. The examiner will also try to determine: the use of ahigh or low explosive; approximate size of the main charge; type of container; where thedevice was placed etc. If an explosive was involved, the nature of the damage close to the siteof the explosion plus any evidence of container fragmentation can permit a reasonable estimateof whether a low or high explosive was involved. It is important to establish as soon as



possible what objects were present before the blast and where they were located. This maypermit estimation of the quantity of explosive, location/placement of the device and assistrecognition of foreign material such as device fragments. Sorensen and McGill (2011) presenta review of blast scene damage observables, specifically structural damage to commonly usedbuilding materials, to inform opinions on size, type and position of the charge. Keane andEsper (2009) also provide a discussion on the forensic investigation of blast damage to anumber of buildings in Britain.

Explosive residue collection

The examination phase includes the search and collection of unconsumed explosive materialsand residues. This phase also involves the collection of suitable environmental controls andreference samples (refer to [84.1780] – [84.1810]). Residues may be recovered by swabbingobjects 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 forexamination in the main laboratory.

Samples and swabs for explosive residue analysis are generally collected from close to the seatof explosion. Samples/swabs can also be collected from surfaces that are facing the seat ofexplosion where residues may have been deposited. If there has been a fire, fire fighting effortsand/or a search and rescue operation, these may have affected the survival of residues. In theseinstances, surfaces that are further away and/or above ground level are often a good source ofresidues (refer to [84.2080] on the Bali Bombings case study).

If swabs are collected in the field, they are collected utilising dry swabs or swabs wetted withorganic solvent, inorganic solvent or a mixture of solvents. Depending on the situation and thesurfaces, vacuuming may also be an alternative (eg, victim’s clothing or floors of secondarypremises). Further details in relation to residue collection procedures are provided in[84.1390]. Commercial “Explosive Residue Swab Kits” are also advertised for sale by privateorganisations. Explosive residue traces may also be sought through sampling of the air at theseat 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 recoveringresidues 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 oftrace amounts of explosives exposed to different environmental conditions. This informationcan be used to inform explosive residue sampling and analysis plans and also the interpretationof results. Abdul-Karim et al (2013) report on research to inform decisions on where residuesamples 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 explosiveresidues, identification materials (eg, fingerprints and DNA) and other physical, trace andelectronic 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 ofthe analytical phase, including types of evidence, discipline capabilities and protocols for theanalysis of explosive residues.

Secondary scenes

[84.1170] Secondary scenes are often a source of key information and in some cases themissing link in reconstructing the device and overall sequence of events. Secondary scenes caninclude:



(a) Morgues and hospitals

Residual evidence of the device and chemical residues may be recovered from the deceasedand/or injured at morgues and hospitals. The post-blast scene examiner should work closelywith the forensic pathologist or other medical practitioner to ensure that potential evidence isrecovered and that relevant questions are answered. Paragraph [84.1220] provides more detailsin 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 canbe prime sources of evidence. These could also include premises, vehicles, boats etc that mayhave been involved in the incident at some stage. Houses/premises where it is believed theoffenders may have constructed (or stored) a device should be examined for evidence of thedevice, 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 personsshould also be examined. Locations (such as open areas) where persons of interest may haveundertaken trials with devices or explosives or hidden materials should also be examined. It isvital that consideration be given to eliminating any potential cross-contamination of thesecondary scene from the primary scene. Steps that can be taken include personnel examiningthe primary scene and equipment utilised in the primary scene, should not enter the secondaryscene. If this cannot be avoided, then appropriate precautions should be taken, includingpersonnel showering and donning new protective clothing and cleaning and testing previouslyutilised equipment prior to entering the secondary scene.

Control swabs should also be taken from the equipment and personnel prior to entering thescene. These precautions are taken to ensure that any evidence located and identified at thesecondary scene is the result of a true connection with the primary scene and not a result ofcross-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, forensiccoordinator) in conjunction with the senior investigating officer prior to entry in order to meetinvestigative priorities and ensure there are no missed opportunities.

A secondary scene may also be a clandestine laboratory where the explosives were or are beingmanufactured/synthesised. These scenes are potentially hazardous and should be processed inconsultation with a forensic chemist or other appropriate hazardous materials responsepersonnel. Typical seizures may include: chemicals; improvised explosives; scientificequipment; personal protective equipment, IED components; literature and experimental notes,including recipes. Speers et al (2013) provide an excellent overview of procedures for the safeand effective examination of clandestine explosive laboratories.

(c) Persons of interest

Samples for trace analysis and reference samples for identification purposes should becollected from persons of interest. Procedures will be guided by the jurisdictional legislationunder which the person has been charged. A number of options exist for when a person can besampled for explosive residues and their clothing collected, however the key points are toprevent the person from destroying potential evidence and ensure that the person cannot comeinto contact with surfaces/persons potentially contaminated with explosives.






Laboratory examination

Forensic disciplines

[84.1210] Once the field examination has commenced and items have been recovered/samples collected, the laboratory examination of these items/samples commences in order toassist in answering the questions outlined in [84.970]. When exhibits from an explosive relatedscene are received at a laboratory, the responsibility for contamination prevention (qualityassurance) transfers to the laboratory. Exhibits should be stored in a secure area and in amanner that prevents the potential for contamination. Where possible, exhibits for traceexplosive residue analysis should be refrigerated prior to examination. This is due to the factthat some explosive compounds are volatile and will volatilise or sublime over time (ietransform into a gas/vapour).

A wide range of scientific and technical specialists can be involved in a post-blastinvestigation, particularly when it comes to examining the recovered evidence. Whilst theobjective of the examination is determined in consultation with the criminal investigators, twoof the primary forensic objectives are: (1) to determine what the IED consisted of and (2) tolink the components to the bomb maker/s. The expertise required depends on thecircumstances and the nature of the evidence. It is important to emphasise the importance of ateam approach, with on-going communication between team members in the laboratory and thefield.

It is important to discuss potential areas of an item or surface to be swabbed for explosiveresidues, DNA, fingerprints and other potential trace evidence with the various scientificspecialists prior to examining items. This maximises the recovery of all potentially significantevidence. A general sequence of examinations by the various disciplines may include:

1. Visual examination (including naked eye and microscopy) to recover intact (orpartially consumed) explosive particles and fragments of interest. This is followed bythe collection of swabs/solvent washes on designated areas of the item for subsequentexplosive residue analysis (usually conducted by the chemist or crime scene officerfollowing consultation with relevant specialists).

2. Latent fingerprint processing by the fingerprint specialists. Depending on the surface,a search may be conducted using oblique lighting prior to swabs being collected instep 1 to assist in identifying suitable areas for explosive residue swabbing andfingerprint recovery.

3. Swabbing for trace DNA by a biologist (or other suitably qualified member).

4. Device reconstruction with post-blast scene examiners, bomb technicians, and otherpersonnel with relevant expertise.

The aforementioned order of examinations may vary depending on the circumstances of theincident under investigation.

Due to the extreme pressures and temperatures that surfaces in contact with and in closeproximity to a device are exposed to during an explosion (in addition to the fire fighting andrescue efforts), the identification and recovery of traditional forensic evidence, includingfingerprints and DNA, becomes more challenging. This section provides an overview ofexaminations that can be conducted by the various scientific disciplines.

Identification materials

[84.1230] Identification materials, such as DNA, fingerprints and hair, are all potentialtypes of evidence that should be considered during a post-blast investigation. Examination ofthese may assist in:



• 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 (fibres and hair), 96 (fingerprints)), however theexamination 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, whetherdeployed to the field or conducting examinations in the laboratory. Suitable surfaces areselected and techniques are applied that would not necessarily be routinely utilised.Notwithstanding the destructive impact of the explosion on identification material, fingerprintscan sometimes be identified on IED fragments. The most probable sources of fingerprints arecontainers eg, bags, boxes, pipe fragments and adhesive tapes.

In Chapter 96 of this work, at paragraph [96.700], Comber et al, (2006) describe procedures torecover and detect fingermarks 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 fingerprints on black electrical tape.

Boyle et al (2004) report on the use of cyanoacrylate (“super glue”) fuming to recoverfingerprints from metal and plastic pipe bomb fragments. The authors determined that theprocess did not significantly interfere with explosive residue recovery and analysis. Thefuming was conducted on-scene and latent print development was undertaken in the laboratory.

Jasuja et al (2007) studied the development of latent fingerprints on the adhesive side of tapesusing phase transfer catalyst and Rose Bengal dye.

The recovery of trace DNA and also explosive residues from areas where fingerprints areobserved is a consideration for forensic scientists in order to maximise the recovery of allpotential evidence. Whilst this recovery will generally only be attempted in the event of a poorquality print (ie not suitable for identification purposes) and in the absence of other DNA ortrace explosive evidence, it is a decision that should be made following consultation withrelevant discipline experts. Research has been conducted into the development of techniques todetect latent fingerprints and subsequently analyse the chemical compounds deposited within,specifically explosives. King (2012) reports on the recovery and identification of explosiveresides deposited in latent fingermarks following the application of different fingermarkdetection methods. The research demonstrates that each fingermark detection method appliedin sequence is likely to reduce the amount of residue remaining. Emmons et al (2009) discussthe use of Raman chemical imaging to detect and identify explosives in contaminatedfingerprints. Hazarika and Russell (2012) provide an overview of advances in fingerprintingtechnology including in relation to identifying chemicals handled by a person and the identityof that person. Verkouteren et al (2010) describe a method based on polarised light microscopyand image analysis for automated mapping of RDX particles in fingerprints deposited using theexplosive C-4. Rowell et al (2012) describe the detection of nitro-organic and peroxideexplosives in latent fingermarks by direct analysis in real time-mass spectrometry (DART-MS)and surface-assisted laser desorption/ionization-time of flight-mass spectrometry (SALDI-TOF-MS). Banas et al (2012) report on the detection of microscopic particles in latentfingerprints utilising synchrotron radiation-based Fourier transform infra-red micro-imaging.Abdelhamid et al (2011) discuss the analysis of explosive residues in fingerprints using opticalcatapulting-laser-induced breakdown spectroscopy (OC-LIBS). Verkouteren (2007) address therecovery of explosive particles (namely RDX and PETN) in fingerprint residues. Phares et al(2000) and Dorozhkin et al (2005) discuss the transfer of explosive residues throughfingerprints.



[84.1250] DNA

Fragments recovered from IEDs should be tested for DNA in the same manner as other objectssuspected of bearing DNA. The heat generated by the explosion does not necessarily negatethe potential for positive results. This was demonstrated by Esslinger et al (2004) who reportedthe recovery of DNA profiles 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 pipebombs, four gave reportable results matching subjects’ DNA profiles, and another eight alsomatched but were below reportable levels. Zamir et al (2000) discuss the extraction andanalysis of DNA from adhesive tapes following processing for fingerprints.

Ramasamy et al (2011) report on the successful recovery of DNA and fingerprints from theexterior and interior of a vehicle following the use of a render safe tool. The authors also reporton the successful recovery of DNA and fingerprints from glass and plastic surfaces of itemsplaced 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 IEDthrough the post blast recovery of DNA from IED containers, in this case - backpacks. Theresearch was successful in recovering DNA from back packs containing smokeless powderfilled pipe bombs (galvanised steel and PVC) following deflagration.

Bille et al (2009) evaluated the effects of cyanoacrylate fuming, time after recovery andlocation of biological material on the recovery of DNA from pipe bombs containing blackpowder substitutes. In summary, only a fraction of the initial DNA deposited was recoveredfrom post-blast pipe fragments. A significant decrease in the amount of DNA recovered wasobserved as time passed since the deflagration (in this case from 1 week to 3 months).Cyanoacrylate fuming did not have a significant effect on the successful recovery and analysisof DNA and greater quantities of DNA were recovered from the pipe nipples compared to theend caps. The paper also includes a discussion on factors that may affect the success of DNAtyping.

These results emphasise the importance of careful handling of post-blast fragments to avoidloss of such evidence. DNA analysis, and the fingerprint examination noted in the precedingsub-paragraph underline the need for a considered and results-based protocol for theexamination of evidence by fingerprint experts, biologists and chemists to ensure that the workof 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 sourceof evidence towards identifying people associated with the device pre-blast. Adhesive tapes arecommonly utilised in the construction of a device and are a prime source of hairs forcomparison to hair from a suspected bomb maker and also DNA if the roots of the hair arepresent.

Hair can also be a source of trace explosive residues, particularly in the case of a bomb-makerand/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 traceevidence should be considered during a post-blast investigation. Physical and trace evidencecommonly associated with post-blast examinations include:



• explosive residues, including control and reference samples;

• metal, plastic, paper/cardboard or rubber (potentially used as a container);

• adhesive tapes, glue;

• monofilament line, string;

• fibres, 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 thisseries (including Chapter 88 (Fibres and Hairs) and Chapter 90 (Paint)) and by Strobel (2012pp 142-144), however the examination of some of the materials in a post-blast context will beaddressed in this section.

Trace evidence from an explosion scene should be examined with a microscope, categorised,reconstructed and analysed as required for identification. If necessary, as the investigationproceeds, items from the scene may have to be compared to standard commercial products ormaterial 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 theexplosive event (eg, closer to the device at the time of initiation). This is because the pressureis greater when closest to the explosive event and decreases as the distance from the deviceincreases. 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 morecommon than others. Examples include: timers, batteries, switches, wires and electricalconnectors, some of which are illustrated by Thurman (2011). Illustration can also be achievedsimply by looking around most homes, shops and electronics stores. There is nothing unusualabout the components of IED initiation mechanisms. What is important is to be able torecognise device components in post-blast debris and reconstruct the device. Industrialproducts can be identified and tracked through thorough police work and consultation withmanufacturing industries and retailers. This investigative process supported by electronic dataprocessing, may lead to identification of customers.

Those involved in examining post-blast debris should be familiar with the potentialsignificance of what they may view under a microscope. This is rather like triage. While theintent may be to seek traces of explosive residues, recognition and understanding thesignificance of battery components or chemicals, electronic parts and burned switchcomponents may advance the investigation in other useful directions.

To be able to make this type of contribution requires the same “3P” approach as lawyers taketo a trial: prepare, prepare, prepare. For the scientist and reconstruction expert alike, the “howto” is: test, test, test. Any likely IED component – as determined by experience, from literature



or by searching the internet, can be acquired, taken apart, and then blown up under conditionsdesigned to maximise recovery. This process provides experience, establishes memory andprovides on-going photographic, documented, physical and chemical databases for futurereference.

A simple looking battery may consist of a painted metal container with interior plasticcontainers 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 beforean explosion so that the components can be identified post-blast.

Electronic devices are complex instruments. The post-blast expert should work together withthe technical specialists in the reconstruction of the device. The specialists can assist inidentifying unknown components or assist in determining the electronic circuitry that wouldhave been utilised to construct the device.

Polymers are another common class of materials associated with IEDs. Examples are paint,fibres and textiles, plastic, glues, rope, monofilament line and adhesive tapes. All can constitutechemical and physical evidence and there is a lot of literature pertaining to their analysis.Polymers can usually be identified by their infrared spectrum. In a comparison of polymericmaterials and other chemical evidence, the objective is to apply analytical methods which aredesigned to detect significant differences in composition whereby the samples can bedifferentiated. For polymers, such additional methods typically include: pyrolysis gaschromatography–mass spectrometry (py GC/MS); scanning electron microscopy with energydispersive x-ray analysis (SEM/EDX); Raman spectroscopy; and micro x-ray fluorescencespectroscopy (XRF). These methods are described in several works including the followingchapters 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 singlefibres as a result of vapour cloud explosions, which may be significant if determining whetherclothes/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 fibres andthe interpretation of analytical results, including measurable effects of destructive processes(including fires and explosions) on fibres.

Quirk et al (2009) discuss the evaluation of carbon and hydrogen stable isotope values ofplastic in order to determine whether fragments of plastic recovered post blast could beassociated with a common source and also with a specific pre-blast source. The specificscenario evaluated in this work was post blast fragments from a two-way radio could beassociated with its undamaged pair. This was achieved when three or more post-blastfragments were recovered.

IED components often are physically bound with adhesive tape. Tape usually survives anexplosion 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 ofcarbon isotope ratio measurements of PVC tape backings to discriminate and also associatesamples as originating from a common source. The carbon isotope values were generallypreserved during the explosion, allowing association of pre- and post- blast samples. Further,adhesive tapes can carry significant physical evidence such as fingerprints and DNA (Zamir etal, 2000), and material such as fibres, hairs and detritus adhering from where and from whomthe 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 usefulgeneral discussion of tape analysis and differentiation, both based on chemical compositionand the potential to perform physical matching/fits between ends of tape.



Document examination

[84.1280] Documents such as personal effects ie identification documents, records, labels,boxes, manuals and notes bearing handwriting, stencils, print etc. can be very useful evidencein 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 ofdocuments to preserve them after being water soaked. The method involved freeze drying andcoating with “parylene”. IR analysis techniques enabled writing in a burned area to be readwhich indicated alterations to a maintenance document. The document contained the probablecause of an air disaster (ie fire caused by under-inflated tyres).

In R v Reyat (1993) 80 CCC (3d) 210; 25 CR (4th) 125n ([84.1900]) the examination of ahandwritten stencil on a cardboard fragment recovered post-blast narrowed the number ofpossible sources of the stereo housing the bomb to single digits out of 4000 produced in Japanand Korea. The cardboard had originated from the box which contained the stereo. The boxmarkings 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 canbe distinguished from impact damage or structural failure. Thus, metallurgical examination canbe a very productive approach to the investigation of suspected explosions, including in theevent 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, 2012Ch 7). If damage to metal is identified as explosive related, then this can assist in identifyingdevice components (eg, containers) and suitable surfaces for further forensic examinations.Examinations of metal plates that may have been utilised to direct force, and metal containersincluding pipes, wires and other metal objects, can be aided by a metallurgist, particularlyduring the reconstruction of the items.

Walsh et al (2003) conducted a study on the post-blast micro-structure and hardness of threecommon metals used in pipe bombs to assist in developing a method for the investigation ofpipe bombs. The damage to the microstructure increased with increasing velocity of detonation(VOD) and pressure generated by the explosive. The material hardness increased sharply andthen plateaued as the pressure and VOD increased. Gregory et al (2010) discuss thecharacterisation of post-blast metal fragments, specifically microstructural changes andmicrohardness, and the potential to correlate the fragment damage with the type of explosivefiller and bomb design.

[84.1300] Toolmarks/serial number restoration

Metal is also a good source of toolmarks. Chapter 85 of this series describes toolmarkidentification. Lang and Klees (2008) have studied toolmarks left by drill bits and determineddrill bit use indicators. They concluded that trace deposits of particulate matter or smears,physical damage including chipping, abrasion and fissuring on the bit, and thermal effects wereprimary indicators of drill use. They also determined that well defined tool marks wereproduced on swarf shavings which could be matched to a particular drill bit. This is pertinentto IEDs such as a pipe bomb in which a hole is drilled to permit insertion of a fuse. The notedpaper provides a good literature review of the topic. Tools such as wrenches used in pipe and



end cap manipulation can leave toolmarks. Toolmarks on wires (and plastic coatings)originating from cutting implements is also useful evidence in associating or excluding aspecific 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. Therestoration of serial numbers from a damaged vehicle chassis during the investigation of theBali 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 thebodies and body parts of deceased persons after an explosion. The examination team(s) maycomprise one or more practitioners from each of the following disciplines:

• DVI practitioner;

• forensic pathologist;

• forensic anthropologist;

• crime scene examiner;

• fingerprint expert;

• forensic chemist; and

• bomb technician.

The forensic pathologist and forensic anthropologist have complementary roles in examiningthe human remains. The role of the forensic pathologist is one of a primary examiner, for thepurposes of identification and to assess any injuries that may be present. The forensicanthropologist can assist the examination, particularly where bone is present, by identifyingdisrupted, heat damaged and badly decomposed body parts for reconstruction and subsequentidentification of individuals.

The examination team also needs to include experienced photographers and scribes. Each teammust work to recognised quality assurance standards using consistent standard operatingprocedures (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 presentdifferently to those that occur after a concentrated explosion. The longer burning effect that isproduced in a dispersed explosion causes greater thermal damage to the skin than that seen ina concentrated explosion. However, the extreme incineration observed in some victims isalmost always caused by post-blast fire, regardless of the type of explosion. Additionally,disruption of the body and typical explosive (triad) injuries may also be observed in victims ofa dispersed explosion, but they are caused by the environment and are not a result of proximityto the point of ignition. Blast injuries also occur after a dispersed explosion.

Six categories of injury resulting from a concentrated explosion have been defined by Marshall(1988) as:



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 thesource of the explosion. The disruption may be localised to one of two regions of thebody – for example, localised, complete disruption of the hands and lower parts of thearms may imply that the source of the explosion was being held. Accordingly, bodyparts assume great importance by implication of contact or very close proximity to thesource of explosion; this should be borne in mind when sampling for explosiveresidues (see below).

2. The second category of injuries is “Explosive Injury” – which consist of a triad ofpenetrating (puncture) injuries, abrasions and bruises. This triad is typically seen invictims who are close to the blast seat but not in contact.

In both “Complete Disruption” and “Explosive Injury” above, there is generally adirty appearance to the skin due to the forceful impregnation of smoke and explosiveresidue.

3 and 4. There may be penetration of the body by fragments of debris from the explosivessource or surroundings. Similarly, dislodged masonry may collapse and causesecondary injuries to the body.

5. Superficial “flash” burns can occur on the skin if the victim is very close to thesource, but they are usually not significant. Most burning of victims is a consequenceof post-blast fire, rather than from the explosion itself.

6. Air pressure changes consequent to an explosion can cause internal injuries, involvingorgans 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.



The interpretation of injuries is important in reconstructing the incident, and placing the victimat the scene. For example, the location on the body, the direction of penetrating injuries andheat 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 primaryfragmentation, but also explosive residues. Recovery of such pertinent physical evidence isvaluable to an investigation. Indeed, the mere existence of such foreign material on a bodyassumes great significance when the primary question is not “What was the explosive?” butrather “Did an explosion occur?” as in an aircraft crash.

As indicated above, it is important not to neglect body parts when attempting to recoverexplosive trace evidence. The evidence may be located on clothing and/or the surface of thebody (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 ofthe body or body part should be made, including photographic record, diagrams and textdescription.

Laposata (1985) has described the protocols listed below for collecting trace evidence frombombing victims.

The external and internal examinations of a body may include a number or all of the stepsbelow; however, these will be dictated by the specific requirements of the incident andavailable resources.

(1) Radiography (plain film x-rays and CT)

(a) dead body

(b) body parts and tissue fragments from the scene

(c) surgical specimens

(d) survivors (including direct magnification radiography)

(2) Recovery of explosive residues

(a) inspect for unconsumed or partially consumed explosives

(b) swab with appropriate solvents, include control swab

(c) collect fingernail 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.



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 hospitaland seize any materials recovered (likewise with the deceased at autopsy). All materialsremoved must be appropriately packaged and submitted to the forensic laboratory via thenormal procedures for continuity of evidence. If a post-blast examiner cannot attend theautopsy or hospital, the pathologist should consult the examiner prior to collection.

Background information

Depending on the circumstances, a forensic pathologist and anthropologist may have attendedthe 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 largeobjects at the scene;

(2) post-explosion alterations of the scene which could produce observed effects to abody other than explosive-related trauma (fire extinguishing chemicals, weather,structural collapse, secondary fire);

(3) suspected bomb type (undisguised, disguised, hidden; that is, an indication of thepossible nature of material from an improvised explosive device (including anycontainers or casing in which the device may be placed) which could be found in oron a body; and

(4) materials in the environment (for example, car interior, room furnishings; ie materialof known origin which might be found in or on the body).

The following literature, and references therein, provide further information on blast injuriesand forensic pathology of victims of explosions:

• The (United States of America) Armed Forces Institute of Pathology (undated) has awebsite 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.




Analysis and identification of explosives

[84.1350] The heart of an IED is the explosive. Identification of the explosive is the taskof the forensic chemist. Chemists can work only on what they receive from investigators andscene examiners. For this section, the assumption for post-blast analysis is that all relevantexhibits have been seized, there are no contamination issues, examinations for fingerprints andDNA have been considered and that the question now is “what was the explosive?”. It is alsoassumed that the laboratory quality assurance issues discussed at [84.1750] are in place andoperational.

There is no universally accepted combination of methods applicable to all cases. Rather, theforensic scientist selects the procedures and instruments which are most appropriate to theexhibits presented and the circumstances of the case. Some techniques cannot be utilised inisolation to identify an explosive or explosive mixture. For instance, portable detectioninstruments such as IMS are generally used as screening techniques to produce results forintelligence purposes or for the triaging of items. Any results that are required to be presentedin court should be confirmed using an analytical technique or combination of techniques backin the laboratory.

Guidelines developed by the Technical Working Group for Fire and Explosives TWGFEX(undated and 2007) for the forensic identification of intact (unconsumed) explosives and theirresidues, provide an overview of the techniques that are regarded as presumptive and therequired combination of techniques to produce a confirmatory result for a range of explosivetypes.

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 nakedeye)?;

• are the results required for court purposes?;

• is the purpose of the analysis to identify the material or to compare with othersamples to confirm common origin?; and

• to what instruments does the chemist have access?

Examination of debris and analytical preparation

[84.1360] A flowchart providing an overview of a generic analytical sequence for theanalysis 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 eachcase. As can be seen in Figure 3, the examination procedure will generally be based on thefollowing five 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. Theapplication of these techniques is discussed in this section. Abbreviations are listed at the startof the chapter.



Figure 3 – Generic analytical sequence for explosive residue analysis



(“I” indicates techniques utilised for the analysis of inorganic compounds and “O” indicatestechniques 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 beanalysed 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 thedebris in airtight containers as soon as practical otherwise these compounds may be lost to theatmosphere.

In order to collect the air sample, a portable pump is sometimes used to sample the air fromaround the seat of the explosion or from material suspected to have been in contact with anexplosive by drawing the air through a substance which adsorbs explosive vapours. The sameprocess is applied in the laboratory to heated debris in nylon bags, mason jars or unused paintcans and is referred to as “direct headspace sampling”. The most commonly used adsorbentsare 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. Thisform of “passive headspace sampling” is achieved by placing the adsorbent material in thesealed container with the debris. The container can then be left to equilibrate at roomtemperature or may be heated in order to volatilise the organic vapours that are subsequentlytrapped on the adsorbent. Adsorbed explosives are recovered by solvent extraction.

Solid Phase Micro Extraction (SPME) is also available for passive headspace sampling. SPMEis based on the adsorption of the volatile organic onto a fibre which consists of a stationaryphase on a fine length of fused silica. This can either be directly injected into an analyticalinstrument such as a GC/MS or extracted with a solvent. Examples of its application arediscussed at [84.1610] and [84.1650].

Visual/microscopical examination for explosives and other traceevidence

[84.1380] Visual and microscopical examination of debris requires meticulous attention todetail combined with the knowledge and ability to recognise and recover pertinent evidence.The efficiency and effectiveness of the examination also reflects the extent to which materialsof high evidential potential have been selected for submission to the laboratory. The emphasisis 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 partiallyreacted explosives. These commonly are low explosives, including grains of propellant powderand components of improvised chemical mixtures. Less commonly, traces of unreacted highexplosives, eg, dynamite, plastic explosives, slurries and emulsions, may be recovered.Significant quantities of unreacted high explosives can be recovered if the explosive “loworders” ie the explosive is not fully converted to gaseous products.



Particles of unreacted explosive or of crystalline residue which are physically recovered fromdebris are examined microscopically and typically analysed by one or a combination of theinstrumental techniques outlined at [84.1410].

High explosives usually are wrapped in paper or plastic. Fragments which survive theexplosion may contain traces of impregnated explosives which can be extracted and identified.Dynamite and some brands of emulsion explosives have paper wrappers. Slurry and emulsionexplosives are frequently packaged in plastic “sausages”, the ends of which are sealed with ametal clip. Metal clips invariably survive an explosion and, if recognised, can provide animmediate clue to the type of explosive used. Access to a reference collection of wrappers ofexplosives is a useful resource for forensic laboratories.

The visual search also incorporates the search for any primary fragmentation that may assistthe reconstruction process. These fragments can also be examined for fingerprints, DNA andtrace 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 themicroscopical examination, then solvent extractions from surfaces of interest are conducted(either by direct solvent washing or collection using a swab). Materials which have sustainedextensive 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 first step, typically, is to collect extractions from materials such as metaland glass which are less likely to produce interfering co-extracted compounds than, forexample, plastics and clothing. Surfaces are also selected based on their suspected locationrelative to the device at time of detonation, with priority given to primary fragments that weresuspected of being part of the device.

Solvent selection depends both on the explosive sought and the material from which theexplosive is to be extracted. The solvent is applied either by swabbing or by direct solventwashing. A minimum quantity of solvent is used. The solvent extract remaining after theswabbing or washing is collected for clean-up procedures ([84.1400]) and subsequentlyinstrumental 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 organicsolvent extraction for oils and waxes prior to use of the polar organic solvent if commercialemulsions are suspected.

The non-polar organic solvent step is included because of the increasing market share ofemulsion explosives which contain oils and waxes which might not be readily soluble in somepolar 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 sodiumnitrate, 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



of “natural” origin, ammonium nitrate from fertilisers, and sodium bicarbonate and ammoniumdihydrogen phosphate from fire extinguishers etc.

This procedure generally yields organic fractions, an inorganic fraction and an insolublefraction (Garner et al, 1986; Beveridge, 1992). Each fraction is analysed systematically (seeFigure 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 boththe 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 orcommercially available medi-wipes (in the field and laboratory) that are extracted with suitableorganic and inorganic solvents. The increasing use of peroxide explosives has resulted in amore specific extraction solvent, eg, acetonitrile.

Twibell et al (1982); Russell (1984); Warren et al (1999); Thompson et al (1999); Broome andTodd (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 oforganic and inorganic explosive residues.

Clean-up procedures

[84.1400] The collected solvent extracts are sometimes subjected to a clean-up procedureprior 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 performanceof columns and detectors; the other is to remove substances which could mask detection oftraces of explosives. In some circumstances, the chemist may decide not to conduct a clean-upprocedure. This may be the case if the extract appears to be relatively clean, the concentrationof the explosive is suspected to be low, or highly specific detection methods are utilised that donot 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 ofpolymer material and then pass a solvent or mixture of solvents through the column. Theexplosive is retained on the column and the contaminants pass through. The explosive issubsequently recovered from the column.

Inorganic extracts can be cleaned-up by centrifuging or filtering. Pre-washed membrane filtersshould be used rather than paper filters, since the latter contain detectable quantities of ionssuch 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 analysedshould not be left standing at room temperature for more than two to three days. Bacterialaction can be counteracted with chemicals such as phenol, methanol and borax. A portion isretained in solution for analysis by methods which require liquid samples, for example, ionchromatography and capillary electrophoresis.

A second portion of the solvent can be evaporated under air or nitrogen at room temperature inorder to analyse the remaining residue. This provides an alternative technique for the analysisof 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); Lloydand King (1990); Beveridge (1992); Song-im et al (2012a); Song-im et al (2012b); Romolo etal (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 continueto improve detection limits for explosives, but no one method can detect all components of all



explosives. Scientists therefore have to analyse explosive residues systematically andcomprehensively. If particles of unreacted explosive are recognised and recovered, then theprotocol required for identification is relatively straightforward. For multi-componentexplosives, like dynamite, several methods may have to be employed. If the question is “Whatbrand of explosive is this?” or “Compare these explosives and determine if they could havehad a common origin” then additives and minor components (such as trace elements) orisotope 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 whichthe retention time (for TLC, retention factor) of an unknown compound matches that of astandard does not by itself constitute identification. This applies to GC, LC, IC, CE and TLC.However, if the detector on the chromatograph is a mass spectrometer, then identification maybe achieved. Techniques like IR, XRF, Raman, XRPD and SEM/EDX may provideunambiguous identification of compounds and elements. Royds et al (2005) provide anoverview of analytical methods for explosive residue analysis, including advantages andlimitations associated with each. Yinon (2007, 1999) and Beveridge (2012) provide in-depthdiscussions on the application of various techniques for the detection, analysis andidentification of explosives.

Examples of techniques that can be utilised for the analysis of bulk explosives and solventextracts 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 operationare provided in Appendix A. For the purpose of this section, instrumentation is groupedaccording to fundamental principle of operation, ie chromatography, electrophoresis,spectrometry or spectroscopy. The results from each of these techniques are generallyproduced 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 performanceliquid 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)



(d) x-ray fluorescence spectroscopy (XRF) and

(e) x-ray powder diffraction spectroscopy (XRPD).

The US-based TWGFEX Laboratory Explosion Group (TWGFEX, 2007) has publishedguideline tables which categorise analytical techniques for intact explosives and post-blastresidues into four groups.

1. Category 1 provides significant structural and/or elemental information and issufficient for identification.

2. Category 2 provides limited structural or elemental information and requires one moresupporting technique for identification.

3. Category 3 provides a high degree of selectivity but requires two more supportingtechniques for identification.

4. Category 4 are useful but do not fall into categories 1, 2 or 3 and require three moresupporting techniques for identification.

Techniques that fall into Categories 1 and 2, include: IR, Raman, GC/MS, LC/MS, XRD andEDX. The material being analysed will dictate whether the technique is regarded as a Category1 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 pointmeasurements.

The bottom line, however, is that while it is essential for forensic scientists to set standards forthemselves, it is the courts which determine whether the evidence is admissible. Like scientifictheories, analytical methods and protocols last for as long as they can withstand challengesfrom counsel well briefed by independent experts who may testify and / or advise counsel. Ifanalytical methods and protocols withstand legal challenges, they are maintained. If they donot, they are revised.

Bulk explosives

[84.1420] Particles of unreacted explosive or of crystalline residue which are physicallyrecovered from debris are examined microscopically and typically analysed by one or acombination 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 undertakinginstrumental analysis).

If the particles are a mixture of organic and inorganic compounds, components can beseparated by solvent extraction and individually identified. The procedures and analyticalmethods are similar to those described below for trace residues except that clean-up is notrequired.

Organic extracts

[84.1430] Materials extracted by organic solvents may contain explosives, non-explosiveadditives and co-extracted contaminants. A high concentration of co-extracted material relativeto explosives usually necessitates clean-up procedures.



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 ANFObeing used in large scale explosions, means that there should also be a screen for petroleumoils and waxes. IR, GC/FID and GC/MS are suitable methods. Since oils and waxes are widelyused products, it is important to analyse relevant control/reference samples.

If nitrate esters, nitramines or nitro-compounds are identified, then the class of explosive isestablished and specific additives may be sought.

Inorganic extracts

[84.1440]

Unevaporated extract

Inorganic solvent extracts are analysed for cations (positive ions) and anions (negative ions) byion chromatography. Since the ions are indicated by response time only, and since responsetimes can be affected by parameters such as concentration, further confirmation is required.One simple method is to “spike” a second sample with the indicated ion and observe theresponse. However, a second method is desirable. Capillary electrophoresis has been shown tobe a complementary method for anion confirmation (McCord et al, 1994). An alternativemethod for confirming 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 analyticalcolumn (ie different stationary phase/packing). This is also an option for GC and LCtechniques when analysing organic extracts.

Evaporated extract

Evaporation is typically achieved quickly on a steam bath or slowly at ambient temperatureusing a stream of nitrogen gas.

(1) Crystalline residue: if the evaporated residue is solid, methods of analysis are drawnfrom IR, Raman, SEM/EDX, micro-XRF, and XRPD.

Depending on the sample composition, these methods can provide definitiveidentification. Spot tests may be used for screening if there is sufficient sample.

If the analysis of an evaporated extract indicates more than one compound, forexample, sodium nitrate and potassium chloride, these compounds might not havebeen present in the residue prior to extraction; the ions might have been originallyassociated as potassium nitrate and sodium chloride.

(2) Syrups: if the residue is a syrup, this could indicate residual sugar. Such samples areunsuitable for analysis by XRPD. Refer to section 84.1600 for a summary ofanalytical techniques for sugars.

Evaporating a sample and analysing the residue by IR, Raman, SEM/EDX, micro-XRF orXRPD, provides non-chromatographic identification (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 mostappropriate.



Insoluble material

[84.1450] Insoluble material in solvent extracts of explosive residues may include suchmaterials as unreacted aluminium from slurries, emulsions and improvised explosives; bariumsulphate from a limited number of dynamites and slurries (particularly those for seismicapplication); 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 andBender and Beveridge 2012, 2012).

Identification and Interpretation

[84.1510] Determination of the appropriateness of analytical techniques and thesignificance of the analytical results are primary responsibilities of a forensic scientist and arethe essence of reporting and expert testimony. That is, what do the results of the analysesmean? This section focuses on issues pertaining to the positive identification of the majorclasses 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 maincharge and initiation systems, the efficiency of the explosion reaction, materials/chemicalspresent in the environment at the time of the blast, and the treatment/handling of the itemscontaining the residues following the blast eg, exposure to the environment and/or otherexamination conducted on the item prior to explosive residue analysis. Murray (2012) providesan overview of key factors with respect to interpretation and determining the significance ofanalytical results. After a reminder that all personnel, working areas, equipment, andinstruments must be demonstrably free of explosives, he discusses the pertinent factorsinfluencing interpretation and significance, and which scientists should consider, to be asfollows:

• 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 commonpath 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 addressesthe post-blast identification of residues, however also encompasses the identification of intactsamples which will aid pre-blast association of samples for common origin or comparison ofpost-blast to pre-blast recovered samples.

Propellants

[84.1520] Low explosives generally encompass propellant powders and inorganicchemical mixtures initiated by flame 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



Beveridge (2012 Ch 11). The following sections discuss the identification of commonpropellants, both pre- and post-blast, including black powders and their substitutes andsmokeless powders.

[84.1530] Black powder and black powder substitutes

Black powder’s 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 identified by IR and Raman spectroscopy.If extracted with water, the ions can be identified by IC and a complementary method such asCE. Sulphur may also be identified by IR spectroscopy or by SEM/EDX. Bradley (2005)discusses a method for the identification of elemental sulphur in explosives and explosiveresidues utilising GC/MS. If an SEM/EDX is equipped with a low element detector, carbonmay be detected. If a sample is burned, some sulphur is converted to sulphate and thiocyanateand carbon to carbonate. Both of these ions can be identified by IR or Raman or in solution byIC and a complementary method (eg, CE).

Many black powder substitutes have appeared on the market with various components andadditives. Black powder substitutes generally consist of a carbonaceous organic fuel andinorganic oxidisers such as KNO3 and/or KClO4. 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 identification of black powders, the morphology and the chemical composition,including each component, should be determined. Table 1 provides an overview of componentsof black powder and substitutes, together with the techniques that can be used for the analysisof 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 samevisual appearance and oxidisers (potassium nitrate, potassium perchlorate), however differentfuels. 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 identified by IR, Raman andXRPD (NB Of these techniques only Raman can identify the presence of carbon). SEM/EDXidentifies Na, K, S and Cl, and may also identify C, N and O if equipped with a low elementdetector. HPLC with a UV detector can indicate the presence of dicyanodiamide (DCDA) andsodium benzoate (Bender, 1989a; Bender and Boyle, 2004), as can GC/MS. Nitrate andperchlorate ions can be detected by ion chromatography and 3-nitrobenzoic acid can bedetermined by GC/MS and FTIR (Bender and Boyle, 2004). In an alternative approach,Dreifuss and Goodpaster (2004) applied reversed phase electron spray ionisation LC/MSmethods to identify nitrate, perchlorate, dicyanodiamide, and benzoic acid in Pyrodex and thesame compounds plus 3-nitrobenzoate in Triple Seven. The method also identified ascorbicacid in intact powders. Klapec and Ng (2001) also discuss the use of CE for the detection ofsodium benzoate. Routon et al (2011) report on the derivitisation of the organic fuels inPyrodex and Triple Seven, with subsequent analysis by GC-MS. The method was successful inthe discrimination of Pyrodex and Triple Seven samples, both intact particles and post blastresidues.

Ascorbic acid has created some analytical difficulties because of its tendency to chemicallydegrade. This property has led to applications directed at identifying degradation products ofascorbic acid. Goodpaster and Keto (2004) have approached the problem by identifying



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 identified

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-flight 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 particlesof black powder and black powder substitutes

Technique BlackPowder

Pyrodex® Triple Seven® JimShockey’s

Gold®

IR,Raman,SEM/EDX,XRPD, IC,CE

potassiumnitrate

potassium nitrate potassium nitrate potassiumnitrate

Raman,SEM/EDX

sulphur sulphur - -

Raman,SEM/EDX

charcoal charcoal charcoal -

IR, RamanSEM/EDX,XRPD, IC,CE

- potassium perchlorate potassium perchlorate potassiumperchlorate

GC/MS,LC/MS IC,CE,IMS/MS

- - - ascorbicacid

GC/MS,LC/MS

- sodium benzoate sodium benzoate -

GC/MS,LC/MS

- dicyanodiamide(DCDA)HN=C(NH2)NHCN

dicyanodiamide(DCDA)HN=C(NH2)NHCN

-

GC/MS,LC/MS

- - 3- nitrobenzoic acid -



Technique BlackPowder

Pyrodex® Triple Seven® JimShockey’s

Gold®

HPLC/ESI-QToFMS

Ascorbate,perchlo-rate,nitrate,chlorateanions

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 ofpost-blast residues (including anions and compounds) from pipe bombs containing blackpowder 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 etal (2010). These data are a summary and representative only, and results will vary dependingon the conditions of the explosion.

TABLE 2 Techniques for the analysis of post-blast residues of black powder andsome black powder substitutes

LiteratureReference/Technique

Black Powder Pyrodex® Triple Seven® Jim Shockey’sGold®

[a] IC/CE NO3-, NO2

-,SO4

2-, HS-,HCO3

-, (Cl-)**

NO3-, NO2

-,Cl-, SO4

2-, HS-,HCO3

-

NO3-, NO2

-,Cl-, ClO3

-,ClO4

-, HCO3-

NO3-, NO2

-,Cl-, ClO4

-,HCO3

-,ascorbate

(* contami-nant)

[b] IC/MS NO3-, NO2

-,Cl-, ClO3

-,ClO4

-, HCO3-,

oxalate,threonate

[c] LC/MS NO3-, ClO4

-,Cl-, CNS-,benzoic acid,DCDA

[d] XRPD K2SO4, KCl,K2CO3

KCl, K2CO3,

[d] HPLC Sodiumbenzoate,DCDA

Sodiumbenzoate,DCDA,3-nitrobenzoicacid



LiteratureReference/Technique

Black Powder Pyrodex® Triple Seven® Jim Shockey’sGold®

[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 reactionproducts which may be relevant to components of different black powders. If intact or partiallyconsumed particles are recovered post-blast, then techniques represented in Table 1 wouldgenerally be utilised for analysis.

[84.1540] Smokeless powders

Smokeless powders, which are widely available in bulk form in the United States of Americafor hand loading, are commonly used as pipe bomb fillers (Wolfe, 1991; National ResearchCouncil, 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 canprovide strong associative evidence if the brand can be determined. To do so requires acombination of morphology and chemical composition including additives Powders aremanufactured in various forms which are designed for burning properties. Some more commonshapes are balls and discs which usually are double base powders, and tubes and rods whichusually are single base powders. Careful measurement of morphology is the first step inforensic examination. Size, shape, colour, surface appearance and texture can give a highdegree of discrimination. Recovered particles can be compared to reference particles. This isfollowed by chemical analysis. Infrared spectroscopy should be used to confirm the presenceof 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 and1159 cm-1.

To determine if the product is single or double base, an examination must be made fornitroglycerine (NG). Appropriate methods range from TLC (Beveridge et al, 1975) toinstrumental methods including GC/MS, LC/CL, LC/MS and others (see below). Thesetechniques can also be utilised to identify the presence of other organic additives. WissingerBR McCord (2002) and Cascio et al (2004) refer to the analysis of smokeless powders usingHPLC.

In post-blast residues, the presence of the various components should be identified in thesolvent extracts (eg, NC and NG in the organic extract). In addition, high levels of nitrate ionsmay be detected with IC and/or CE.

Identification of a powder as single or double base may suffice in minor investigations, but ifthe purpose is to identify a manufacturer or to compare samples from a scene to powder inpossession of a suspect, then analysis and identification of the additives and their derivatives(eg, DPA; N-nitrosodiphenylamine, N-NODPA; 2-nitropdiphenylamine, 2-NDPA; and4-nitrodiphenylamine, 4-NDPA) should be undertaken. Additives can be extracted with anorganic solvent such as methylene chloride (ie dichloromethane) or chloroform and beanalysed with techniques including: TLC, FTIR, LC, GC, GC/MS, and CE. There isconsiderable literature on the topic of additive residue analysis since the IED field overlaps thelegitimate field of propellants used in ammunition.



Chemically, organic gunshot residue has the same composition as that of smokeless powdersused in an IED. The quantity of intact powder in the residue from an IED; however, is muchhigher than in organic gunshot residue. Burleson et al (2009) report on a SPME technique toextract organic gunshot residues (including DPA, EC and MC) from a single particle ofpartially burnt smokeless powder. The samples were analysed utilising a GC-nitrogenphosphorus detector (NPD).

Lopez et al (2013) also report on a method to estimate the age of gunpowder samples based onthe concentration of DPA and its derivatives (as determined by HPLC) over time.

One of the first reported methods for the analysis for additives and their products was TLC(Archer, 1975). McCrehan and Reardon (2002) of the United States of America NationalInstitute of Standards and Technology conducted a study with the purpose of determining thestate-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 recoveredby ultrasonic extraction and analysed with micellar CE (MEKC), compositional informationwas obtained.

LC and CE are often the methods of choice, in part because they are operated at ambienttemperature which eliminates the problem of thermal degradation of additives which can be aproblem with GC analyses. McCrehan and Bedner (2006) used both methods to derive an LCreference standard containing NG, DPA, N-nitrosodiphenylamine, and ethyl centralite.McCrehan et al (2002) used CE to compare propellant powders using a propellant: stabiliserratio to compare organic gunshot residue to unfired powder and to determine the extent towhich cartridges in a box could be associated.

In a different application, Hopper and McCord (2005) used capillary zone electrophoresis toanalyse inorganic ions in smokeless powders. IC was used as a complementary technique.They analysed intact powders, residues from burning and residues from pipe bombs. Theyconcluded that in general, differences in relative and overall ionic concentration can be usefulin distinguishing between individual powders and between smokeless powders and inorganicmixtures.

McCord and co-scientists have also researched the application of gradient reversed phase LCfor the analysis and comparison of smokeless powders using a UV detector (Wissinger andMcCord, 2002) and an MS detector (Mathis and McCord, 2004).

In one of the largest studies of smokeless powders, Rankin and Cottle (2004) combined HPLCwith a diode array detector (UV) and GC/MS to analyse over 300 samples. By application ofmultivariate statistics they reported that for double base powders, the combination of NG, DPAand 2,4 DNT concentrations was highly discriminating, and for single base powders, the ratioof 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 powdersusing SPME sampling and analysis by GC-MS, GC-µECD and IMS. A technique for the fielddetection of smokeless powders using an IMS detector is demonstrated through the study of 65smokeless powders. Energetic materials and additives, including: diphenylamine, ethylcentralite, methyl centralite, 2,4-DNT and NG (in the case of double base powder) were allsuccessfully detected.

Perre et al (2012) report on the application of capillary electrochromatography coupled to UVand time of flight-mass spectrometry (TOF-MS) for the separation and identification of



fourteen organic compounds commonly encountered as additives in smokeless powders. Themethod shows potential in differentiating brands of smokeless powders.

Even if successful, Kelly and Mothershead (2001) note some potential complications inidentifying a brand, particularly:

• manufacturer change of suppliers;

• wholesale marketers may switch bulk products (powders may have differentcompositions 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 flash powder mixtures are relatively straightforward to analyse. Analytical schemeshave been published by Meyers (1978) and Midkiff (1989).

The post-blast residues may contain traces of unreacted powder and also reaction products. Inintact particles, chlorates are readily identified by IR, XRPD and Raman. The metal fuel can beidentified by XRF and/or SEM/EDX. Flash powders generally produce chlorides as thereaction product. Sodium and potassium chloride are transparent in IR so cannot be used foridentification. XRPD and Raman are suitable, and IC/CE of an aqueous extract can show thepresence of chloride, sodium and/or potassium ions. The metal component is converted tometal oxide which can be identified by XRPD and analysis by SEM/EDX will give aqualitative analysis of the elements present.

Phillips (2001) reported that flash powders deflagrated both unconfined and confined in pipesproducing spherical particulate residues, the composition of which were characteristic of thecomposition of the metal fuel. SEM/EDX was utilised for the analysis of the residues. Kosankeet al (2003, 2006) subsequently reported similar findings.

Other pyrotechnics

Pyrotechnics contain chemicals for specific effects, one being whistling fireworks. Fung (1985)has reported the use of such mixtures as the explosive component of pipe bombs. IR spectra ofsolvent extracts of a white powder revealed compositions of potassium perchlorate and sodiumsalicylate in one instance and potassium perchlorate and potassium benzoate in the other.These mixtures were attributed to whistling fireworks, one of which matched a known brand.

Brandsma and De Bruyn (2001) reported on the application of ion chromatography to screenfor oxidisers and use of spot tests, x-ray fluorescence and SEM/EDX for confirmation. Theyfurther reported an ion chromatography system for monovalent and divalent cations.

Vermeij et al (2009) examined the morphology and composition of post blast pyrotechnicresidues at different levels of confinement. Three different flash powder compositions and ablack powder composition were evaluated, with residues analysed using SEM/EDX and XRD.Although the level of confinement was reported to have a minor effect on the morphology ofthe residues, further work was recommended.



Castro et al (2011) have also reported on the successful analysis of several confiscatedfireworks samples using Raman, SEM-EDS and FTIR. A comparison of the techniques for theidentification of the core components and also additives is included.

An advantage of IR, Raman and XRPD analysis of inorganic compounds isolated intactwithout 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 CEand 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 volatileorganic compounds (EGDN and NG) and non-volatile organic compounds (eg, NC) through towater-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]). Thesecomponents can be recovered from hand swabs or from post-blast debris by systematicanalysis. Earlier approaches were discussed and illustrated by Beveridge et al (1975) based onsuccessive solvent extraction and methods based on IR and TLC among others. Developmentsover following decades particularly have enhanced analysis and identification of the organiccomponents 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 productsas prills (solidified droplets typically around 1.5 to 2.0 millimetres in diameter) which canreadily be identified as AN from its characteristic infrared spectrum (Zitrin and Tamiri, 2012Ch 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 Nessler’s reagent) (Amas andYallop, 1966) which can be applied to screen large quantities of residue. In residues recoveredas swabs, AN typically is sought as its constituent ammonium and nitrate ions. The primarytechnique is IC complemented by another technique, eg, CE.

In emulsions, the AN, frequently in combination with sodium nitrate, is combined with variousoils and waxes, sensitisers and often aluminium. Analysis of emulsion explosives and theirpost-blast residues generally has consisted of extraction with non-polar solvents for oils andwaxes, and with water for the nitrate salts, leaving residual solids. Analysis has been relativelystraightforward, drawing for example on: spot tests; IR; GC/FID; LC/UV; IC; SEM/EDX andXRPD (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 ANand 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 isotoperatio mass spectrometry. The widespread use of AN as a fertiliser also makes it a primeprecursor for illegal explosives (National Research Council, Committee on Marketing,Rendering Inert, and Licensing of Explosive Materials, 1998, Chs 4 and 5). The analysis andidentification 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



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 analysedby IR and TLC. Commercial and military explosives are designed to be efficient and as such, ifthey high order, little, if any at all, will be recovered intact. If a device containing such highexplosives low orders, then intact particles may be recovered for analysis.

Intact particles of explosives such as RDX, TNT, PETN, and tetryl can generally be identifiedutilising FTIR (Zitrin and Tamiri, 2012 Ch 16). When analysing post-blast residues, if any arerecovered, then the compounds can be identified by GC and LC connected to an MS or CLdetector. Highly volatile compounds are more suited to analysis by LC as opposed to GC as thelow operating temperature of the LC reduces the likeliness of thermal decomposition of theselabile compounds. TLC methods are also long established and can also be utilised for theclean-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 productsand thermal fragmentation pathways are provided.

Yinon (1999) provides an overview of the degradation processes and products of variousexplosives. These potential products for TNT, tetryl, RDX and nitrate ester explosivesincluding NG and PETN, should be considered during the interpretation of results if sampleshave been exposed to various environmental conditions eg, water, sunlight, and microorganisms(eg, in soil).

Basch et al (1986) discuss the recovery and identification of dinitrate and trinitrate esters ofpentaerythritol post explosions involving PETN. Tamiri and Zitrin (2012, Ch 15) provides aconcise discussion and illustration of complex rearrangement products in the MS of PETN.

Dinitrotoluene (DNT) and dinitrobenzene (DNB) have been discussed as two of the mainpost-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 associatedsafety, it can be utilised to understand some of the decomposition products of some commonorganic high explosives which may be encountered during the interpretation of results.

Lai et al (2010) address the identification of volatile taggants, including cyclohexanone andDMNB, in plastic explosives (C-4, Semtex, and Detasheet).

The GC instrument section in Appendix A provides further references for the analysis oforganic 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 improvisedexplosive mixtures to aid first responders. We note, however, that improvised explosivemixtures should only be handled, sampled or disposed of by bomb technicians and/or forensicchemists trained, equipped and aware of the deadly inherent dangers which such mixturespose. Further, interpretation of the significance of chemical precursors lies with forensicchemists.

The National Research Council, Committee on Marketing, Rendering Inert, and Licensing ofExplosive Materials (1998, 126-132, 147) has discussed and assessed chemicals most likely to



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 bereacted to produce explosive compounds. Some of these chemicals are discussed below.

Improvised low explosives typically are mechanical mixtures of fuels (eg, carbon-rich fuelslike sugar and metal powders like aluminium) and oxidisers (eg, nitrates, chlorates orperchlorates) (National Research Council Committee on Marketing, Rendering Inert, andLicensing of Explosive Materials, 1998, 126-132, 147). The residues can consist of unreactedchemicals and products of the oxidation / reduction reaction (see Table 3). The samples areanalysed using the same approach as for other samples, including microscopy and subsequentinstrumental analysis (including FTIR, XRPD, Raman, XRF and SEM/EDX) of recoveredparticles and solvent extractions.

The organic solvent extract would be analysed for carbonaceous fuels by GC/MS and/orLC/MS. The aqueous extract is analysed using ion chromatography complemented by CE orby evaporation and analysis of the solid residue as described previously. Insoluble materialsuch as metals and metal oxides are analysed by the same methods noted for physicallyremoved solids. Sulphur may also be identified by IR or by SEM/EDX. Bradley (2005)discusses a method for the identification of elemental sulphur in explosives and explosiveresidues utilising GC/MS.

Examples of analysis of components of improvised explosive mixtures are provided byWakefield 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) havedescribed the application of a portable CE instrument to on-scene identification of inorganicpost-blast residues. Kuila et al (2006) discuss the analysis of a range of improvised lowexplosives and their post-blast residues utilising IC and SEM/EDX. Lim et al (2007) havedescribed a protocol based on Raman spectroscopy and have illustrated its ability to determinechemical 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 borneimprovised explosive device” (VBIED) (Sachtleben 2012, Ch 10). This device is a vehiclebearing explosives. During the “troubles” in Northern Ireland, chlorate–sugar mixtures wereused; however, fertiliser bombs have become a more commonly used improvised mixture. Twofertilisers typically used for this purpose are ammonium nitrate and urea nitrate. Chlorate andperchlorate based devices continue to be used, with an increase observed in different regionsover the past decade (section 84.1630 refers).

Ammonium nitrate based improvised explosives

Improvised explosives made with ammonium nitrate fertiliser have been widely used in illegalbombings. The Irish Republican Army used mixtures with sugar in large vehicle bombs in bothIreland and the United Kingdom. Authorities tried to reduce the effectiveness of such mixturesby mixing the ammonium nitrate with calcium carbonate to reduce its explosive sensitivity(National Research Council, Committee on Marketing, Rendering Inert, and Licensing ofExplosive 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 recoveryand analysis of residues from large bombs composed of AN / sugar and calcium ammoniumnitrate / sugar respectively. Brown et al (2004) describes the analysis of AN using SPME andGC/MS.



Residual sugar may be sought by derivatising the aqueous extract or its residue on evaporationand analysing by GC/MS (Beveridge et al, 1983; Nowicki and Pauling, 1988). The presence ofresidual sugars may also be indicated by IC (Walker et al, 2001) and by colour tests (eg,Fehling’s solution). Phillips et al (2000) provide excellent details of experimental conditionsboth for analysis by IC of ammonium and nitrate ions and of sugars. They also fully describean LC/UV method for detection of sugars. The ammonium and nitrate ions were typicallyrecovered after the large bomb explosions but sucrose was not. Some explosions did yieldglucose.

The fuel oil component of improvised or commercial ANFO may be extracted with a suitableorganic solvent (eg, pentane or dichloromethane) and analysed by GC/FID and/or GC/MS. Theremaining 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 inANFO. Post-blast, the fuel oil component may be recovered by an organic solventswab/washing from the surface of interest. Alternatively, a charcoal strip can be added to thepackaging 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 berecovered post-blast through the use of a water swab/wash of the surface of interest. AN is alsopartially soluble in acetone.

Additional details in relation to the analysis and identification of ammonium nitrate basedcommercial 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 andnitric acid. It was reportedly used in the World Trade Centre bombing in New York in 1993and is reportedly used by suicide bombers in Israel (Almog et al, 2007). UNi can be identifiedby its IR spectrum, but not in trace amounts.

Israeli scientists have published several papers on the detection and identification of UNi.These were designed to overcome the tendency of UNi to hydrolyse in hot water to urea andnitric acid, especially in trace quantities. Almog et al (2005) have described a field test basedon the formation of a red pigment from the reaction of UNi withp-dimethylaminocinnamaldehyde (P-DMAC). A similar reaction has been produced withparadimethylamonobenzaldehyde to produce a yellow dye. The structures of the dyes havebeen determined (Lemberger and Almog, 2007). Almog et al (2007) have reported ananalytical method in which UNi was extracted with hot acetone, cleaned up on a chromosorbG-HP column and analysed by HPLC/MS using atmospheric pressure ionisation. UNi tracesthus recovered were identified by MS. However, under certain conditions, UNi can be formedduring the analytical process from urea nitrate salts and acids or acidic salts (Tamiri and Zitrin2012, Ch 15 p. 655). Tamiri et al (2009) discuss initial research towards trace characterisationof UNi post-blast, specifically the extraction from solid mixtures to organic solvents usingCrown ethers and analysis by LC/MS. Almog et al (2013) further discuss the successfulanalysis of urea nitrate post-blast by GC-MS.

Phillips et al (2000) have described the post-blast scene outcome of a large (545kg) urea nitratebomb.

As with other inorganic compounds of explosive significance, in the event that intact particlesare not recovered and multiple anions and cations are identified in the solvent extract, theoriginal ion pairings cannot be determined with certainty. This means that if urea and nitrateions are detected in an aqueous extract, the confirmed association of these ions cannot be madeie urea nitrate cannot generally be conclusively identified as the source compound. De Perre et





al (2012) discuss the need for selective methods for the detection of UNi and AN. The authorsdescribe a method based on electrospray ionisation time-of-flight mass spectrometry for thedetection of UNi and AN

DePerre and McCord (2011) also discuss a method for the analysis of trace levels of ureanitrate using liquid chromatography-UV/fluorescence. The method detects the presence of theurea 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 andother inorganic compounds, and powdered metals. The significance of identifying ionspost-blast in the inorganic extracts needs to be interpreted in conjunction with appropriateenvironmental controls collected during the investigation and other analytical results. This isalso of significance for organic residues, particular with respect to sites suspected to becontaminated with background levels of organic explosives (such as explosive ranges, quarriesand locations where land mines have been utilised). Understanding potential reaction productsis an important factor in piecing together what the explosive charge may have been. Table 3shows 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 forinorganic ions.

Reaction products or unreactedcomponents

Possible original component

Chloride (Cl–) Chlorate (ClO3–), perchlorate (ClO4

–)

Chlorate (ClO3–) Perchlorate (ClO4

–), chlorate (ClO3–)

Nitrite (NO2–), nitrate (NO3

–) Nitrate (NO3–)

Carbonate (CO32–), bicarbonate (HCO3

–) Sucrose (C12 H22 O11), charcoal, ascorbicacid

Metal oxide Al, Mg, Zn

Sulphate (SO42–), thiosulphate (S2O3

2–) Sulphur

[84.1640] Nitromethane

Nitromethane is an energetic material which is used as racing car fuel. It is listed as anexplosive on its own and has reportedly been used as an adjunct explosive in ammoniumnitrate 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. Identification was based onanalysis 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 bySchulte-Ladbeck et al (2006) and further discussed by Yeager (2012) and Doyle (2012). TATP

TABLE 3 Post-blast products of chemical ractants

was first 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. Theyreported that LC separation is preferred to GC separation of thermally labile compounds likeHMTD. They interfaced an LC to a quadrupole MS with an atmospheric pressure chemicalionisation interface in positive mode and achieved identification of HMTD at levels ofdetection 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) appliedHPLC/APCI-MS/MS to the analysis of TATP and HMTD and were able to achieveidentification of both peroxides in the same analytical run. The method was successfullyapplied to post-blast identification of TATP. Tamiri and Zitrin discuss and illustrate massspectra of peroxide explosives (2012, Ch 15 pp 646-648; 657). Doyle (2012, Ch 13pp 563-566) discuss practical issues in identifying TATP and HMTD, and present datasupporting 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 directlyfrom 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 SPMEfollowed by GC/MS. The authors reported successful use of the method for identification of 54exhibits of post-blast samples of TATP over a 1 year period. Nakamura and Arai (2001)reported the successful identification of TATP from post-explosion debris using GC/MS inelectron impact mode. Subsequently, Nakamura et al (2004) published analytical data on theanalysis of HMTD, TATP and a by-product of its synthesis, diacetone diperoxide (DADP) byRaman and IR spectroscopy and by GC/ECD, GC/MS and HPLC/UV (photodiode arraydetector). HMTD was also analysed by GC/CL.

Egan et al (2004) studied the GC/MS analysis of TATP and HMTD. They concluded that theapplication of positive chemical ionisation allowed more definitive identification than electronimpact alone. They reported that ammonia was a better reagent gas for TATP while methanewas better for HMTD. Both SPME and evaporation of acetone solutions were usefulpreparation techniques for each peroxide.

Buttigieg et al (2003) characterised TATP by nuclear magnetic resonance, Raman and IR. Theysubsequently analysed it by IMS and by coupling the IMS to a mass spectrometer were able toidentify 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 IMSand GC/MS. Armitt et al (2008) provide a discussion on the analysis and detection of TATPand other organic peroxides, including degradation and decomposition products. Cotte-Rodriguez et al (2008) discuss the in situ detection of peroxide explosives using desorptionelectrospray ionisation and desorption atmospheric pressure chemical ionisation. Schulte-Ladbeck et al (2003) also discuss a method for the recovery and analysis of TATP in theambient air.

Oxley et al (2008) discuss a study comparing Raman and infrared spectroscopy for the analysisof TATP, HMTD and other peroxide-ring structures.

Burks and Hage (2009) present a review in developments in the detection of peroxide-basedexplosives 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 planarsolid-phase microextraction coupled to an IMS detector.



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 anddegradation products (Matyáš et al, 2011; Haroune et al, 2011; Partridge et al, 2010; Fitzgeraldand Bilusich, 2011; Fitzgerald and Bilusich, 2012). These methods can assist with sampleidentification, as well as provide indications of synthesis conditions, starting materials andultimately source association.

Unlike the peroxide based explosives (such as TATP and HMTD), the analysis andidentification of the hydrogen peroxide organic material mixtures are reliant upon the recoveryand analysis of the individual components of the original mixture. A number of papers discussthe 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 analyseperoxide explosives, both unreacted and post-blast. In the former case, it is prudent not tohandle or store bulk material in a laboratory.

As with all explosives casework, laboratories must decide based on the literature and their owntests 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 thesignificance of the analytical results. Primary sources are the literature, contacts withmanufacturers and regulatory agencies, conference attendance and professional visits.Scientists engaged in explosive residue analysis obtain extensive technical information fromexperiments on an explosives range by collecting and analysing residues of availableexplosives on a variety of typical substrates. The usefulness and limitations of availablemethods are also assessed by experimenting in the laboratory by applying traditional and noveltechniques to explosives, to substrates, to substrates plus explosives and finally topost-explosion debris.

In each analysis performed, an unknown compound is compared to standards of explosivecompounds to determine whether it is an explosive. As discussed, some of the techniques thatare utilised are considered confirmatory while others are presumptive. The distinction betweenthese two types of tests must be made clear when reporting results.

If an explosive material is detected using a confirmatory technique, then the sample can be saidto contain explosive residues. That is, a compound in the sample has been identified as aparticular explosive.

The analytical results from any individual technique must be considered with reference to theresults from other tests conducted. For example, an XRF spectrum that shows the presence ofchlorine, potassium and aluminium must be considered alongside the CE or IC result forexample indicating the presence of perchlorate and potassium ions. In this example, it could bereported that “potassium and perchlorate ions were detected in the sample, along withaluminium. These are the residues expected from an explosive mixture comprising potassiumperchlorate and aluminium flakes, commonly referred to as flash powder”.

In the event of recovering and analysing intact particles – if a crystal was analysed by FTIRand found to be potassium perchlorate, and aluminium flakes were identified by XRF, it ispossible to report that “an explosive mixture containing potassium perchlorate and aluminiumflakes was identified”.

If a presumptive test such as an IMS, eg, the Ionscan®, returned a positive result that could notbe confirmed, the result should be reported with stated qualifications. In this instance, the



positive presumptive result could be due to a number of reasons including: the amount ofexplosive material in the sample was so small that it could not be confirmed; the trace ofexplosive present was removed and consumed during the IMS analysis; or the positive resultfrom the presumptive test was a false positive. These possibilities should be made clear in anyfinal 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 (iecontaining residues) or the potential that an explosive or chemical compound may be presentthat is not detectable by the presumptive test being utilised. Consideration should also be givento whether any potential compounds may have been masked by other materials present on theswab or in the solvent extract.

The presence of explosive residues in the environment must also be considered in interpretingresults. Organic explosives are not naturally found in the environment however someenvironments may be contaminated with organic explosives (eg, explosive military ranges).Many inorganic ions that are indicative of an explosive material or a component in anexplosive mixture can be found in the environment. As a result, environmental backgroundsampling and testing is often required to determine the presence and level of inorganiccompounds in the environment (refer to [84.1790]). Of particular concern is the use ofammonium nitrate as a fertiliser. This means that ammonium and nitrate ions are often found insoil. It is therefore imperative that adequate control soil samples are taken and analysed if thepresence of an ammonium nitrate based explosive is suspected. The levels of inorganic ionsfound in swabs collected from the environment must be assessed before reaching a conclusionwith respect to the significance of the presence of inorganic ions in scene samples.

Suitable controls (as discussed at [84.1780]) should also be collected, analysed and reported onwhen positive results are being reported. This demonstrates that the surfaces that may havecome into contact with the item (eg, examiner or examination bench) were not a potentialsource of contamination.

It must be remembered that not all explosive materials can be detected by all tests. The finalreport produced should clearly state what samples were analysed, techniques utilised,explosive compounds or residues for which the samples were tested, analytical test results andtheir significance in the context of the investigation.






QUALITY ASSURANCE[84.1750] The term quality assurance (QA) encompasses a range of aspects relating to theway in which scientists perform their examinations and report on their findings. 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 qualityassurance system.

Accreditation

[84.1760] Most forensic laboratories are accredited against internationally recognisedstandards by a national organisation, for example the National Association of TestingAuthorities (NATA) in Australia, American Society of Crime Laboratory Directors/LaboratoryAccreditation Board (ASCLD/LAB) in the United States, the United Kingdom AccreditationService (UKAS) in the United Kingdom and the Canadian Standards Association in Canada.ISO/IEC 17025:2005 specifies the general requirements for the laboratory to perform testsand/or calibrations, including sampling. The Supplementary Requirements for Accreditation inthe Field of Forensic Science outline requirements specific to laboratories conducting andreporting on forensic examinations. Accreditation works towards ensuring that laboratories areoperating according to their procedures and to a certain standard, ensuring that customers ofthe laboratory receive quality results and opinions. Laboratories have a series of manuals thatoutline the quality, occupational health and safety and training requirements for that facility. Inaddition, standard operating procedures are generally in place for each examination typeconducted and instrument utilised.

Demonstrating that method performance characteristics meet the requirements of the intendedapplication is essential in forensic science and is achieved through method/procedurevalidation. Various publications are available that provide detailed descriptions of theperformance 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. Theperformance 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 significance of the results. Method validation is anexpectation placed on all forensic laboratories, and indeed any laboratory accredited againstthe international standard ISO 17025.

Laboratories perform routine calibrations and checks of instruments and procedures todemonstrate their performance over time. The frequency of the calibrations/checks will bedependent on the instrument and procedure.

Challenges to the work of investigators and laboratory scientists can come through reports andtestimony of independent experts. Challenges can deal with methods and procedures,significance (foundation of opinion) and contamination issues. If challenges are upheld in courtthis may lead to changes in standard procedures and quality manuals to ensure againstrepetition.





Contamination prevention

[84.1770] As mentioned at [84.1050], a fundamental aspect of all forensic examinations,both in the field and in the laboratory, is the need to minimise the potential for contaminationto occur. In a post-blast investigation, like any forensic examination, contamination can relateto any potential evidence type present at trace levels that may be of significance to theinvestigation at hand, eg, fingerprints, DNA, hairs and fibres. The key difference in a post-blastinvestigation is the need to take additional precautions in relation to trace explosive residues.

Awareness of the dangers of contamination is the first step towards ensuring that it does notoccur. Investigators and analysts alike must be able to assure a court with documentation thatexplosive traces detected in debris could not have originated from contamination duringcollection, transportation, analysis or storage. This assurance can only be given by rigidadherence to standard operating procedures and documentation.

If the investigation results in a trial, one of the first areas that counsel may examine is thepossibility of explosive traces (unrelated to the investigation at hand) being broughtunintentionally onto the scene by investigators or others.

Samples are collected from persons and items prior to entering a scene or prior to examiningan item for trace explosive residues. It is important to collect the control samples prior to theperson or equipment being exposed to the scene or item under examination. If the controls arecollected after accessing the scene, it becomes difficult to demonstrate whether the person wascontaminated 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 ascreening instrument and/or a swab for future analysis in the laboratory. These swabs can bereferred to as “pre-entry swabs”. All personnel, equipment, apparatus and containers taken onscene should be swabbed up until a point in the examination phase (either in the scene or thelaboratory) where swabs have been collected for trace explosive residues. All items should nothave been physically associated with any sources of explosives eg, “bomb squad” personneland equipment.

Swabs can be tested by portable detection equipment in order to provide a real time responseto those entering a scene. If a positive result is returned from a person, they should changetheir protective clothing and re-test their clothing. In the case of equipment, items can becleaned down with appropriate solvents and re-tested until a negative result is returned. In thecase of consumables, these should be discarded, replaced and re-tested. Operators should beaware of any limitations of the portable detection equipment being utilised particularly withrespect to the range of explosives that can be detected by the equipment. Working explosivedetection dogs can also be used for screening personnel and equipment. The same cautionsapply as with instruments.

Note: the logistics and practicality of collecting pre-entry swabs of all members, equipmentand items entering a primary post-blast scene often do not allow for such swabs to be collected(eg, fire-fighting and search and rescue operations are paramount and often occurring beforethe 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 circumstancesat hand (eg, entry to scene by a bomb technician prior to the collection of samples forexplosive residues analysis). Once considered, these issues can be addressed by the scientist asto their potential impact on the scene and samples. It is often the case that the potential sourcesof 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 explosivetraces at a secondary scene can often imply association with the primary scene. In thissituation, it is critical that pre-entry swabs are collected from personnel and equipment enteringsecondary scenes where trace explosive residues are of interest.

QUALITY ASSURANCE [84.1770]


The steps outlined above provide an example of precautions that can be taken, however eachcase will present its own individual circumstances on which appropriate procedures will needto be implemented.

In the case of a bomb technician who enters the scene to conduct an initial sweep, whether theindividual dons clean protective clothing or not, consideration should be given to the collectionof pre-entry swabs. Analysis of the swabs will identify the types of explosives the individualwas contaminated with, which may often be different to the explosive of interest in the case athand and will ultimately assist with the overall interpretation of the results. Upon exiting thescene, the bomb technician must also document any contact with surfaces so that thisinformation can be used by forensic chemists in interpreting the significance of positive resultsfor explosives residues.

Quality control procedures used at the United Kingdom Forensic Explosives Laboratory havebeen detailed by Crowson et al (2001), Crowson et al (2007), Beardah et al (2007) andCrowson and Cawthorne (2012). Beveridge (2012) contains several chapters (authored byDoyle (Ch 13), Murray (Ch 18), Broome and Todd (Ch 6) and Strobel (Ch 5)) which discusscontamination and its prevention.




Control samples

[84.1780] As discussed at [84.1770], the key mechanism to demonstrate that contaminationhas not occurred is the collection of control samples (eg, pre-entry swabs). Surfaces fromwhich control samples are collected will be dependent on the situation at hand. As mentionedearlier, control samples should be collected from all surfaces that may come into contact witha surface of interest with respect to trace explosive residues. For example, when examining apost-blast scene, control samples can be collected from the protective clothing of thoseentering the scene and their equipment.

In the laboratory context, Oxley et al (2003) have studied the spillage potential and retentionpotential of several commonly encountered explosives. TNT, PETN, RDX, HMX and TATP inpowdered form showed similar spillage and adhesion to glass but plasticised forms of PETNand RDX showed little potential. Such studies indicate the need for controls.

Controls can be collected from the protective clothing of the examiner, their equipment, theexamination bench and any other surface that the item being examined or the examiner maycome into contact with during the examination. These controls do not necessarily need to beexamined, but should be examined in the event of a positive result. In the event of a positiveresult from a control, the type of explosive should be compared to that identified in the scenesamples. If the explosive type is the same, then it may not be possible to exclude theperson/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 becollected pre-blast (eg, in the event that high risk areas / potential targets have been identified)or post-blast from surfaces in the surrounding area, but outside of the inner blast site. It is alsoa very important step to collect any samples/chemicals from the scene which could interferewith analysis of residues from the explosion, eg, soil or dry chemical fire extinguisher. Suchcontrols assist the forensic chemist in determining the significance of any positive results thatmay be obtained from scene samples. This is particularly important when inorganic compoundsof potential explosive significance are identified as it is more likely that these may be naturallypresent in the environment compared to organic explosives such as TNT or RDX. To aidinterpretation, several studies have been conducted and published. In most of the studies themethods used are IC, CE and SEM/EDX. Unlike case work, one method was often consideredto 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 ininterpreting the significance of finding such reaction products on exhibits from a post-blastscene or on persons or property. The cited studies, other local studies and control samples fromthe 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 similarsubstrate/matrix as that being examined for trace explosive residues. This also assists indetermining the significance of any positive results, particularly in the event of inorganiccompounds. These controls demonstrate whether the compound may have been inherent in thematrix of the surface being analysed. An example of this would be the swabbing or extraction

QUALITY ASSURANCE [84.1800]


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. Anyrecognisable container material (be it a car, a stereo or a suitcase) and/or recognisable parts ofan IED (such as wires, electronic parts, adhesive tapes etc) can provide an immediate lead forthe investigators. Acquisition of a duplicate item for comparison and identification purposescan 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, considerationshould be given as to whether these are regarded as exhibits and treated accordingly or asinternal database samples for casework reference.

Analytical and quality control samples

[84.1820] In order to demonstrate the performance of a technique or instrument, qualitycontrol or analytical standards are routinely analysed. Such standards assist in demonstratingthe performance of the instrument with respect to its ability to detect the components ofinterest. In addition, system blanks are analysed in order to demonstrate that no carry overfrom the previously measured or analysed sample has occurred. This is often conducted withanalytical techniques such as GC, LC, IC and CE.




CASE STUDY – FORENSIC CHEMISTRY IN ACOMPLEX 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 Pacific Airlines flight fromVancouver to Tokyo exploded at Narita International Airport, Japan, shortly after the aircraftlanded. The suitcase was being transferred to an Air India flight bound for Bangkok. Twobaggage handlers were killed and two were seriously injured.

The investigation took several years to complete. The evidence ultimately led to the arrest ofthe suspected bomb maker and his extradition from the United Kingdom to Canada to standtrial for manslaughter and explosives offences. The evidence was largely circumstantial.

This case study focuses on the role of forensic chemistry in the investigation and illustratesmany of the materials, besides explosives, which have to be dealt with by forensic laboratoriesin major explosives incidents.

Jurisdiction

[84.1920] Canada assumed jurisdiction for the criminal investigation, on the basis that anact committed in Canada caused deaths in Japan.

Response teams

[84.1930] Task forces were immediately established in Japan and Canada, andinformation flows 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 Agencyand 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-blastanalysis and a “bomb squad” officer attended the briefings as consultants to the RCMP taskforce.

Canadian teams which subsequently visited Japan consisted of one or two investigators, aforensic 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 heldthere and to conduct preliminary interviews with potential witnesses.


The scene

[84.1940] Immediately after the explosion, the scene – the baggage transfer area at Naritaairport – 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 subsequentlyscreened 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 followingseven 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 highexplosive in a metal container, which Japanese forensic scientists quickly identified as a Sanyostereo tuner, model FMT 611K.

Water pipes had broken and flooded the scene, and two types of dry chemical fire extinguisherhad added ammonium and sodium ions to the scene. Both events complicated residue analysis,since many explosive residues are water soluble and many explosives formulations containammonium and sodium nitrate.

Canadian scientist/investigator teams visited the scene, discussed the formulations of Canadianexplosives, and presented videos of test explosions and residue samples. All exhibits wereexamined in order to identify and negotiate release of material for use as reference standardsfor a search of the suspect’s residence and for comparison to material subsequently seized.

Relevant exhibits were requested through diplomatic channels by way of Notes Verbale. As theinvestigation evolved, this process was repeated several times.

2. Forensic examinations

[84.1970] Japanese forensic scientists examined material from the scene in order toreconstruct the device and identify the explosive. Standards of tuners, timers etc werepurchased in Canada based on the information received and were sent to Japan for furthercomparison.

Canadian scientists concentrated on comparison of material from the scene to material seizedfrom the residence and workplace of the suspect. Every trace of material in every bag wasminutely examined with a microscope to assess its potential significance. A team approach was



used for analysis. The explosives industry was consulted about sourcing dynamite found inpossession of the suspect. Communication with post-blast explosive experts, investigators andJapanese counterparts was continuous.

Analytical protocols were adjusted to deal with contamination of the scene by dry chemical fireextinguishers.

Residue of single base smokeless powder and fragments from an ether can were identifiedearly in the investigation. However, test explosions with smokeless powder and ether usingsimulated “tuners” confirmed the conclusion from fragmentation and damage that the primaryexplosive was a high explosive.

The high explosive was not identified until some five years after the explosion. Dynamitetraces were identified on clothing exhibits, including victims’ clothing. This was achieved by amodified clean-up procedure followed by analysis using the selective TEA® detector. Themethods were GC/TEA® confirmed by HPLC/TEA® and GC/MS. Older methods such asTLC, IR and GC/ECD were completely ineffective because contamination prevented detectionof the trace quantities of residual explosive: Beveridge (1993).

Physical evidence

Laboratory investigation of explosions typically involves much more than identification ofchemical residues. The most important physical evidence found at the scene and subsequentlyassociated 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 andprinting by DocumentsSection)

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 ONCIRCUMSTANTIAL EVIDENCE [84.1970]


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 (victim’sbody)

: MIC, SEM/EDX

(7) Explosives

Smokeless powder (victim’sclothing)

: MIC, IR,TLC

Dynamite residue (clothing) : MIC, extraction, clean-up,

GC/TEA®, HPLC/TEA®,

GC/MS, SEM/EDX

Dynamite (suspect’s home) : MIC, extraction, GC/TEA®,

IR, TLC, SEM/EDX

The tuner proved to be very significant, since a suspect had purchased the same model a fewweeks prior to the explosion and was unable to account for it. Differences in paint,composition and construction distinguished Japanese production from Korean. A Japaneseproduction run of over 2000 tuners was narrowed to the suspect purchasing one of “the veryfew tuners in the world (only five) that could have housed the bomb” in the opinion of thejudge. This was achieved by recovery of a small blackened piece of cardboard bearing a singleletter (“M”) which a document examiner was able to compare positively to a hand writtenstencil which had been placed onto a limited number of tuner cardboard boxes at the Canadiandistribution centre. Wire comparison indicated that the tuner electronics had been removedleaving only the control knob wires inside the metal casing. Recovery of traces of theoperations manual supported recency of purchase.



Another valuable piece of physical evidence which survived the explosion was green adhesivetape from the tuner cardboard box which was indistinguishable from green tape found in thesuspect’s home on another box. Attempts to purchase a standard for comparison showed that itwas not a readily available item.

3. Initial forensic opinions to investigators

[84.1980] Results of comparisons and initial forensic opinions were immediately relayedto the investigators leading to follow-ups in Canada and Japan, further exhibit submissions andfurther consultations. This influenced the direction of the investigation by supporting or notsupporting on-going theories.

4. Forensic reports to investigators

[84.1990] Over 35 forensic chemistry reports were issued. Copies were sent by theinvestigators to the prosecution and thence to the defence as required by provisions for fulldisclosure.

Affidavits were produced for the extradition process through which the accused was returnedfrom 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 chargingquestions, eg, the significance of positive comparisons between exhibits seized from thesuspect and from the scene. Canadian and Japanese forensic findings were correlated.

6. Organisation of testimony

[84.2010] One aspect of trial preparation which was particularly helpful involvedconsolidating 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 testsconducted and fully detailed all measurements and opinions. Photographs and videotapes oftest explosions were also included. A copy was given to the defence to aid in following thetestimony and organising cross-examination.

Commercial products purchased for use as standards for comparison to material recoveredfrom the scene of the explosion and from the suspect, the examination of which formed thefoundation of an opinion, were entered as exhibits.

Keeping track of exhibits and analytical data was greatly assisted by having:

(1) a separate file for each exhibit; and

(2) summary files containing photocopies of all pertinent spectra and chromatograms foreach type of material.

7. Testimony as expert witness

[84.2020] The consolidated report, the summary files, and specific exhibit files were onhand during testimony. By both Crown and defence following the consolidated report, it wasrelatively easy to keep track of the many exhibits and examinations (Jardine, 2012 Ch 20).



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 ofexhibits examined; and

(3) presentation of 68 photographs and six videotapes of tests (reasons, conclusions, andresidues).

One aspect of evidence-in-chief was to negate, by video taped test explosions and presentationof damaged material, some conclusions expressed by a defence expert in an affidavit to theextradition hearing in the United Kingdom that the explosion had been caused by a largecharge of a low explosive.

Cross examination

Defence counsel referred to the consolidated report throughout cross-examination, whichassisted everyone in following the testimony.

Trial

[84.2030] Many police and forensic witnesses from Canada and Japan testified in the ninemonth 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 tomake 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. Thecase against the accused was primarily based on circumstantial evidence. The judge drew uponan Australian case to clarify the issues: Martin v Osborne (1936) 55 CLR 367 (HCA), aprosecution under the Transport Regulation Act 1933 (Vic).



In dealing with the physical evidence, Paris J wrote:

The combination of all the above circumstances disclosed by the physical evidence issufficient to satisfy me beyond a reasonable doubt of Reyat’s participation in the fabricationof 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 theevidence demonstrates that during the period shortly before when the bomb must have beenfabricated Reyat obtained and was in possession of that unique combination of exactlycorresponding materials. “According to the common course of human affairs” that uniquecombination of circumstances could not be fortuitous. The only reasonable inference is thatReyat was involved in the fabrication of the bomb. The contrary cannot reasonably besupposed.

Mr Reyat was convicted of manslaughter and sentenced to ten years in prison over and abovethe three years spent in custody during extradition proceedings, trial preparation and the trialitself. The verdict and sentence were upheld on appeal.






CASE STUDY – THE BALI BOMBINGS(12 OCTOBER 2002)

[84.2080] The forensic response to the three bombings that occurred on the Indonesianisland of Bali on 12 October 2002 is utilised in this section as a case study to demonstrate therequirement for a multi-disciplined approach to a post-blast investigation and also highlightsome of the challenges that scientists may encounter. The joint Bali bombing investigation andvictim identification process is known as Operation ALLIANCE, of which the forensicresponse played a major role in its success.

The incident

[84.2090] Around 11.00pm on a busy Saturday night (12 October 2002) in the maintourist area of Kuta on the Indonesian island of Bali, three explosive devices detonated withinminutes of each other. These bombings resulted in the death of 202 people and the injury ofmore than 200 others. The first explosion was a TNT based device concealed in a suicide vestthat was detonated inside Paddy’s Bar. Within moments of the first explosion, a second largervehicle borne device, consisting of a chlorate, aluminium and sulphur mixture, was initiatedoutside the Sari Club (across the road from Paddy’s Bar). A third device (containing TNT)detonated approximately 10 km away, in the Denpasar suburb of Renon, on a roadsideapproximately 100m from the boundary fence of the United States of America Consulate. Thisthird device was a relatively small improvised explosive device (IED) causing only slightinjury to one person. The forensic response to the third device is not discussed in depth in thiscase study; however, a key development in the forensic response was the recovery of mobilephone components which resulted in the identification of the mobile phone (including makeand model). This was the first indication to the examiners and investigators that the devicescould have been initiated by mobile phones.

The response

[84.2100] At the time of the bombings, two Australian Federal Police (AFP) ForensicOfficers were travelling to Jakarta to deliver a workshop on major incident crime scenemanagement. The members were redirected to Bali, where they arrived on 13 October. Thissmall Australian presence grew relatively quickly as the AFP Commissioner met with the headof the Indonesian National Police (INP) in Bali and signed an agreement to form a jointAustralian-Indonesian Police investigation and intelligence team. Investigators and forensicofficers from Australia (including: five crime scene examiners, three post-blast chemists, twofingerprint experts, one biologist and two bomb technicians) commenced deployment to Balion 15 October. Resources were sourced not only from the AFP, but from all Australian Stateand 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 includelogistics and exhibit officers, odontologists, pathologists, and additional biologists andfingerprint experts to conduct the massive Disaster Victim Identification (DVI) process.Representatives from numerous international law enforcement agencies also joined the jointinvestigation, of which the AFP became the lead with respect to international assistance.


The INP had jurisdiction for the investigation of the incident, and the international agencieswere there to support. A command centre was established at a local hotel, from which the AFPinvestigation, intelligence, forensic and DVI teams operated. All responses were coordinatedfrom this central location. A clear command structure was established with a Forensic and DVICommander assigned to oversee the Australian/International forensic response. Team leaderswere assigned to the Forensic Response and the DVI teams. The Forensic and DVICommander reported twice daily to the Australian Investigation Commander and as significantadvances occurred. Regular reporting was also occurring between the INP and AFPinvestigation teams. Investigators from up to 10 countries joined the INP and AFP in theinvestigation.

The scenes

[84.2110] Despite the Australian teams being off-shore, the scenes were examinedutilising the key principles of post-blast scene examination. Decisions were obviously madebased on the environment and conditions of the scene. The best part of the forensicexamination of the two main post-blast scenes continued for approximately seven days.Following this, the scenes were attended to examine specific areas as required.

As with most post-blast scene examinations, the examination of the two main scenes could notcommence until the fires had been extinguished and all victims had been rescued and thedeceased recovered. Due to the extreme fires that followed the initial blasts in both Paddy’sBar and the Sari Club, the structural integrity of the buildings also had to be determined beforethe examiners could conduct a full examination. Each of these priority tasks had a potentialimpact on the recovery of forensic evidence and needed to be considered by the scientistswhen conducting their examination ie:

1. fires destroyed potential evidence, either by consuming items such as explosiveresidues or burning/distorting items (eg, primary fragmentation) beyond recognition;

2. fire fighting efforts (combined with a broken water main under the road which filledthe crater outside the Sari Club) may have washed evidence away, including explosiveresidues, 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 tandemwith the scene examination) may have resulted in the movement/potential destructionof evidence.

Another factor that may have affected the recovery and identification of explosive residues wasthe humidity in the environment on the island.

Paddy’s Bar

[84.2120] Paddy’s Bar was a two-storey building accommodating a popular bar/nightclub.This is where the first device was detonated on the evening of 12 October 2002.

[84.2130] Scene interpretation

The fire that resulted from the initial explosion had burnt the majority of the structure, inparticular the upper floor which was completely burnt out. The apparent seat of the blast wasidentified due to localised damage to the lower floor, including minor fragment and blastdamage to furniture and body spatter and connective tissue on the ceiling towards the rear ofthe bar. The extent of the localised damage indicated that the actual explosion had not been alarge explosion and that the main explosive charge was relatively small (ie less than 10 kg).



The absence of a crater indicated that the device was not placed on the ground, hence waselevated at the time of detonation. Trajectory assisted in estimating that the device was80–120 cm above the ground at time of detonation.

Post-mortem Examination

The body parts of a young male were recovered from the Paddy’s Bar scene and examined atthe local mortuary. The body parts consisted of a head with associated neck and back skin flapsand a portion of upper left shoulder. Two legs, left and right, were present and were amputatedin the upper thigh region. Physical evidence was recovered from a number of the wound tractspresent on the body parts (see Physical Evidence)).

The under surface of the chin exhibited considerable disruption, which continued upwards ontoboth cheeks. Triad-type injuries were noted on much of the skin surface. Blackening of theskin margins was observed. The directionality of the wound tracts indicated an upwardtrajectory of the fragmentation and blast.

The lower legs both exhibited triad-type injuries, large tunnelling injuries and skin blackeningon both upper calf regions. Small puncture injuries on the heel regions were also noted. Thefront surface of the legs exhibited puncture injuries on the upper surface of the feet and a largetunnelling injury at the level of the right knee. The directionality of these wound tractsindicated 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 Paddy’sBar; however, the few items that were recovered contributed significantly towards ascertainingwhat happened. During the search, small sections of tartan fragment were recovered (each nobigger than a few cm in length). Due to the damage to the fabric, including shredding intosmall fragments and torn/singed edges, it was apparent that the fabric had been in contact orclose proximity to the device at time of detonation. The distribution was centered in one cornerof the bar indicating that it was not uniformly surrounding the main charge. This fabric wassubsequently compared to fibres recovered during autopsy from wound tracks on body parts ofthe 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 insize) were recovered inside the bar and also recovered from the victims and deceased. Thereappeared to be blood and skin in some of the folds of the metal, suggesting that they weretravelling fast enough to pass through people. Some were embedded in fittings and furniture,which was consistent with relatively high velocities. The distribution of the recoveredfragments was relatively wide (ie to most parts of the room) which indicated that the initialdistribution of the fragments may have been centered in/around the explosive charge. Analysisof the metal fragments utilising x-ray fluorescence spectroscopy (XRF) revealed that theyconsisted of 100 per cent iron, with an outer protective layer of aluminium (~96 per cent) andzinc (~6 per cent). It was later revealed that these metal fragments had originated from thesame source and had been added to the device worn by the suicide bomber to increase fatalitiesand injuries in the club.

Fragments of grey plastic were recovered during the autopsy of some body parts. These werevery small indicating that they had been near the device at time of detonation, possibly servingas the container for the device. Later analysis and comparison of these fragments with greypolypropylene pipes (detailed during the confession by one of the bombers) revealed that theplastic was physically and chemically similar to the plastic of the end caps of the referencepipes purchased, but not the body of the pipe.

A battery clip (indicative of a battery serving as the power source) and black insulated monocore copper wire (possibly originating from detonator lead wires) with apparent explosivedamage and fibres attached were also recovered. TNT was identified on the wire.

CASE STUDY – THE BALI BOMBINGS (12 OCTOBER 2002) [84.2140]


[84.2150] Explosive residue analysis

Despite the odds appearing to be against the recovery of trace explosive residues (eg, fire, firefighting, humidity and the large rescue effort), a considered and meticulous approach to sceneexamination resulted in the identification of the components utilised in the main explosivecharge. Swabs for analysis were collected from surfaces above ground level (including fromthe ceiling above the suspected seat of explosion) and from fragments that were recoveredfrom behind a metal barrier that was surrounding a concrete pillar in the club. These swabs andfragments had been protected in part from human traffic, fire and fire fighting efforts.

Initial analysis was conducted in the temporary laboratory (see [84.2250]) utilising an IMSdetector. Indications of TNT were reported on the copper wire, sections of the fabric and alsofrom swabs collected from the head of the suspected suicide bomber. These results werereported to investigators the same day of collection. The samples were subsequently prioritisedfor analysis back in the central laboratory in Canberra, Australia. The swabs were treated asexhibits from the time of collection and their continuity maintained. The results for TNT wereconfirmed utilising ion mobility spectrometry (IMS), gas chromatography–chemiluminescence(GC/CL) and gas chromatography–mass spectrometry with negative chemical ionisation(GC/nci-MS) within two weeks of collection. Positive results for TNT were obtained on onlyfive of the hundreds of samples analysed in relation to the Paddy’s Bar explosion.

[84.2160] Device reconstruction

Based on the interpretation of the scene, the recovered evidence and laboratory analyses thefollowing 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] Identification material

Connective tissue and spatter marks were visible on the ceiling above where the device wasbelieved to have been detonated. Samples were collected for DNA analysis to identify peoplesitting around a table (area of interest) and possibly interview those people (if alive). Theresults demonstrated that the material had originated from one individual which led to theinitial suspicion of a suicide bomber. The DNA profile from the spatter was compared to theDNA profile from two lower legs and a head being examined in the morgue. The DNA profilesfrom the spatter, limbs and head matched. The DNA profile was compared to a database inorder to seek the person’s parents and confirm his/her identify.

No fingerprints 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 popularbar/nightclub. The large vehicle borne device exploded outside of this club following thedetonation of the first device inside Paddy’s Bar across the road.

[84.2190] Scene interpretation

Whilst a fire had burnt the majority of the Sari Club (in part due to the highly flammablematerials, including a thatched palm leaf roof) and the vehicles out the front were significantlydamaged, the seat of the blast was identified by the large crater on the roadside. Pieces of metal



were recovered that had originated from a vehicle that appeared to have been close to orcontaining the device at time of initiation. Due to the size (approximately 3–4 metres wide and0.5–1.0 metres deep) and location of the crater and the significantly damaged vehicle parts, thedevice was identified as probably being a large vehicle borne device. The damage in closeproximity to the crater indicated a possible high explosive; however, the longer range damage,crater and subsequent fire 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 thelocal mortuary. The majority of the human remains exhibited evidence of incineration andadvanced 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 largejoints (hip, knee and shoulder) were recovered. Long bone shafts were often broken in themid-shaft region. Feet and lower legs frequently exhibited thermal damage.

The body parts were described, photographed and DNA samples were taken, when the remainswere considered viable, as part of the DVI process (see Identification Material).

[84.2200] Physical evidence

The Sari Club scene examination involved the massive crater and its surrounds. Surroundingthe crater were vehicles and twisted bits of metal. The metal and vehicles were examined todetermine their approximate proximity to the device at time of initiation. A chassis rail thatappeared to have been in close proximity to the device was examined for chassis and enginenumbers. These numbers had been filed away; however, serial number restoration procedureswere employed by the INP to recover the chassis number. In addition, and more clearly, aroutine vehicle inspection number (a DPR number – Denpasar number for passenger-carryingvehicles) had been stamped on the chassis rail and had not been filed down. This number wasthe breakthrough for the INP in tracing the vehicle back to the responsible terrorists (Royds etal, 2005). No other primary fragmentation was recovered during the search. This is most likelydue to the fire destroying fragments and fragments being washed away during the firefighting/burst water main.

[84.2210] Explosive residue analysis

Swabs for explosive residue analysis were collected from cracks in the bitumen around thecrater 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 theeffects of the fire, fire fighting response and the heavy throughput of people during the rescueand recovery phase. Samples of water were also collected from the water in the crater in caseany remaining residues had dissolved in this medium.

Of the swabs analysed in country, no positive results were obtained. Despite this, the solventswabs were sent back to Canberra for analysis. Prioritised samples were independentlyanalysed by two additional laboratories. Due to the size of the crater, it was believed that animprovised explosive mixture had been utilised, as it is generally not likely that the requiredamount of high explosive (to produce such a crater size) would be utilised primarily due toavailability. Laboratory analysis resulted in the identification of chlorate ions in six of thehundreds of samples analysed in relation to the Sari Club bombing. The presence of chloratewas confirmed in water extractions utilising both ion chromatography (IC) and capillaryelectrophoresis (CE) techniques. Chlorate was confirmed on swabs/extracts collected from inand around the crater and elevated surfaces of lamp posts. The early recovery and preservationof the samples allowed this relatively reactive ion to be recovered and identified. Elevatedlevels of chloride and potassium ions were also identified on the swabs. Chlorate and chloridewere not identified in the temporary laboratory in Indonesia as the IMS technique can not



detect chlorates, combined with the fact that it was only present on a very small proportion ofthe swabs. Scanning electron microscopy/energy dispersive x-ray detection (SEM/EDX) wasalso utilised to identify the presence of chloride and potassium on a number of metal streetsigns.

In order to determine the significance of the identification of chlorate and elevated levels ofchloride ions, swabs were collected from surfaces in adjacent streets to determine whetherchlorate and chloride were common to the environment, and if so, at what concentration/level.Chlorate was not identified in the surrounding environment and only trace levels of chloridewere detected, thus assisting the chemists in determining whether the chlorate and chloridewere 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 devicereconstruction based on scene examination and laboratory analysis consisted of:

1. Initiation device: unknown

2. Explosive: chlorate based improvised mixture

3. Container: vehicle

[84.2230] Identification material

The identification of the suicide bomber in relation to the Sari Club bombing was madeutilising DNA from recovered body parts at the scene. These parts were collected as part of theDVI process, which highlights the importance of the DVI process in also potentiallyidentifying suicide bombers.

Secondary scenes

[84.2240] As the police investigation progressed, vehicles and premises of interest wereidentified. The post-blast scene examiners and chemists were tasked with processing over 25secondary scenes over the next 6 months. Approximately four months after the blasts, a teamof scientists were called to an address. Like all the others, the premises were clean and did notshow any visible signs of device construction or explosive manufacturing. Despite this, thesame protocols of wearing protective clothing and collecting control samples from all membersentering were conducted. Royds et al (2005) refer to the successful processing of this particularaddress. It was here that two pieces of evidence that were vital in connecting the premises tothe bombings were recovered. This evidence included: two particles of explosive mixture (eachless than 1 mm in diameter) recovered by the examiner through the vacuuming of the floor.These particles consisted of potassium chlorate, aluminium and sulphur and were onlyrecovered after days of searching the collected debris under a microscope. The potassiumchlorate was confirmed utilising Fourier transform infrared spectroscopy (FTIR), and thealuminium and sulphur confirmed utilising SEM/EDX and XRF. PETN, TNT, and tetryl wereconfirmed in solvent extractions from the floor vacummings and also solvent swabs fromsurfaces in the premises. These were confirmed utilising GC/CL and GC/nci-MS. Chlorate andchloride 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 thebombers on a newspaper in the house, hence linking the bomber to the premises.



Other aspects

[84.2250] Another aspect to the post-blast investigation that was occurring in Australiaduring the initial stages was the collection of clothing of victims and witnesses who werereturning to Australia. The clothing was collected from people at airports and hospitals forexplosive residue analysis in the central laboratory in Canberra, Australia. TNT was detectedon the clothing from six people before samples were collected from the primary scene forforensic analysis. The timely preliminary results were quickly fed back to the investigators incountry.

In response to the bombings, two forensic chemists were deployed to Bali to work as part ofthe post-blast examination team. Whilst the chemists assisted with scene examinations andcollected samples for explosive residue analysis, the major successes of the chemists were inrelation to the analysis of samples in a temporary laboratory that was established in a localhotel room in close proximity to the investigation forward command post. The laboratory wasutilised for approximately three months to analyse samples from both the primary andsecondary scenes. A microscope, a range of chemical colour tests, and portable IMS and IRequipment were utilised for the analysis of samples.

Prior to utilising the laboratory for examining items, the room was cleaned and control sampleswere taken from the various surfaces in the room (including: tiled floor, benches, chairs,phones and light switches). These samples were analysed utilising an IMS that was operatingin the room and solvent swabs were also collected for future laboratory analysis. Membersentering the room were required to don protective clothing at the front door and collect acontrol sample from themselves prior to commencing examinations.

Portable instruments were utilised to screen and prioritise the approximately 2000 exhibits thatwere submitted to the AFP’s central laboratory in Canberra, Australia. High priority sampleswere also analysed by two independent laboratories (one in Australia and one overseas). Dueto the effective prioritisation of samples utilising the temporary laboratory in Bali,confirmatory results from the central laboratory in Australia became available within twoweeks of the bombing. For completeness, the full examination of all the exhibits took over fivemonths, 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. Somehave 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 ofinformation from confessions from the accused and the results from the forensic investigation:

1. Paddy’s 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 linedblack vest



e) position – between 80-120 cm above the floor 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 lowordered

d) container – 12 four-drawer plastic filing cabinets (containing main explosivecharge) connected by detonating cord (PETN) in the back of a whiteMitsubishi L300 van

e) position – roadside, outside Sari Club

f) initiation – command: suicide bomber. There was also evidence of back-upremote 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 UnitedStates of America Consulate

f) initiation – remotely by mobile phone

Acknowledgments

[84.2280] The authors wish to acknowledge the efforts of all those who worked tirelesslyon the Bali bombing investigation (2002), in particular the INP and the Australian forensicscientists and investigators. The authors also wish to thank Dr Alanah Buck and Dr Clive Cookfor their contribution to the Pathology Section at [84.1325].




APPENDIX A: ANALYTICAL TECHNIQUES FORTHE ANALYSIS OF EXPLOSIVES

[84.2310] Instruments utilised in laboratories performing explosive residue analysis arebriefly discussed in this appendix. Literature references providing further detailed descriptionsof each technique are provided.

The classical non-instrumental methods of analysis are chemical colour tests (“spot tests”) andTLC. These, along with IR and XRPD were the principal methods of the 1970s, and remaineffective for the identification of bulk samples (Beveridge et al, 1975). However, theapplication and interpretation of the results of TLC analyses and colour tests were amongseveral issues raised in challenges in the United Kingdom Court of Appeal in the late 1980sand early 1990s to some convictions in bombings in the United Kingdom attributed to the IrishRepublican Army in the mid-1970s. Several convictions were overturned (Schurr, 1993;Scaplehorn, 1993) and a judicial enquiry was held (May, 1992). In consequence, explosivesanalysis 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 ofAmerica (USDOJ/OIG Special Report, 1997). This report also resulted in significant changesin quality assurance and both laboratories involved in these reviews have long since beenrecognised as world leaders.

Several advances in instrumentation applications were made through the 1980s and into the1990s such as routine application of GC, HPLC, IC, MS and SEM/EDX for the analysis ofexplosives. These methods significantly improved detection limits for the detection andidentification of trace explosive residues (Beveridge, 1992; Yinon and Zitrin, 1993). The turnof the century (2000) saw a strong focus on the miniaturisation of traditional laboratory-basedanalytical techniques to allow for on-site (field) rapid screening and analysis of samples.

A brief description of each technique is provided, along with references containing in-depthdiscussions and information for readers who wish for more detail. Research and developmentis on-going in relation to the application and/or development of new techniques for the analysisof explosives. Whilst some of the research is touched on, this section does not address new andemerging techniques for the analysis of explosives – rather it is limited to published literatureup to early-2013.

Non instrumental techniques – Chemical colour tests (spot tests) andthin layer chromatography

[84.2320] Chemical spot tests or colour tests involve either applying chemical reagents tosamples of explosive or burning them and observing the colour produced. The first scheme forthe systematic analysis of explosives was based on spot tests (Amas and Yallop, 1966 and1969). Many of the tests were not specific and most have been replaced by more definitiveinstrumental analyses.

The value and limitations of the “Griess” test for nitrate esters, and other spot tests used in theBirmingham Six Pub Bombing Case in the United Kingdom have been critiqued (Scaplehorn,


1993). In particular, although nitroglycerine does give a positive Griess test, the test is notspecific for nitroglycerine whereby other nitrate esters such as nitrocellulose and PETN reactsimilarly.

If there is sufficient residual material to be examined for explosive residue, colour testing stillcan be a useful screening method. If sample size is limited, then destructive tests such ascolour tests are generally not utilised. Indeed colour testing is frequently used for screening atexplosives scenes in Israel (Almog, 2006). Royds et al (2005) provide a summary of some ofthe colour tests available for screening explosives.

Thin Layer Chromatography (TLC) involves a solution of explosive or residue being spottedonto a thin layer of silica gel or alumina on a plate. The plate is placed into a solvent mixturein a tank. The solvent migrates through the layer carrying the components of the explosivesample with it. With appropriate solvent selection, components of the sample migrate atdifferent rates, and can be visualised as coloured spots by exposure to specific chemicalreagents sprayed onto the plate (Doyle 2012, Ch 13 pp. 554-557; McCord et al, 2012, Ch 14pp. 601-603).

It is standard practice to analyse known explosives on the same plate as unknown samples inorder to compare the retention factor (Rf: the ratio of the distance travelled by the componentto 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).Confirmation acceptable to the courts is normally achieved by instrumental analysis such asGC/MS (described below) (Zitrin, 1986). Sharma (2005) discuss research utilising a range oftechniques, including TLC, for the characterisation and identification of explosives and theirresidues.

Quality issues pertaining to TLC, namely: contamination, reference standards, interpretationand 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 identification of organic explosives, including TLC, GC,HPLC, IC and CE techniques. Each of these techniques (except TLC) involves the injection ofa sample onto a column and the use of the retention time (ie time taken to pass through thecolumn) 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 theGC. The injection port needs to be hot enough to immediately vaporise the sample. The sampleis 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 splitmode in which only part of the sample goes onto the column, the remainder being vented tothe atmosphere. Split injections can be used in situations where the sample is too large orconcentrated to run through the column.

The gas mobile phase flows from a source past the injector and carries the injected mixturethrough a long capillary column whose inside walls are thinly coated with a waxy stationaryphase. The components of the mixture separate and elute one after another from the end of thecolumn.



The movement of mixture components along the column will depend on their volatilities andinteraction with the stationary phase. The stronger the affinity (attraction) the components havewith the particular stationary phase, the more time they will spend on the column and hencethe longer the retention time. This is a major factor controlling the rate of movement of asubstance through a column.

Because volatility is such an important factor in GC, the chromatographic column is containedin an oven. For very volatile compounds the oven may be operated at 30-40°C; for relativelynon-volatile substances, temperatures of 200-350°C may be needed. For GC analysis, thecolumn may be operated at one fixed temperature (isothermally) or over a temperature range(temperature programming).

Detected components are recorded as peaks on a plot (the gas chromatogram). The area of eachpeak corresponds to the amount/quantity of the represented component. The time it takes thecomponents to pass through the column indicates the identity of the component. The time atwhich the peak maximum occurs is referred to as the retention time; different compounds havecharacteristic retention times which can be used to assist in identification. Components cannotbe identified solely by GC, hence the need for combined techniques such as GC/MS to confirmthe identity of substances.

The analytical column inside the GC oven provides the sample separation. Whilst a wide rangeof analytical columns are available (eg, of varying length, width and stationary phase) forensiclaboratories tend to select an analytical column that will suit the range of materials that theyroutinely analyse. A common column type may consist of a capillary column, 15 or 30 metresin length, with a non-polar to medium polarity stationary phase. Selection of a stationary phaseshould generally be based on the polarity of the sample. A very general rule is like dissolveslike. Column polarity has the greatest effect on how the column separates the compounds ofinterest as the sample interacts with the stationary phase. A polar component (eg, an alcoholsuch 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-polarstationary phases.

The inside diameter of the capillary column has an effect on the column’s resolving power andits capacity or concentration range. In general, the larger the inside diameter of the column, thelarger the sample capacity is. However, the larger the inside diameter, the lower the resolutionis and the higher the flow rate necessary to achieve good performance.

The phase or film thickness will primarily affect the retentive character and the capacity of thecolumn. Increasing the film thickness will cause an increase in the retention of the compoundsbeing analysed. Thick film columns are primarily used for extremely volatile compounds. Thethicker phases will retain components longer, allowing them to interact longer with thestationary phase, thereby increasing the separation of closely eluting compounds.

The effect of the column length on a separation becomes less important as column lengthincreases. Resolution is a function of the square root of the column length. For example if youwant to double the separation between two peaks without changing the stationary phase, insidediameter, film thickness or GC conditions, it would take a four-fold increase in the columnlength. 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 variousdetectors, including those described below. Yinon (1999) provides an overview of the theory ofoperation of GC/ECD, GC/FID, GC/CL and GC/MS instruments. Tebbett (1992) also providesa discussion of gas chromatography in forensic science.

APPENDIX A: ANALYTICAL TECHNIQUES FOR THE ANALYSIS OF EXPLOSIVES [84.2350]


[84.2360] Flame ionisation detectors (FID)

Components emerging from the GC column are burned continuously in the flame of the FIDafter being mixed with hydrogen and air. Ions and electrons formed when emerging organicsburn in the flame are detected electronically. The flow of current is monitored, amplified andpassed to the recording system.

This detector is insensitive to non-combustible gases such as H2O, CO2, SO2 and NOX. Theflame 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 iswidely used for GC analysis of compounds such as gasoline, but it is not selective forexplosives. As the detector is not specific for explosives, it is often difficult to identify thepresence of explosive compounds in samples containing complex mixtures. As a result,selective detectors (such as MS) are often preferred. FID was superseded firstly by ECD andlater by CL and MS detectors. However, the increasing market share of slurry and emulsionexplosives, 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 waxeswhereas 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 significantelectrophilic substituents (eg, halogens) enter the gap, they capture electrons resulting in adecrease in the current in the electrode gap. This change in current is amplified and results inthe representation of a peak. The ECD has better sensitivity than the FID for electrophiliccompounds (including organic explosive compounds containing nitro-groups), and very poorsensitivity for other components, permitting the selective detection of electrophilic components.The ECD is a valuable back-up for explosive residue identification; however it is importantthat the detector is only exposed to very clean samples as it is easily contaminated. In routineanalyses of “real world” explosive residue samples, ECD largely has been replaced by CL orMS 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 asensitivity similar to the ECD (Douse, 1983; Fine et al, 1984). Nitro- or nitroso-compounds arebroken down by heat to form nitrogen monoxide (NO) by catalytic action. The NO isconverted by reaction with ozone to form excited NO2, which emits light in a specificwavelength range in the infrared spectrum. The detector contains a filter which allows onlylight of this narrow wavelength range to pass and produce a signal. Thus, only compoundswith -NO or -NO2 should respond. Because it is based on light emission, the technique isreferred to as chemiluminescent detection. A commercially available CL detector is theThermal Energy Analyser (TEA®).

The GC/CL (GC/TEA®) combination is a useful screening technique for nitrated organicexplosives due it its selective nature for these types of compounds; however, it does not detectemulsion explosives, ANFO or peroxide explosives. The TEA® detector’s selective lack ofresponse to co-extracted compounds which are not nitrated is its major advantage over the FIDand ECD due to the production of chromatograms with few interfering peaks and flatbaselines. This same selectivity can also be considered a disadvantage as it is unable to detectnon-nitrated explosive compounds. A field portable version of GC/CL is available under theproprietary name of EGIS®.



[84.2390] Mass spectrometers (MS)

GC/MS used for the identification of explosives has been extensively reviewed by Yinon(1991). Yinon and Zitrin (1981 and 1993) have described the basic techniques in their twobooks on the analysis of explosives. Application of GC/MS to explosive residue analysis hasbeen further discussed by Zitrin (1986), Tamiri and Zitrin (1986), Tamiri et al (1993), Sigmanet al (2001), Calderara et al (2004), Perr et al (2005), Sharma et al (2005) and Tamiri andZitrin 2012, Ch 15.

Yinon (1999) and Tamiri and Zitrin (2012, Ch 15) provide an overview of the identification ofexplosives utilising MS. Yinon (1999) also provides an overview of the principles of operationof the different types of MS detectors, including: magnetic sector; time-of-flight (TOF);quadrupole; ion trap; and tandem MS/MS. New applications of MS enhancing the detectionand identification of explosives are constantly under development, for example techniques suchas GC/MS/MS offer improved selectivity for the identification of target compounds,particularly when co-eluting compounds mask the compounds of interest (Yinon, 2003; Perr etal, 2005; Collin et al, 2009). Desorption electrospray ionization (DESI) is another MSionisation technique for the detection and identification 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 ionsource of the mass spectrometer. The components are normally ionised either by an electronbeam (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 bythe analyser part of the mass spectrometer, generally a quadrupole. The quadrupole useselectric fields to separate ions according to mass-to-charge ratios (m/z). These molecular andfragment ions compose the mass spectrum.

[NB: An ion of mass (m) having a single positive charge (z = 1) has a mass-to-charge ratio ofm/z = m/1 = m.]

The mass spectrometer scans continuously over a mass range. As the mixture is injected ontothe 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 anotherright throughout the chromatogram and hundreds of mass spectra may be recorded in a routineGC/MS run.

The computer adds up all the ion peaks in each mass spectrum to give a total ion current forthe mass spectrum. These total ion currents are plotted along a x-axis (time for elution) and ay-axis (amount of total ion current) to give a total ion current chromatogram (TIC) showing theelution of all the components of a mixture. If reference materials are available, then the TICcan be examined at a particular retention time and the mass spectrum of the peak of interestobtained for comparison. An alternative is to conduct extracted ion monitoring (EIM) from theTIC to highlight the presence or absence of compounds of interest by extracting the knownions relating to the compound of interest. This results in a chromatogram containing peaksrepresenting 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 identifythe component either through the skill/experience of the scientist or by comparison to referencespectra either stored in an existing spectral database or obtained as a result of the analysis of areference material.

A library of spectra, such as that published by the National Institute of Standards andTechnology (NIST) assembled from an archive of >80,000 mass spectra, can be utilised toidentify peaks of interest. The computer uses search software to provide a shortlist of the bestmatches between the library spectra and the one measured.



Selected ion monitoring

Selected Ion Monitoring (SIM) is a technique that can significantly increase the detectablelevels of organic compounds by looking at very specific masses only. This results insensitivities that are 100x greater than levels attainable in Full Scan (TIC) mode, where the MSscans over an entire mass range. The disadvantage of SIM is that the entire mass spectral dataare not available.

When setting up a method for SIM, ions must be chosen for the analytes of interest. Thefollowing 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 mayco-elute; and

• sensitivities are greater when fewer ions are selected, however more ions allow for anincreased specificity.

Electron ionisation (EI)

The EI ion source works on the principle of electron ionisation, whereby a heated filamentproduces a beam of electrons. The high energy electrons interact with the vaporised samplemolecules eluting from the GC column. The molecules are fragmented into ions characteristicof the original molecule as a result of this interaction. The ions are measured by the m/zanalyser.

Chemical ionisation (CI)

Chemical Ionisation (CI) uses an inner ionisation source different from that of ElectronIonisation (EI).

When a reagent gas such as methane or ammonia is introduced into the ion chamber of thesource, it is bombarded with the electron beam, thereby producing reagent gas ions. Byproducing a higher source pressure (than EI) in the CI ion chamber, reactions occur betweenthe neutral analyte and ions of the reagent gas. The reaction can involve a transfer of anelectron, proton, or other charged species.

In Positive CI mode, usually the positive sample ions are detected, eg, MH+; in Negative CImode, negative ions are detected, eg, M-.

Negative CI involves the capture of an electron by an electronegative sample, such as ahalogenated or oxygenated compound, to produce M- ions. A gas is required in the ionisationsource 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 “moregentle” than direct electron impact. This has the advantage over EI of producing fewerfragment ions, in a simpler pattern, and usually results in a “molecular ion”. This permits themolecular weight of the molecule, and hence its probable identity to be determined. CI is thussometimes the favoured method of ionisation for nitrated organic molecules. The ionisationmay 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 quasimolecularions and few fragment ions. It is advantageous to run both CI and EI spectra on the samecompound to obtain complementary information.



High performance liquid chromatography (HPLC)

[84.2420] Various scientific literature provide overviews of the analysis of organicexplosives using LC (Minet et al, 2001; Xu et al, 2004a and 2004b; Paull et al, 2004; Mathisand McCord, 2005b; Gaurav et al, 2007a and 2007b; Oehrle, 2008; Song and Bartness, 2009and Zitrin and Tamiri, 2012 Ch 15). The field has also been reviewed in depth by Lloyd(1991). Yinon (2003) provides a comprehensive overview of the analysis of explosives byLC/MS, including theory of operation of electrospray ionisation (ESI) and atmosphericpressure chemical ionisation (APCI).

HPLC: Partition chromatography

[84.2430] The solute (dissolved explosive) is injected onto the analytical column where itis divided (partitioned) between two immiscible liquid phases, one stationary (the columnpacking) and one mobile (pumped through the column). The amount of solute which dissolvesin the two liquid phases depends on the chemical nature of the phases and the solute. If thenature of the solute is known, the composition and polarity of the phases can beselected/adjusted to optimise separation.

If the composition of the mobile phase (eluent) remains unchanged throughout the analysis, theprocedure is called “isocratic” elution. If the composition of the mobile phase is varied, theprocedure is called “gradient” elution. HPLC is conducted at a fixed temperature (usually closeto room temperature).

The separation procedure is called “normal phase” or “reversed phase” depending on therelative polarity of the liquid phases:

(1) Normal phase chromatography: the stationary phase is polar and the mobile phase isnon-polar.

(2) Reversed phase chromatography: the stationary phase is non-polar and the mobilephase is polar.

Liquid chromatography has two advantages over GC: analysis at a fixed low temperaturewhich minimises thermal decomposition (which is important for energetic compounds), andthe ability to separate high molecular weight compounds which cannot be separated by GC. Adisadvantage is that HPLC typically requires some 20 times more sample and often exhibitsless resolution.

Detectors

[84.2440] Detectors used for HPLC analysis of explosives include: UV, CL (TEA®), andMS.

(1) UV detector

A UV detector detects the reduction of intensity of the UV light as the light is absorbed by themolecules passing through. A UV detector is quite sensitive, and is effective with analysis ofrelatively pure samples. A diode array UV detector also records the UV spectrum whichcomplements the chromatography retention time data (Paull et al, 2004). The lack of selectivitycan 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 ofmonitoring the effectiveness of clean-up procedures.



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 istrapped out in a “cold trap” placed before the detector. Since water would form ice and blockthe system, the CL detector cannot be used for aqueous reversed phase systems (Fine et al,1984). The selectivity of the detector is a significant advantage over the UV detector fordetection of explosive residues.

(3) MS detector

The use of MS with LC provides a very stable and suitable system for analysis of explosivesresidues. Developments in HPLC/MS and HPLC MS/MS technology in the 2000s are makingthese techniques methods of choice in laboratories specialising in explosives analysis (Yinonand Zhao, 2001; Xu et al, 2004a and 2004b).

Ion chromatography (IC)

[84.2500] Ion chromatography is very widely used in protocols for analysis of inorganicexplosives 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 aqueousextracts. An advantage over evaporation techniques is that it detects ions such as ammoniumand 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 ionexchange column. The column packing contains charged groups and the mobile phase containsoppositely charged species which associate with the column packing. When a sample is passedthrough the column, neutral molecules and ions with the same charge as the column packingpass 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. Weaklyassociated ions pass through the column more rapidly than strongly associated ions andseparation is thus achieved. As the ions leave the column, they are detected by a conductivitydetector. This detector generates a series of chromatographic peaks corresponding to thedifferent times in which components of the analyte mixture emerge from the column. Theconcentration of the ion is proportional to the response from the detector, and the associatedchromatographic peak area.

Chemically suppressed IC (conductivity detection)

In chemical suppression, a second column removes highly conducting ions from the mobilephase 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 themobile phase from a highly conducting solution of base to a weakly conducting solution ofacid. Conversely, separated sample anions (negative ions eg, nitrate) are converted to highlyconducting strong acids which are readily detected by conductivity. That is, optimal conditionsfor detection are established by highly conducting sample ions in a weakly conducting mobilephase. Anions which do not form strong acids by this process are difficult to detect by thismethod. 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 ishigher and hence sensitivity is lower than suppressed IC.



UV detection

Many inorganic ions absorb in the UV range and thus can be detected. A UV detector iseffective for several ions found in explosives (Skelly, 1982).






Electrophoresis: Capillary electrophoresis (CE)

[84.2510] Capillary electrophoresis is frequently utilised as a complementary techniquefor IC. CE involves separating charged species on the basis of ion conductance (movement)created by an applied electric field (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 inforensic science, including for the analysis of explosives. Pumera (2008, 2006) provides anoverview of research in the field of microchip and conventional CE for analysis of explosives.Hutchinson et al (2007) discuss the identification of inorganic improvised explosive mixturesby analysis of post-blast residues using a portable CE. Lewis et al, 2013 also provide a reviewon the development of portable CE systems.Capillary zone electrophoresis (CZE), otherwisereferred to as capillary electrophoresis (CE), involves the separation of ions of interest (eitheranions such as nitrate and chlorates or cations such as ammonium or potassium) using acapillary column filled with a buffer solution. The application of a voltage to the columnresults in the movement of the ions. This movement is referred to as the electro-osmotic flow(EOF). The movement results in the separation of the ions. The speed at which an ion willmove 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 CEknown as Micellar Electrokinetic Chromatography (MEKC), where a surfactant (detergent-likesolution) is added to the buffer to form micelles (spherical arrangement of molecules in anaqueous solution). Neutral compounds interact with the micelles and a partition is set upbetween the buffer and the micelle. Different neutral species will spend different amounts oftime in the micelle and the buffer, resulting in separation.

Detection of analytes after CE separation is usually through the use of a diode array. Othertypes of detectors that can be utilised include mass spectrometry, conductivity andamperemetry.






Spectrometry

[84.2520] Three techniques for explosives analysis that operate based on the principle ofspectrometry are addressed in this section, namely: mass spectrometry, ion mobilityspectrometry and isotope ratio mass spectrometry.

Mass spectrometry (MS)

[84.2530] Refer to [84.1410] for details on mass spectrometers and their application to theanalysis of explosives.

Ion mobility spectrometry (IMS)

[84.2540] IMS is a widely used screening technique for a range of organic explosives andthe inorganic nitrate ion. It is very fast and sensitive, but is prone to contamination by dirtysamples. An object to be screened is swabbed and the swab inserted into the instrument whereit is heated to volatilise any explosive traces. If present, they are carried into a chamber wherethey are ionised by a radioactive source and carried into a column where they are separated ina drift tube under the effect of a weak electrical field. The ions are separated based on their ionmass, size and shape and detected in the sequence of their mobility. The principles underlyingthe operation of the IMS technique have been reviewed in detail by Ewing et al (2001).

IMS is the most widely used technology for the field detection of trace levels of explosives andother contraband materials (Eiceman and Stone, 2004). Keller et al (2006) discuss theapplication of IMS for the analysis of post-blast samples. Yinon (1999) also discusses theapplication of IMS for the detection of explosives.

IMS analysers can detect and identify trace amounts of up to fifty explosives (Ewing et al,2001); however, only a limited number can be programmed into the detection algorithm at anygiven 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 todetect these organic explosives, the technique cannot be utilised for the analysis of typicalinorganic oxidiser/fuel type explosive mixtures including chlorate and perchlorate basedmixtures. The technique can be optimised for the detection of other types of explosives, suchas TATP (Moore, 2004); however, this often decreases the sensitivity of the technique to theother compounds of interest. Various sampling and pre-concentration devices can also be usedfor 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 spectrometersthat produce precise and accurate measurements of variations in the natural isotopic abundanceof light stable isotopes. Isotopes are atoms of an element that differ in the number of neutronspresent 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: 13C and12C, not 14C), oxygen (isotopes: 16O, 17O, and 18O), hydrogen (isotopes: 1H, 2H, but not 3H),nitrogen (isotopes: 14N and 15N) and sulphur (isotopes: 32S, 33S, 34S, and 36S). Chlorine (Cl),Silicon (Si) and Selenium (Se) isotopes are less frequently analysed.

Two of the main characteristics differentiating IRMS instruments from conventional organicmass spectrometers previously discussed are:



1 sample peaks are converted to a representative analyte gas (eg, CO2 for carbon, N2 fornitrogen, CO for oxygen and H2 for hydrogen) following elution from a GC columnas opposed to passing directly to a MS detector; and

2 they do not scan a mass range for characteristic fragment ions in order to providestructural information on the sample being analysed (Meier-Augenstein, 1999),instead they have a magnetic sector field MS with high sensitivity which collects therespective 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 thisappendix, it is generally not possible to distinguish one source of the same explosive fromanother. IRMS shows the potential to be able to distinguish one source of the same explosivefrom another due to the use of different starting materials, manufacturing processes, storageconditions 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 andMeier-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 theforensic applications of IRMS, including for the analysis of explosives.




Spectroscopy

[84.2560] Primary spectroscopic methods utilised for the analysis of organic andinorganic explosives are infrared and Raman. Additional spectroscopic techniques are utilisedfor the elemental analysis of explosives and these are addressed at [84.2590].

Infrared spectroscopy (IR)

[84.2570] IR is an excellent method for the identification of relatively pure components ofexplosives and their residues. IR is primarily utilised for the analysis and identification ofintact particles of organic or inorganic explosives. During the analysis of a sample, IR light ispassed through the sample. This light is in the same energy range as molecular vibrations,hence some of the light is absorbed at specific wavelengths as determined by the arrangementof 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 materialsstored in a database to identify the compound.

Two types of instrument are in common use, with the older “dispersive” instruments nowgiving 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 specific wavelengths of the infrared radiation are absorbed by the chemical bonds of thesubstance. The wavelengths of IR radiation absorbed are indicative for a particular chemicalbond and its immediate chemical environment. Infrared spectroscopy is a non-destructivetechnique.

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) andTamiri and Zitrin (2012, Ch 15). Smith (1996) and Banas et al (2009) also are useful referencesfor the operation of the technique.

Raman spectroscopy

[84.2580] Raman spectroscopy is an instrumental technique that analyses the bonds withina substance, either organic or inorganic in nature (solid, liquid or gas), to provide informationabout its chemical composition. Raman spectroscopy involves illuminating a sample withintense monochromatic light, and analysing the change in frequency of the scattered light togive a Raman spectrum of the sample. The particular combination of the bands present in theRaman spectrum of the unknown sample is used for its identification by means of comparisonwith characteristic band patterns of reference materials stored in a database. Raman spectra canbe obtained non-invasively through transparent/translucent barriers such as plastics, glass,polymer laminates and protective clearcoats on paint. This non-invasive sampling is importantespecially in the analysis of sealed, potentially dangerous unknown substances such as thoseretrieved 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 Ramantechnique. Pitt et al (2005) discuss advances in the application of new Raman instrumentation,including Raman-near field optical systems and Raman-SEM combinations. One of the areasdiscussed 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 Ramaninstruments. Ali et al (2009a and 2009b) discuss the use of confocal Raman microscopy for thein-situ detection of explosive particles on clothing (including particles of PETN, TNT andAN). Eliasson et al (2007, 2008) discuss the detection of concealed sugar and hydrogen



peroxide solutions utilising spatially offset Raman spectroscopy (SORS). Gaft et al (2008)discuss the use of a Raman system for the field detection and identification of small amounts ofexplosives on surfaces up to distances of 30 metres. Lim et al (2007) have applied Ramanspectroscopy to low explosive chemical mixtures. Journal references discussing other Ramanbased techniques include the following: surface-enhanced Raman spectroscopy (SERS)(Wackerbarth et al, 2010; Chou et al, 2012), and stand-off Raman spectroscopy (Zachhuber etal, 2011; Moros et al, 2013).




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 primarytechniques utilised for the analysis of explosives are based on x-ray spectroscopy.

Scanning electron microscopy/energy dispersive x-rayspectroscopy (SEM/EDX or SEM/EDS)

[84.2600] A scanning electron microscope (SEM) is a type of microscope that uses anelectron beam rather than visible light (which is used in an optical microscope) to producehighly resolved, linearly magnified images with large depth of field. The SEM operates byfocusing a beam of high energy electrons on a sample. The point of focus of this electron beamis systematically scanned over the sample. The electrons interact with the sample to produceseveral kinds of measurable emissions, the most commonly analysed emissions beingsecondary electrons (SE), backscattered electrons (BSE), photons (ie light) and x-rays.

The different emission signals are measured by dedicated detectors attached to the SEM. Thex-rays released from the beam-sample interaction are analysed by an energy dispersivespectrometer (EDS) which is used to identify the elements present in the sample as well astheir relative quantities. The technique is most useful for the analysis of bulk orparticulates/crystals of inorganic explosives. SEM/EDX also permits rapid and sensitivedetermination of metal composition. The process is rapid and non-destructive. Thecombination of IR with elemental analysis by SEM/EDX permits identification of manyinorganic components of explosives. Goodhew et al (2001) and Goldstein et al (2003) serve asa good source of information in relation to the theory of operation of SEM/EDX.

Micro x-ray fluorescence spectroscopy (XRF)

[84.2610] During the analysis of a sample utilising x-ray fluorescence spectroscopy(XRF), x-rays generated by an x-ray tube are used to excite the sample. The x-rays knock anelectron out of an inner orbital causing an electron from a higher energy orbital to fall back toa lower energy orbital. Energy is released in the form of an x-ray with a discrete amount ofenergy. This x-ray fluorescence is indicative of the atom from which it was generated. Thus, byusing XRF an elemental profile of the sample can be obtained. X-ray fluorescencespectroscopy (XRF) can be used to analyse bulk explosives or crystalline/particulate inorganicexplosives. XRF also permits rapid and sensitive determination of metal composition. X-raysproduced 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-destructivetechnique. Janssens et al (2001) serves as a useful reference for microscopic x-ray fluorescenceanalysis.

X-ray powder diffraction (XRPD)

[84.2620] XRPD is a traditional method of analysis for crystalline compounds. It is usefulfor the identification of relatively pure substances and has applications both to components ofexplosives and to residues (Beveridge et al, 1975; Yinon and Zitrin, 1981). The sample isground into a powder and placed in an x-ray beam. The crystals cause the beam to diffract intocharacteristic patterns that are related to the structure of the crystal. The patterns can becompared to extensive libraries of standards to assist with identification.



Kotrly (2006) provides an overview of the applications of XRD for the analysis of explosivesand post-blast residues.




Portable explosive detection instruments

[84.2630] Significant advances in the miniaturisation of traditional analyticalinstrumentation for use in the field have been achieved over the last decade. Theseachievements have resulted in the delivery of a new capability for use in the transport security,first responder, law enforcement and military communities for the onsite detection and analysisof threat materials. A range of techniques are commercially available and utilised bylaboratories around the world for on-site screening and analysis of items for explosiveresidues. Techniques include: ion mobility spectrometry (IMS); gas chromatography coupledwith IMS (GC/IMS); gas chromatography coupled with mass spectrometry (GC/MS); gaschromatography coupled with a thermal energy analyser detector (GC/TEA®); gaschromatography coupled with a surface acoustic wave detector (GC/SAW); ion chromatography(IC); CE; FTIR spectroscopy and Raman spectroscopy. Reviews of currently available portableexplosive detection instruments are provided by Hannum and Parmeter (1998), Rhykerd et al(1999), Theisen et al (2005), and McMahon (2007). Applications are discussed and illustratedby Benson et al (2012, Ch 17). See also [84.2250]






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