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Forensic Science International: Synergy 6 (2023) 100298
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Interpol review of the analysis and detection of explosives and
explosives residues
Douglas J. Klapec
a
,
*
, Greg Czarnopys
b
, Julie Pannuto
c
a
Arson and Explosives Section I, United States Department of Justice, Bureau of Alcohol, Tobacco, Firearms and Explosives, Forensic Science Laboratory, 6000
Ammendale Road, Ammendale, MD, 20705, USA
b
Forensic Services, United States Department of Justice, Bureau of Alcohol, Tobacco, Firearms and Explosives, Forensic Science Laboratory, 6000 Ammendale Road,
Ammendale, MD, 20705, USA
c
United States Department of Justice, Bureau of Alcohol, Tobacco, Firearms and Explosives, Forensic Science Laboratory, 6000 Ammendale Road, Ammendale, MD,
20705, USA
1. Introduction and coverage of the literature
The authors would rst recommend that readers review the previous
three review papers from 2013, 2016 and 2019 [22–24]. Those may
have some articles on technology that laboratory managers might nd
useful and adaptable to their current approaches to explosives analysis
and that may be of use in future real-world applications.
The international situation in 2022 is notably different from that in
2019 when the last iteration of this paper was published. There is
considerably less focus on in theater devices and explosives as Allied
Forces have mostly withdrawn from the Middle East and Afghanistan.
Unfortunately, however, because of this withdrawal and the resulting
dearth of human intelligence, people who engage in terrorist activities
are less restrained in securing improvised explosives and precursors.
Additionally, and dangerously, these terrorists now have access to war
material left behind by withdrawing forces, including military grade
explosives and munitions. A re-focused effort on traditional military
high explosive detection and analysis may be needed for laboratories
worldwide if these are deployed in both criminal and terrorist bombings.
Another crisis that may result in concerns for years to come for many
countries is the current war in Ukraine. All wars give rise to the long-
term problem of criminals and terrorists having access to excess muni-
tions and explosives well after the war has come to a close. This was
evident after the wars in Iraq and Afghanistan, but also after the wars
during the breakup of former Yugoslavia. Those munitions and explo-
sives bleed over into neighboring countries impacting the security of the
region.
Beginning in 2020 the United States experienced a substantial in-
crease in incidents of civil unrest. The criminal misuse of explosives and
ignitable liquids was widespread and was recorded from large urban
centers to smaller towns. While some explosives were deployed against
government entities from police ofcers to court houses, some oppor-
tunistic individuals used the cover of riots and protests to engage in
criminal bombings for monetary gain, especially by trying to breach
ATM’s. Almost all of the devices deployed were low explosive pyro-
technic devices and some were modied with shrapnel. Almost all of the
increases in backlogs at our laboratory were from such civil unrest.
As we wrote in the last (2019) paper, “One of the most important yet
difcult areas for the past ten to twenty years for the explosive analyst is
the ever-changing type of explosives employed by the criminal bomber
and terrorists. Restrictions on widely used commercial and military high
explosives are often circumvented by the illicit production of homemade
explosives. While there have been attempts to restrict chemical pre-
cursors and some oxidizers and fuels, criminal and terrorist bombings
are still frequently using homemade explosives. Some of these explosive
formulations are difcult to detect in chaotic and contaminated scenes,
with matrices that are additionally problematic. The two biggest reasons
for failure to identify a post-blast homemade explosive in some of these
cases are the failure to collect samples in a timely manner and the failure
to properly extract the analytes from difcult matrices. While training of
rst responders and others may help with the rst issue, the second issue
falls mostly on the explosives forensic community. There is not a lot of
research in this area, but a few referenced papers do address this second
issue” [24].
Introducing new techniques into the suite of analytical schemes or
standard approaches has become increasingly more laborious as most
laboratories are now accredited, many to ISO 17025. Accreditation
standards demand more data and study before a new technique can be
validated and brought online by a laboratory. This even extends to more
simple transitions like swapping out columns with slightly different
chemistries. Yet many laboratories do not have dedicated analytical
groups to do this kind of validation work. This may add to the hesitancy
of laboratory managers to adopt new techniques. If the new techniques
ll a crucial need or cover a gap in overall explosives coverage those
hesitancies should be put aside and efforts made to complete validations.
This review of the literature will hopefully demonstrate that there
* Corresponding author.
E-mail address: Doug.J.Klapec@usdoj.gov (D.J. Klapec).
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2
are many applications in the world of explosives analysis from many
elds that are of interest to the forensic laboratory manager. The authors
and chemists at the ATF National Laboratory Center have spent hun-
dreds of hours of reviewing and classifying abstracts, reading papers,
and selecting pertinent papers to highlight in this review. Additionally,
hundreds more citations are available in the bibliography. We have
drawn from explosives detection, environmental, academic, and case
study articles to try to cover the range of probable areas of interest.
There are still dozens of references in this area, ranging from theoretical
research to applied systems that are already in eld use.
There are 1004 references in this review. The bibliography portion of
the paper includes numerous references not specically highlighted in
the paper which may be of interest to the reader. It starts on page 23 and
follows the same category structure as the paper. Many of these refer-
ences could fall into two or even three categories. They will not be
presented in multiple places, so it would be advantageous for the reader
to peruse all of the sections. The organization of this paper follows the
same pattern as the previous reviews.
2. Review Articles
This three-year cycle includes several review publications. While
some are broad schemes of analysis, others are reviews of a specic class
of instrumentation or eld of study. Others are self-described as reviews.
Review papers are useful to give a broad overview of advances in
particular aspects or categories of forensic explosive analysis.
Evans-Nguyen, K. and Hutches, K. have a book on The Forensic
Analysis of Fire Debris and Explosives and is a very solid accounting of
the current state in the analysis of explosives [13].
There is a brief but interesting chapter by Wolfgang Greibel on what
end users on the scene of an explosion or bombing have at their disposal
instrument wise and additional techniques which may be used in the
future [15].
Cagan, A. and Oxley, J. have published a comprehensive Second
Edition of Counterterrorism Detection Techniques of Explosives which
covers “updated research ndings that will be used for the next gener-
ation of explosive detection technologies.” including the most currently
employed open-source detection technologies [10]. While many tech-
niques cannot be directly translated or used in a forensic laboratory
because detection has different standards than identication, it is well
worth the time reading.
Forbes, T., Krauss, S., and Gillen, G., have published a very thorough
and interesting review of the challenges of analyzing for trace home-
made fuel-oxidizer mixtures. It is a comprehensive front to back analysis
of the current state of analysis and detection for forensic laboratories
[14].
Crocombe, R.A., Leary, P.E., and Kammrath, B.W., published Volume
One of the technology and instruments used in portable spectroscopy.
This covers a general discussion of XRF, UV–Visible, near-infrared, mid-
infrared, and Raman. In addition to traditional portable spectroscopy
techniques this review also considers LIBS, NMR, and others [11].
In Volume two the above authors show how these instruments are
used in various elds. They also discuss the algorithms for detection,
library and method development, and the future of portable spectros-
copy [11].
Sisco, E., and Forbes, T.P., reviewed the application of DART-MS to a
variety of forensic samples including explosives. In addition to a thor-
ough review of the advances for the last ve years, the authors identied
areas where additional research is needed to continue to advance the
technique [39]. As we write below DART-MS is an increasingly useful
tool in forensic chemistry.
Herweyer, D., et al. reviewed the advancements made in new
“Green” primary energetic materials concentrating on potassium based
energetic salts, metal-free ionic energetic salts and metal-free covalent
energetic materials. The paper summarizes the “explosive performance,
initiability, safety and environmental impact” of several new materials
[18].
Nanoexplosives are another eld where new materials continue to be
developed. While this paper could be placed in novel explosives, nano-
explosive materials have been around long enough to be reviewed by
Yetter, R.A. This review covers how to “… understand how to manipu-
late and build energetic materials at the nanoscale …” [46].
3. Explosive Standards and References, Laboratory Quality
Control, Contamination Prevention
While this category is rather broad, it encompasses many references
that could be highly useful in a forensic laboratory setting. As instru-
mentation becomes more and more sensitive having a framework for
things ranging from engineering controls to standard approaches to
prevent contamination is imperative.
Gareth Collett has published a fantastic report focused primarily on
precursors for Homemade Explosives (HME) including recommenda-
tions for preventative actions that could limit access to the materials. It
also recommends a global repository for HME based IED’s and addi-
tionally links every non war zone HME IED attack with the conrmed or
suspected HME used since 1970 [52]. It should be required reading for
any analyst in the eld.
Schachel, T.D., et al. propose a “pan-European Forensic Substance
Database on Explosives” to include not just the base explosives but more
importantly for sourcing and or brand identication, the additives in
various products. They used a combination of HPLC-HRMS (high reso-
lution mass spectrometry), XRD, and XRF and identied 41 additives
with diagnostic potential [55].
Stein, J., did a thesis at Virginia Commonwealth University looking
at transfers of explosives used in render safe procedures to device
components of simulated IED’s. The author considered specically the
use of a Percussion Actuated Disrupter (PAN) and a water bottle shot
with detonating cord. Transfers were detected [56]. This research
highlights the necessity of communication between the eld and the
laboratory.
ASTM International has published ASTM E2520-21: Standard Practice
for Measuring and Scoring Performance of Trace Chemical Detectors and is a
good resource for assessing the performance of trace explosives de-
tectors that use swabs [49].
Also, ASTM International published ASTM E2677-20: Standard Test
Method for Estimating Limits of Detection in Trace Detectors for Explosives
and Drugs of Interest [50]. This standard may be of interest to labs
establishing limits of detection for new or existing methods.
4. Sampling and Concentration of Explosive Traces
Despite the volume of research done in this category over the past
several years there remain signicant gaps in the eld of sampling and
concentrating explosive samples in the post-blast debris and trace
detection realm. Ease of use and robustness of any given technique are
necessary as is universality. It is the latter, universality, that is hardest to
achieve because there are simply so many classes of explosives and their
post-blast reaction products.
Irlam, R.C., et al. researched seven different sorbents (solid phase
extraction) for recoveries of 14 types of explosives and matrices that ran
the gamut from dirt to cooking oil to wastewater to determine which was
the best for analyte recovery. They found that “With the exception of
river water, the matrix effects were lowest using dual sorbent SPE, with
little/no compromise in recovery.” They report that this approach
resulted in an approximate 10-fold limit of detection over the single
sorbent approach. Finally, they report that Oasis HLB and Isolute ENV +
yielded the best recoveries quantitative wise [68].
Additionally, Irlam, R.C., et al. have applied 3-D printed LEGO ®
inspired miniature blocks for SPE extractions of explosives in a variety of
matrices. It is believed that this is the rst reported use of 3-D printed
SPE blocks. Efciencies of the extractions look promising [67].
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In the area of ion chromatography, Mauricio F.G.M., et al. evaluated
swabs and syringe lters and found that of six syringe lters only two
were free of interfering analytes (such as Na, K, Mg, Ca, Cl and SO4). All
“forensic” swabs had signicant amounts of these as well. They further
analyzed commercially available cotton swabs, cotton balls, and cotton
discs and found these to have similar interferents albeit on a, surpris-
ingly, lower level than the forensic ones. Finally, they report that all
sampling materials can be cleaned of these ions through three washes
[71]. The nature of post-blast analysis of inorganic explosives is such
that these types of ions are often all that remains to be detected.
Therefore, selection of a swabbing material that has minimal interfering
analytes is advantageous and contributes to a stronger conclusion
making this particularly relevant research.
While pertinent to an environmental application, Temple T., et al.
researched four different types of one step extraction processes (stirring,
shaking, sonication and accelerated solvent extraction (ASE)) on ve
different soil types and report that shaking is the most reproducible, but
less efcient than stirring and ASE was the least reproducible. Also, they
report that soils high in organic content (>2%) unsurprisingly affected
both extraction efciency and reproducibility [774].
Rodriquez J., and Almirall, J., demonstrated the efciency in volatile
vapor sampling using continuous capillary microextraction and reported
recoveries of 3.0–89%. By comparison they reported headspace and
simulated open air sampling resulted in less recoveries. The analytes
were 3-NT, 2,4-DNT, DPA, EC, DBP and 2-NDPA, all compounds that can
be found in smokeless powders [74].
Glackin, J.M.E., et al. published an article on coating swabs with a
uoropolymer which was then used to swab an explosive and thermally
desorbed, “… causing the quenching of light emission from a thin lm
luminescent sensor.” They rst tried it with 2,4-DNT and reported an
increase of three orders of magnitude in sensitivity over standard col-
ormetric tests. Then it was used on PETN, RDX, and TNT, and even on
post-blast samples [66].
Evans-Nguyen, K.M., at al reported on employing a solventless,
noncontact electrostatic sampling method for drugs and explosives.
They used a hand-held Van de Graaf generator and wire mesh held close
to the sampling substrate. The particles transferred to the mesh and were
analyzed by thermal desorption electrospray ionization and mass spec-
trometry [62].
Avissar, Y.Y., et al. described using hot water to extract post-blast
samples. Then they conducted a liquid-liquid extraction with a very
small amount of dichloromethane (DCM) before analyzing by GC-MS.
They extracted several different types of substrates (metal, sponge,
asphalt, gravel) and reported that this method leads to notably less
sensitivity loss in the GS-MS after 40 injections than a traditional solvent
extraction This extraction technique has been used successfully on real
life samples [59].
Novosselov, Igor V., et al. completed a study on the recovery of
certain high explosives in the swabbing of various surfaces found in
security (mass transit) settings. They desorbed the analytes in various
ways but found “… nylon had the lowest collection efciency (CE%) for
all cases (appx. 10%) and stainless-steel mesh had the lowest CE% for
the evaluated traps” [72].
5. Identication of explosives, explosive residues and explosive
properties
There are several articles describing the properties of explosives and
theoretical modeling of explosive behavior. Also of interest is the area of
novel explosives and proposed improvements to existing commercial
and military explosives. Some of these articles also describe analytical
techniques.
A. Commercial Explosives
Gao et al. reported on 3-D photopolymerization printing of a CL-20
based propellent with the goal of improve the energy content and
combustion performance of propellants made with additive
manufacturing techniques [106]. It is unknown if 3-D printing on a large
scale will be economically feasible for mass production or more suited
for quick synthesis of new combinations of materials.
Ali, F., et al. report on using waste lubricant oil as a partial substitute
for fuel oil in ANFO formulations. They found that the formulations
exhibited both effective explosive performance and were within the
permissible limit for toxic fumes and particulate formation [78].
Lennert, E., and Bridge, C., used statistical analysis to associate
smokeless powder residues from burned smokeless powder to the orig-
inal smokeless powder using Sorensen-Dice similarity coefcients. The
samples were run on GC/MS. They also explored the pyrolysis products
of the smokeless powder constituents. Their results were mixed, stating,
“The complexity of burning a mixture, such as SP, compared to burning
single components may contribute to the generally low similarity co-
efcients observed in the comparison” [118].
Krejcir, K., Adam, J., and Buldra, R. conducted a multi-temperature
study on the depletion of three common stabilizers used in smokeless
powder over time. The study aims to provide background information
for stability testing of smokeless powders [116].
Wang, Y., et al. explored the usage of different gases in the sensitizing
microballoons in emulsion explosives and reported that the use of
hydrogen gas (as opposed to helium, oxygen and nitrogen) can improve
the power and energy of the emulsion explosive. Oxygen and nitrogen
provide little improvement and helium is both difcult to incorporate
into the explosive system and had a negative inuence on performance
[147].
B. Homemade Explosives
The area of Homemade Explosives (HME) is of tremendous interest
to the forensic explosive’s community. As we stated in our 2019 paper,
“Sometimes called Improvised Explosives (as opposed to an Improvised
Explosive Device that may or may not use HME), these explosives can, in
general terms, be dened as non-factory manufactured explosives. It is
uncommon, but not unheard of, however, that makers of HME will
attempt to make a “commercial” type of explosive” [24].
We additionally wrote, “The actual usage of HME is constantly
changing and it is difcult for forensic laboratories to have adequate
protocols for every possibility” [24]. This axiom still holds true now.
There is no adequate way for a regular forensic laboratory to have every
possibility of HME usage covered in a post-blast situation. Intel and
scene examination can help steer analysis but having the protocols in
place for every eventuality, especially for a novel HME, is nearly
impossible. That said, it can help if analysts keep up with current trends
in HME usage worldwide.
Cory Christopher Pye reports a cautionary tale on the long-term
storage of a consumer bottle of 2-propanol wherein TATP formation
was noted after a dozen years past the expiration date of the product
[172]. Anecdotally, the ATF lab has elded calls where this has been
found to have occurred. Fortunately, these calls are infrequent, but it is a
valuable safety point for hazmat teams in particular to be aware of as
well as for laboratory personnel answering questions from those in the
eld.
Horvath, T., and Ember, I., discuss the use of Raman and FTIR
handheld instruments for on scene identication of HME and highlights
the value of using the technologies in parallel [168].
Stromberg, J. and Castillo Rolon, M. conducted a study on TATP
headspace using quadrapole LC/MS and found TATP was the only
measurable component in the headspace, and it was noted that “the
results of this study strongly suggest the proposal that diacetone alcohol
and acetone are intractable components of TATP’s ‘vapor signature’ is
incorrect” [174].
D’Uva, J., et al. synthesized urea nitrate from a variety of commer-
cially available urea sources and then analyzed the product by FTIR,
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SEM/EDS, and most importantly by ICP-MS where trace elements could
be determined [166]. Although chemometrics and statistical analysis
were not undertaken, this proof-of-concept approach to possibly provide
investigative leads etc., is very promising.
C. Other Explosives including Novel or New Explosives:
Throughout the course of history there has been a desire to develop
new explosives or improve upon existing ones. The experimentation and
development have been towards cheaper, more stable, more energetic,
less energetic, more environmentally friendly, less susceptible to acci-
dental initiation, more simple manufacturing processes, and more t for
immediate purpose, to name some of the objectives. Thousands of ex-
plosives have been designed and tested for decades if not centuries, but
most were rejected as they did not improve upon existing explosives in
the areas listed above. In this section we will include both reported
improvements to existing military or commercial explosives and some
unique explosives.
While not exactly novel, Yang, M., Ma, H., and Shen, Z., proposed
and studied the effects of repurposing decommissioned RDX with
emulsion explosive formulation. They were able to reduce the critical
diameter of the original emulsion [307].
In a similar vein Cui, Q., et al. proposed a novel way of introducing
TNT into porous aluminum powders and were able to simplify the
method of controlling the amount of TNT through a temperature
gradient [191].
Liu, Y., et al. report on a new equation on the theoretical detonation
performance of aluminized RDX [251].
In the area of nanotechnology Van Riet, R., et al. report on lling
nanoporous carbon with an oxidizer. While oxidizer-carbon mixtures
are common, the nanostructure of the carbon is a novel report [282].
Similarly, Ma, X., et al. described improving structural control over
nanoenergetic materials in an overview paper [257]. Once costs are
brought down and scalability makes these products economically
feasible these products will most likely nd their way into the
marketplace.
Li, M., et al. described the production of “photocurable energetic
resin based propellants fabricated by 3D printing [242].
6. Instrumental Analysis of Explosives
A) LC/HPLC/UPLC
As was reported in 2019, “Liquid chromatography (LC), high per-
formance liquid chromatography (HPLC), and ultra-high performance
liquid chromatography (UHPLC) are all excellent separation techniques
and have the advantage of being less destructive to thermally sensitive
high explosives than gas chromatography techniques” [24].
Freye, C.E., et al. researched two types of liquid chromatography for
measuring the aging and degradation of the PBX 9501. First low mo-
lecular weight components of the explosive were measured with HPLC
while the high molecular weight compounds were measured using size
exclusion chromatography (SEC) [332]. The parameters for each can be
found in their paper. These tools may be useful for forensic applications
such as comparisons of PBX explosives.
Steiner, A. and Lurie, I. compiled an overview on using diode array
detectors (DAD) coupled with both HPLC and supercritical uid chro-
matography (SFC) for a variety of analytes including explosives [332].
Veresmortean, C., explored an LCMS method development for eight
selected organic high explosive compounds from wastewater. The
importance of being able to extract and analyze both the original com-
pounds (TNT, RDX, etc.) and their degradation products and optimize
for both was stressed [333].
Freye, C., Nguyen, T., and Tappan, B. used UHPLC-MS/MS to explore
the synthesis impurities due to the manufacturing process of ETN. They
found 12 such impurities and were able to analyze for them [328].
Kotrly, M. et al. reported on using derivatization of aliphatic and
aromatic amines with HPLC-uorescent detection and having
femtomole-level detection [331].
B) Ion Chromatography
The technique of ion chromatography (IC) is often used in forensic
explosives analysis for the analysis of inorganic and some organic ex-
plosives. Many detectors are used including mass spectrometry. Ion
chromatography has the advantage over other inorganic characteriza-
tion methods because a relative prole of many anions or cations in a
sample can be compared against known post-blast proles of certain
explosive types.
Hutchinson, J.P. et al. report on using two techniques for the forensic
analysis of explosives and their post-blast products. Mostly exploring
inorganic low explosives, they looked at using capillary electrophoresis
and ion chromatography as orthogonal techniques, each instrument
with its own pluses and minuses [338].
Gallidabino, M.D. et al. used ion chromatography coupled with high
resolution mass spectrometry (IC-HRMS) and an ethanol-based eluent. It
was interesting that their method did not detect chloride or nitrite. Their
ethanol eluent-based approach was reported to be an improvement over
methods using an aqueous eluent [335].
C) Gas Chromatography
Gas chromatography has been a workhorse for the qualitative ori-
ented forensic chemist for many decades now and remains pertinent to
the examination of many classes of explosives. It provides for quick
separations for a variety of compounds and the methods can be rela-
tively easily modied when required.
Qualley, A., Hughes, G.T., and Rubenstein, M.H. report on a method
of improving the data in eld-portable GS-MS by using the “pre-incor-
poration of isotopic analogues (of the target analytes) onto thermal
desorption tubes in advance of eld distribution …” [346].
Cruse, C. and Goodpaster, J. reported that they optimized various
parameters (inlet temperatures, ow rate, and detector gas pressure) for
a GC/VUV (gas chromatography-vacuum ultraviolet) system for the
examination of several organic high explosives using statistical analysis
called response surface methodology or RSM [343].
M. Li et al. published their work on developing a micro GC with a
micro-photoionization detector which reportedly with sub-picogram
detection limits on trace vapors for optimizing eld GC’s [345].
D) Capillary Electrophoresis
Capillary electrophoresis (CE) is a separation technique that utilizes
charged elds instead of pressure to examine many types of analytes
including explosives. It can be used orthogonally with Ion Chromatog-
raphy or, with a mass spectrometer, as a solo technique.
Krauss, S.T. et al. demonstrated the utility of a wipe based com-
mercial GreyScan ETD-100 capillary electrophoresis for the detection of
several inorganic oxidizers including nitrate, chlorate and perchlorate
and post combustion inorganic ions [351].
Rapid capillary electrophoresis screening and chemical classication
of reworks was reported by Bezemer, K. et al. The Dutch police pro-
vided samples and it should be noted the Dutch civilian use of reworks
is quite common. The detection was indirect UV-detection and the re-
sults showed that chemical classication between primarily homemade
and commercial pyrotechnics was determined by Ca2+and Mg2+cat-
ions [349].
Krauss, S.T., Forbes, T.P., and Jobes D. reported on using gradient
elution moving boundary electrophoresis (GEMBE) as a “robust elec-
trokinetic separation technique” for the separation and detection of
inorganic oxidizers frequently seen in explosives. They stated that ni-
trate, chlorate and perchlorate oxidizers were detected from low
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explosives and that many possible inorganic and organic fuels did not
interfere, and even detected and separated nitrate in post-blast samples
[352].
E) General Spectroscopy: Fluorescence, Luminescence, Spectrophoto-
metric, UV, Chemiluminescence
There are hundreds of research papers and reports in this area. They
are varied in their practical application to forensic and/or security work.
Some could eventually be used in commercial, military, security and law
enforcement applications. Still others will prove to be too costly and are
too focused on one class of explosives or even a single explosive. There
are a few papers the authors wish to highlight.
F) Mass Spectrometry
Mass spectrometry continues to be the most popular technique for
forensic explosives analysis and detection. It could be called the “gold
standard” of post-blast explosives analysis. Even so, it remains heavily
researched for a variety of reasons including sampling optimization,
matrices issues because of the nature of criminal use of explosives, and
the similarity of lighter compounds, especially nitrate esters, that are
harder to positively identify without an orthogonal approach. Soft
ionization is rigorously being examined in many publications. One of the
most researched aspects in mass spectrometry in the last three years has
been in quick sampling and/or screening techniques such as Direct
Analysis in Real Time (DART) or similar sampling methods.
Because canines have shown a propensity to detect potassium chlo-
rate even though the vapor pressure of chlorates at ambient tempera-
tures is negligible and decomposition requires temperatures of 300◦
Celsius, Cajigas, Perez-Amodovar and De Greeff used on ber SPME
derivatization to detect the resultant chloro-2-propanol proving the
outgassing of chlorine [457].
Taudte, R.V., et al. described an automated online Solid Phase
Extraction (SPE) for a Triple Quadrapole direct introduction analysis for
the determination of ve compounds typically encountered in smokeless
powders. The analytes were introduced into soil and a simulated organic
GSR scenario and extracted by this automated SPE with good results.
The report 8 s analysis times [484].
ShuQi An et al. published a paper on DART-MS and varied the
discharge gases (helium, nitrogen and argon) and found that for TNT
and 2,4-DNT the results were that using nitrogen produced mass spectra
“dominated by the oxidation products” suggesting nitrogen provides for
a highly oxidative environment. They also tested some substrates with
thermal desorption DART-MS and reported better results than tradi-
tional DART for 14 explosive compounds [450].
Chelsea Black published a Master’s Thesis on exploring the appli-
cability of DART-MS to identify homemade explosive residues post-blast
[453]. And then also published with D’Souza, T., Smith, J., and Hearns,
N. a paper on using DART-MS for TATP, HMTD, and MEKP with actual
(not spiked) post-blast samples of those. The method worked well with
actual IED fragments, dry swabs or wet swabs, with dry swabbing pro-
ducing the least interferants [454]. The fact that this was done with
actual post-bast samples and not simulated or spiked ones is promising.
R. Boyea published a Master’s Thesis on using multivariate statistical
analysis using GC-MS to compare red cartridge cases with unburned
smokeless powder [456].
Gaiffe, G. et al. used DART-HRMS to examine 83 plastic explosives
and polymer constituents that may be encountered in PBX’s and post-
blast samples of some PBX’s. They conrmed a suite of polymeric
compounds in Semtex 10. They also were able to see what the changes
were post-blast noting “… the best way to describe post-blast polymer
samples is that they are less oxygenated and, above all, more unsatu-
rated than the original starting material” [466].
Using ICP-MS and principal component analysis (PCA) Joshua A.
D’Uva et al. categorized 48 intact sparkler compositions by looking at 50
elements and could categorize eight distinct groups using the elements
V, Co, Ni, Sr, Sn, Sb, and W [461]. It would be interesting to see if in
unknown post-blast samples, the patterns could apply as well.
Similar to DART, Fowble, K.L. and Musah, R.A. used laser ablation
direct analysis mass spectrometry to hyperfocus on ngerprint ridge
details for a variety of illicit substances including the explosive RDX
[464].
DART-MS is primarily a fast technique wherein it’s use as a sample
screening tool is theoretically very useful. Frazier, J., Beneeld, V., and
Zhang, M. test ve different types of DART-MS sample introduction
techniques for a suite of explosives and reported that a Dart gas stream
of 200 ◦C as well as the addition of an acetic acid dopant to wet swabs
produced the best results as other methods even including thermal
desorption “failed in one aspect or another to be high-throughput, sen-
sitive, and/or robust” [465].
Another sampling technique pre GC-MS/MS introduction is
described in a paper by Galmiche, M., et al. Explosives were sampled
from water using stir bar sorptive extraction (SBSE). They varied type of
stir bars, ionic strength, added organic solvent as well as varied times of
extraction and desorption. For those analysts seeking explosives sam-
pling from aqueous solutions, this paper is well worth reading [467].
Gonzalez-Mendez, R., and Mayhew, C.A. published an article on
using soft chemical ionization for quantitation of ve additives
commonly used in smokeless powders through thermal desorption and
qToF-MS but all for pre-blast (i.e. intact) smokeless. A follow up study on
detection post-blast with this technique might prove useful [469].
Bonnar, C., Popelka-Filcoff, R., and Kirkbride, K. used direct sample
analysis ion source integrated with a ToF MS for nitroglycerin and a host
of common additives found often in smokeless powders both in intact
and post combustion modes with limited results on an attempt at organic
gunshot residues on a shooter’s hands. There is a detailed discussion of
the ionization and fragmentation patterns well worth perusing [455].
Supajariyawat, P. and Gonzalez-Rodriguez J. validated explosive
samples taken using the Ionscan® swabs and run on an Ionscan® system
via atmospheric pressure chemical ionization (APCI) in negative ion
mode and an LC-qToF mass spectrometer [483].
Kober, S., Hollert, H., and Frohme, M. used a matrix-assisted laser
desorption/ionization time of ight mass spectrometry (MALDI-TOF
MS) for quick analysis of TNT in soils [475].
McCulloch, R.D. and Amo-Gonzalez, M. reported picogram limits of
detection for several explosives using eld-free atmospheric pressure
photoionization (APPI) combined with a thermal desorption introduc-
tion with differential mobility analysis (DMA) tandem mass spectrom-
etry (MS/MS) [478].
Pavlov, J. et al. showed that 1,4-Benzoquinone is an efcient dopant
for enhanced ionization and detection of nitramine explosives on a
single quadrupole mass spectrometer tted with a helium-plasma ioni-
zation source [481].
Field MS is always a bit tricky for the explosive analyst and mostly
requires suitable ambient ionization and often requires operation with
no power sources, gas supplies, and ow control or heating devices.
Pintabona, L. et al. studied the use of surface acoustic wave nebulization
(SAWN) with MS for ambient ionization suitable for led use and report
“excellent sensitivity of nitrate-based organic explosives was observed
for nitrate-based explosives when operating the MS in the negative
mode” [482].
Organic high explosives are frequently either light molecules with
high vapor pressures or heavier and nonvolatile. Bi, L et al. developed an
“ultrasonic cutter blade coupled barrier discharge ionization” method to
detect ultra trace levels of nonvolatile explosives among other nonvol-
atile compounds [452].
G) Isotope Ratio Mass Spectrometry, IRMS
Isotope ratioing is a technique that can be used to sort or cluster
products, in this case explosives, in order to possibly source the origin of
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that product. For it to be successful large databases are generally
required. There have been successful uses of this technique in both in-
telligence applications and with agricultural products wherein certain
countries are under embargos. It may be useful in forensics especially as
an excluder of commonality of two items but, is of limited use in
denitive inclusions without the aforementioned database for that
product.
Comparison of the homemade explosive erythritol tetranitrate (ETN)
with its precursors was explored in a paper published by Bezemer, K
et al. Keying in on carbon and nitrogen they report that “… robust linear
relationships between precursor and the end product were observed for
these isotopes … that support the hypothesis that a given erythritol or
nitrate precursor was used to synthesis a specic ETN batch.” [488].
C. Hu et al. propose a recrystallization technique to purify ammo-
nium nitrate (AN) to achieve better results from real world AN com-
parisons. They found that without purication contributions from other
materials mixed in with the AN can skew an isotope ratio analysis [489].
Kim, N.Y., et al. studied the propellants from nine different shotshells
from several countries and clustered them by using IRMS. Adding
organic component analysis as well, they were able to discriminate all
nine [490]. Applying this in a post-blast or post-red scenario might
prove useful for sourcing to provide investigative leads although as al-
ways larger databases are needed.
H) FTIR
Fourier Transform Infrared Spectroscopy (FTIR) is a workhorse in-
strument in forensic explosives analysis. Some useful papers are
included in the bibliography.
I) Raman Spectroscopy
Raman spectroscopy continues to be applied for explosives analysis
in the lab as well as in the eld for hazard assessment. There are
numerous advantages to this technique, as we wrote in 2019, “it is fast,
discriminatory, non-destructive and vetted for legal proceedings” [24].
Additionally, it does not require sample prep and is capable of sampling
materials in situ, through containers, and at signicant distances
(stand-off).
Gulia, S. et al. reported on using spatially offset Raman spectroscopy
(SORS) as a method to overcome the limitations of conventional Raman
spectroscopy when applied to testing through colored glass, high density
polyethylene (HDPE), Teon etc. [512]. This will prove useful both in
security settings and for examination of materials in searches.
Colob-Gonzalez, F.M., et al. described a method for detecting TNT,
PETN, and RDX on a variety of hair types with non-invasive Raman
spectroscopy. They found, not surprisingly, that gray hair was the best
substrate for detection [505].
In a unique approach to extremely small samples Kotrly, M., and
Turkova, I., used a stepped approach with SEM/FIB (focused ion beam)
to get 3D reconstruction of the materials in post-blast samples, EDS/
WDS for surface elemental mapping, and high-resolution Raman spec-
troscopy. By using this compliment of techniques, they could easily
focus in on materials of interest and carry out complex analysis on
microscopic particles [518]. In one regard this can be seen as a sampling
technique. This combined instrument set-up could prove valuable for
post-blast analysis where minimal residue is available.
J) DSC, Thermal Analysis, TG
This category is applicable to the examination of explosives and
mixtures and can further characterize an unknown material. These
techniques have been around for decades and while they have limited
applications in the forensic lab setting, they are still useful, especially for
evaluating new explosives and explosive formulations.
7. Nanotechnology
Nanotechnology can be used for the miniaturization of instrumen-
tation which can be much more easily deployed for eld analytical use.
It also can signicantly enhance detection of very small amounts of
analytes. Also in this category is the production and manufacture of
nanoexplosives which are more efcient and theoretically at least
portend less environmental contamination due to the efciency of the
explosive.
Using Raman spectroscopy coupled with nanomotors Novotny, F.,
Plutnar, M., and Pumera, M., detected picric acid. Their synthesis of the
nanomotors was done using the seeded growth wet chemical method as
opposed to planar substrate methods, and they report that this method is
highly scalable [551].
Bhatt, P.V., et al. also wrote about using nanotechnology as a means
of tagging explosives as well as general advances in nanotechnology and
a summation of the current trends [538].
8. General detection
A) Canine Explosives Detection
Canine explosive detection is both very effective, given the right
training and reasoned deployment, and simultaneously the most frus-
trating for analysts who cannot replicate this efciency and selectivity
using man made instrumentation. Research in this area continues to try
and shed light on the complexities of how canines process and detect
target odors and the optimization of training aids and odor presentation.
There are many considerations for training and maintaining an effective
explosives detection canine team, some of which are discussed in the
papers in this section.
Sacharczuk, M. et al. published a fascinating study on canine per-
formance and selected canine olfactory receptor genes. They identied
the ten canines with the best performance and the ten with the worst out
of 91 drug detecting canines and 57 explosive detecting dogs. They then
examined several genes in order to predict, before training, which ca-
nines would be best suited for detection work [566].
One potentially signicant problem with canines is their receptive-
ness to handler cues. Lazarowski, L. et al. reported that responsiveness to
human cues decreased with age but the ability to locate the reward
increased and “Furthermore, a lack of susceptibility to deceptive social
cues was predictive of future success as a detection dog” [564].
DeGreeff, L. and Peranich, K. published an article on using a Mixed
Odor Delivery Device (MODD) to increase prociency in canines for the
detection of mixtures that contain a target odor. The paper nds that
canines exposed to mixtures in training had more success detecting odors
in a mixture than those that had not previously trained on mixtures. The
odorants were veried using SPME-GC/MS for quality control [559].
Gazit, I. et al. designed an experiment to test a canine’s ability to
correctly alert on individual odors when previously exposed to a mixture
of those odorants. They found dogs can indeed quickly recognize indi-
vidual components [563].
Simon, A.G., et al. described using DART-MS to monitor in real time
TATP released from a polydimethylsiloxane canine training aid and
compared it to other training aids for the same analyte. They report this
training aid style had similar odor output to a traditional style container
with holes in the lid. The authors also used DART to assess real time odor
availability from both styles of training aids in various search congu-
rations [568].
B) LIBS Detection
Romolo, F.S. and Palucci, A. have published a review chapter on the
advances with detection techniques for security purposes in the areas of
laser induced breakdown spectroscopy (Stand-off) or LIBS, Raman
(stand-off), surface enhanced Raman spectroscopy (SERS) and laser
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photoacoustic spectroscopy They discuss the detection limits and the
drawbacks of these techniques and discuss how they can be used to
advance an investigation. One such example was helping to reduce the
number of samples sent to the lab [577].
C) Neutron
Seman, J., Giraldo, C.H.C., and Johnson, C.E. reported on a proposed
nuclear barcode to be used as a chemical detection agent. Part of the
coding employs a unique combination of taggant elements at different
concentration levels that could be used to provide specic information
about where and when the explosive was manufactured which could
provide valuable investigative leads in criminal or terrorist bombings.
The paper examines the stability of the ratios over time and found that
the technique could work if the concentration levels were separated at
least 100 ppb [583].
D) Terahertz
E) Nuclear Techniques
Yu, P., et al. monitored the droplet size distribution in ANFO emul-
sion explosives at different temperature and storage conditions to assess
any impact of the storage condition on the stability of the emulsion.
They used Nuclear Magnetic Resonance (NMR) Pulsed Field Gradient
(PFG) and found storage at 50◦Celsius for 12 weeks lead to a 60% in-
crease in mean droplet size. Adding 5% calcium nitrate to the aqueous
phase suppressed this thermal degradation [602].
F) X-Ray
G) Ion Mobility Spectrometry
While Ion Mobility Spectrometry is often used in security screening
settings because of its rapid sampling times and relative accuracy, it
often has not been used often in forensic laboratories because of its
limited ability to separate analytes, its propensity for being overloaded
quickly requiring a period of cleaning of the system, and its potential for
false positives. There have been advances made to allow for limited
separations and quicker recovery times improving the usefulness of this
technology.
Hauck B., Harden C., and McHugh V. evaluated ve possible cali-
brants for an ion mobility time of ight instrument. They reported that
di(propylene glycol) methyl ether (DPM) was the most useful and rec-
ommended against 2,4-pentanedione (PDO) and methyl salicylate
(MES) [610].
Thangadurai S. and Gurusamy K. advocated for use of IMS in post-
blast debris samples and reported that several explosives were detec-
ted in various matrices. They discuss sample preparation and screening
and highlight the advantages and limitations of the technique for the
detection of explosives [616].
Chilluwal, U. published a dissertation arguing for tandem IMS using
chlorine adducts of RDX, PETN and NG for the analysis. By using tandem
IMS there was a reported elimination of the false positives often
encountered with IMS results due to interferents [608].
In a similar fashion, Mullen, M., and Giordano, B. used the combined
technique of secondary electrospray and corona discharge ionization
(SECDI) to achieve more sensitivity for TNT and 2,6-DNT [612]. These
approaches that eliminate the problems inherent in IMS may prove
valuable as a very rapid analytical tool.
The drift tube design for IMS was enhanced in a paper published by
Smith, B. et al. They designed a exible drift tube and report “the DT
(drift tube) is constructed from a exible printed circuit board (PCB)
with a bespoke ‘dog-leg’ track design, that can be rolled up for ease of
assembly.” This design was reported to have a low cost and low footprint
with limits of detection in the low nanograms [615].
Fisher, D., et al. proposed applying machine learning to IMS for a
preliminary study using ve nitrate explosives, AN, ANFO, Urea Nitrate,
environmental pollution nitrates and blanks. Their supposition is that
machine learning can enhance selectivity for actual threats [609].
Bohnhorst, A., et al. wrote about their new approach to enhancing
separation by increasing the resolving power of the drift time IMS
without employing higher drift voltages. Instead, they employed a
moving eld IMS (MOF-IMS) to use the available voltage to a smaller
segmented drift region [607].
H) Novel Detection
Novel detection is a catchall category for detection that does not fall
neatly into another category. It could be completely novel or it could be
something based on other techniques but different enough to be
included in this section of the paper or bibliography.
Filipi, J., et al. described the use of honeybees as a tool that could be
used in humanitarian demining efforts. The bees can be used in passive
searches to detect the present of landmines in an area or active searches
of pinpointing locations. The system relies on the detection of explosives
residue on the body of honey bees that were foraging [638].
Simic, M. et al. described a similar use of honeybees. As a passive
system honeybees can “electrostatically collect particles from the air in
the ying and foraging areas, which in conjunction with organic-based
explosive vapor sensing lms, placed at the entrance of a beehive, can
be used as a passive explosive sensing mechanism.” Furthermore, hon-
eybees can be trained to react to certain explosives [685].
In a similar vein of using animals to detect explosives, Alsaleh, S.,
Barron, L., and Sturzenbaum, S. published a paper on the use of the
invertebrate nematode Caenorhabditis elegans (worm) for the detection
of ground soil perchlorate [620].
Liu, C. et al. integrated a smart phone with a urea-functionalized
polyionic liquid photonic spheres to construct a colorimetric sensor
array that can detect and identify ve nitroaromatic explosives [660].
Lefferts, M.J., et al. used “ANFO chemiresistive vapour sensors based
on polypyrrole (PPy) percolation networks to enhance” GC-MS results
and reported improved sensitivity over thin lm and detected “13–180
ppb of ammonia emitted by a variety of different ammonium nitrate …”
mixtures [656].
Blanco, S., et al. proposed wetting TATP as they form TATP-water
adducts which could then be detected by microwave spectroscopy
[625].
I) Stand Off
9. Environmental
As we wrote in 2019, Environmental scientists and chemists have
long sought to test and eventually remediate explosives in environ-
mental samples. Some of these methods can be directly borrowed from
this eld for use in forensic laboratories. Still other research, such as
degradation studies, may assist the analyst in background knowledge of
the explosive in certain matrices, especially soils [24].
Nawala, J. et al. used GC-MS/MS, LC-HRMS and NMR to examine
explosives excavated from the Baltic Sea. There are tons of unexploded
ordinance on the sea bed, so classifying it is important. They found that
most samples indicated that it was a TNT, RDX, aluminum mixture
known as “torpex” [770].
Rindelaub, J.D., et al. used XRF to measure particulate matter from
reworks usage in New Zealand to postulate source material (e.g. Cl
from perchlorate oxidizers) and compared air quality vis-`
a-vis standard
environmental exposure recommendations [776].
10. Other (safety, denitions, etc.)
While this article could be placed in the review category, we have
included it here. Richard Crocombe has done an extensive review of
portable spectroscopy including a discussion of the future of the
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8
technology. He looked at the deployment numbers and usage of portable
IMS, XRF, FTIR and Raman instruments, most of which are deployed in
security operations or with re or police hazmat responders [823].
da Silva, L., et al. published an interesting paper on pipe bomb
fragmentation with varying case (wall) thickness. They used aluminized
ammonium nitrate detonated with a PETN based detonator and a 5-g
booter made of PETN and nitrocellulose and noted that the size and
velocity of the fragments correlated to the pipe size [825]. It would be
interesting, since the quality control on the pipes and test design was
well thought out, to do similar tests with a suite of low explosives and
not boosted or detonated.
Amaral, M., et al. studied transfer dynamics of ammonium nitrate
showing transfers “… even when contact occurs for a short duration
with a relatively low force” [796]. They report a variety of test condi-
tions which may be useful in understanding transfer in the context of
crime scenes or swabbing techniques. This reference could also be
placed in the sampling category.
Collett, G. et al. tackled the predictive threat assessment process for
Homemade Explosives (HME) precursors, specically the regional dis-
tribution of hydrogen peroxide, ammonium nitrate and potassium
chlorate [821].
Although there were many articles published on the Beirut Port
ammonium nitrate explosion, Yu, G. et al. published perhaps the most
comprehensive one. By looking at many post-blast factors, measure-
ments, and reports, they calculated the TNT equivalent of the AN ex-
plosion to be approximately 950.3 tons and the fatality radius to be 487
m from the center. They also included an evaluation other safety related
considerations relating to the accident and future ammonium nitrate
storage considerations [954].
Oluwoye, I., et al. used XRD and IR to examine rust on iron-based
containers to show oxygen decient Fe
2
O
3
clusters can serve as an
agent to reduce ignition temperatures with ammonium nitrate reactions.
They report “The dihydroxylation of hydrated iron (III) oxide, present
on the surfaces of rust, exposes the Fe sites that react exothermically
with AN, before the material assumes the ordered Fe
2
O
3
phase.” It may
be prudent to monitor AN storage conditions in steel storage containers,
especially older ones. AN is a strong oxidizer and does not require a high
percentage of fuel to react or even detonate [898].
Rettinger, R., et al. published an article on lab scale (2 g) and eld
scale (5 kg) testing for combinations of several oxidizers (potassium
nitrate, potassium chlorate, potassium permanganate, potassium iodate,
ammonium nitrate and ammonium perchlorate) mixed with sucrose and
aluminum to compare explosive potentials of each [910].
Tin, D., Margus, C., and Ciottone, G., did a comprehensive review of
all terrorist events for the last 50 years, including ones deploying ex-
plosives. They report 48.78% of these 168,003 events used explosives
since 1970 [934]. This paper is a tting note to end on, highlighting the
continued need for research and development to combat the threat of
explosives.
Final notes
We have tried to review as much literature as possible these last few
years and have written here about dozens of publications. There are
indeed hundreds more citations listed in the bibliography, many of
which may have some useful information for your forensic laboratory
and explosive analysts.
Acknowledgements
The authors would like to express our deepest gratitude to Ms. Logan
Tapscott, Librarian for the Bureau of Alcohol, Tobacco, Firearms and
Explosives Laboratory. Additionally, the tireless work of the staff of the
Arson and Explosives Sections at the ATF Forensic Science Laboratory,
Washington, especially Malinda Durand and Delonn Ng have been
invaluable.
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