Study of gunshot residue by NAA and ESEM/EDX using several kinds of weapon and ammunition

Study of gunshot residue by NAA and ESEM/EDX

using several kinds of weapon and ammunitionQ1 Q10

Q9 M. Chohra a, B. Beladel b, L. Baba Ahmed c, M. Mouzai d, D. Akretche e,A. Zeghdaoui f, A. Mansouri g, M.E.A. Benamar c,*

a Sous Direction de la Police Scientifique et Technique/DPJ/DGSN, Chateauneuf, Algeriab Ziane Achour University, Department of Physics, Djelfa 17000, Algeriac Laboratoire de Physique Fondamentale et Appliqu�ee, Universit�e Saad Dahlab, Blida, B.P. 270, Blida 09000, Algeriad Centre de Recherche Nucl�eaire de Draria, B.P. 43 Sebala, Draria, AlgeriaQ2e Universit�e des Sciences et de la Technologie Houari Boumediene, BP 32 El Alia, Algeriaf Ecole Normale Sup�erieur, Bachir El Ibrahimi B.P.92, Kouba, Algeriag Nuclear Research Centre of Algiers, 02, Frantz Fanon Street, P.O. Box 399, Algiers, AlgeriaQ3

a r t i c l e i n f o

Article history:

Received 10 November 2014

Received in revised form

22 February 2015

Accepted 27 February 2015

Available online xxx

Keywords:

GSR

SEM/EDX

NAA

Chemical ballistic

Scientific Police of Algeria

a b s t r a c t

This work is realized in view to determine appropriate techniques for the revelation of

mineral gun shoot residues. Picked up from the crime scene, these indicial traces are used

as material proofs for helping and guiding judicial investigations. As achievement of this

process, two (02) technics were employed for mineral gun shoot residues, namely; Neutron

Activation Analysis, and scanning electron microscopy/EDX. Samples of metallic powder

residue were realized after several shoots by different kind of weapons with local and

foreign ammunitions. So, this study was undertaken to develop chemical ballistic specialty

in order to improve forensic investigations and drive benefit to Technical and Scientific

Police of Algeria to be use for judicial investigation.

It turns out that the SEM/EDX method is more adequate to this type of investigation,

despite the high sensitivity of the NAA. This is stated; NAA remains a complementary

methods.

Copyright © 2015, The Egyptian Society of Radiation Sciences and Applications. Production

and hosting by Elsevier B.V. This is an open access article under the CC BY-NC-ND license

(http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction

The revelation of ballistic gunshot residue (GSR) is commonly

performed with the aim of determining whether or not a

suspect handled a firearm and or to estimate a firing distance

(Gallusser, Bonfanti, & Schutz, 2002; Kersh et al., 2014).

Generally, the GSR particles are formed with a diameter

which is most often in the range of 0.1e10 mm and occa-

sionally up to 55 mm or above (Basu, 1982; Wolten & Nesbitt,

1980). Q4

Gunshot residues are collected after shooting sessions

using tamponnoirs to determine the composition of the

GSR reference by various techniques to choose methods

and techniques most suitable for this type of analysis, such

* Corresponding author.E-mail address: [email protected] (M.E.A. Benamar).

Peer review under responsibility of The Egyptian Society of Radiation Sciences and Applications.

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J o u r n a l o f R a d i a t i o n R e s e a r c h and A p p l i e d S c i e n c e s x x x ( 2 0 1 5 ) 1e7

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http://dx.doi.org/10.1016/j.jrras.2015.02.012

1687-8507/Copyright© 2015, The Egyptian Society of Radiation Sciences andApplications. Production and hosting by Elsevier B.V. This is an

open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Please cite this article in press as: Chohra, M., et al., Study of gunshot residue by NAA and ESEM/EDX using several kinds ofweapon and ammunition, Journal of Radiation Research and Applied Sciences (2015), http://dx.doi.org/10.1016/j.jrras.2015.02.012

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as scanning electron microscopy coupled with X-ray

microanalysis (SEM/EDX) (Gilchrist et al., 2012; Lopez-

Lopez, Delgado, & Garcia-Ruiz, 2013) and Neutron Activa-

tion Analysis (NAA) (Bonfanti & Gallusser, 1995; Romolo &

Margot, 2001).

A scanning electronmicroscope equippedwith the energy-

disperssion X-ray (SEM/EDX) is a spectral technique providing

visual identification (morphological information) of mineral

particles of powder residue after firing (from the primer)

mainly composed of Lead (Pb), barium (Ba) and antimony (Sb)

(Basu, 1982; Wolten & Nesbitt, 1980), furthermore, the

analytical analysis identifying the elemental composition

contributes as a second identification to confirm a significant

presence of the mineral particles cortege of ballistic gunshot

residue, whichwe can detect false positives caused by sources

of pollution (Mosher, McVicar, Randall, & Su, 1998; Romolo &

Margot, 2001). The analysis of gunshot residue of inorganic

nature, is always preferable using scanning electron micro-

scopy coupled with the X-ray microanalysis (SEM/EDX)

(Brozek-Mucha, 2014; Taudte et al., 2014), because it is non-

destructive and allows the chemical and morphological

identification of mineral particles (DeGaetano & Siegel, 1990;

Romolo & Margot, 2001).

This study aims to make the choice of national (Seriana-S)

and international (Geco) ammunition. These results should be

addressed to the court so we must be convincing, without

prejudice to the suspect. Other spectral techniques such as

neutron activation analysis (NAA), proton induced X-ray

emission (PIXE) and atomic absorption spectroscopy (AAS) can

be complementary in terms of quantity (May & Pinte, 1991;

Sen et al., 1982; Taudte et al., 2014).

2. Materials and methods

2.1. Firearms used in the shootings

To collect GSR, firing tests were performed using local and

foreign ammunition, using several different types of weapons,

brand, model and caliber, namely: Automatic rifle KALACH-

NIKOV caliber: 7.62 � 39 mm (using National ammunition

Seriana); Shotgun Saint-Etienne 16 (using national ammuni-

tion; Onex), Semi-automatic handgun “P.Beretta” 7.65 mm

(using national ammunition; Seriana) and 38 SP Smitt &

Wesson Revolver (using foreign ammunition, Geco).

The shots were made in a special device called a water

channel, designed for firing shot, the latter as evidenced by its

name is as long alcove dimension 395 � larg130 � prof174

(cm3) filled with water (6000 L), which serves as a braking

system powered projectiles (Fig. 1).

2.2. Sampling method

The samples were taken on revealing places and according to

the usedweapons, on the skin: both sides of hands (palms and

outer sides) and tissue supports (sleeves, shoulders, and hair)

(Fig. 2).

The White swab: It is essential to achieve a “white”, i-e a

circular carbon adhesive tapes (12.5 mm in diameter) (Fig. 3)

mounted on an aluminum stub, which, in principle, has not

been in contact with GSR but exposed on the location of levies

(Romolo & Margot, 2001).

2.3. Neutron activation analysis

For the determination of shooting residues, a qualitative

analysis of traces was performed. The experiment was to

determine the trace elements from the residues contained in

four Levies Supports of Graphite (LSG). These LSG represent an

ideal matrix for the technique, because the graphite is trans-

parent to thermal neutrons; it does not constitute a source of

interference. Note that the plastic holder was removed from

Abbreviations

BSED Back Scattered Electron Detector

CRND Centre de Recherche Nucl�eaire de Draria

DGSN Direction G�en�erale de la Suret�e Nationale

DPJ Direction De la Police Judiciaire

EDAX Energie Dispersive Analyse X-Ray

ELH External Left Hand

ENFCI European Network of Forensic Science

Institutes

ERH External Right Hand

GSR.V3 Gun Shoot Residue software Version 3

IRH Internal Right Hand

ILH Internal Left Hand

LH Left Hand

LCPS Laboratoire Centrale de Police Scientifique

LSG Levies Supports of Graphite

SEM/EDX Scanning Electron Microscopy/Energy

Dispersive X-Ray

NAA Neutronique Activation Analyse

PA Person Adjacent

RH Right Hand

SED Secondary Electron Detector

SP Soft Point

SDPS Sous-Direction de la Police Scientifique et

Technique

Fig. 1 e The test firing carried out in the water channel

(LCPS/SDPST/DPJ/DGSN).

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the LSG. The four samples analyzed are called Geco-38Ssp/

IRH; Geco-38sp/ERH; SERIANA-7.65 mm/IRH and SERIANA-

7.65 mm/ERH. Before being irradiated in the reactor, each

sample was wrapped in aluminum of high purity (99.99%). An

empty envelope and two blank LSG are also analyzed. The lot

consists of seven samples is irradiated for 2 h at a flux of

1013 neutrons/cm2 s provided by the nuclear reactor NUR at

Nuclear Research Centre of Draria-Algiers. The gamma ray

spectra resulting from the decay of the elements activated by

the neutrons is then analyzed using a gamma spectrometer

using a High Resolution germanium detector. The software

used for the deconvolution of the spectrum is 32 GAMMA

VISION. Fig. 4 below shows the gamma spectrum from the

sample Geco-38sp/ERH.

2.4. Scanning electron microscopy with X-ray

microanalysis

The characterization was realized by ESEM Microscope-type

Quanta 400 MK2 brand FEI e coupled to an X-ray micro-

analyzer “EDAX” and equipped with a secondary electron

detector (SED), a backscattered electron detector (BSED), an X-

ray detector “EDAX” and two video screens with a “Quanta,

EDAX Genesis GSR” software (Postek, Howard, Johnson, &

McMichael, 1980; Tassa & Zeldes, 1979; Zeichner, Levin, &

Springer, 1996). Automated classification and assistance GSR

particles were carried out by the GSR software “GsrV3”. The

latter has an advanced automatic calibration procedure that

allows full and dynamic adjustment of the microscope col-

umn, the motorized stage, the BSED and an X-ray analysis

system (automatic search) (White & Owens, 1987). The X-ray

sensitivity parameters were calibrated using certified stan-

dards. The samples are disposed on the platinum in a regular

or irregular pattern to more than 16 samples.

3. Results

3.1. Neutron activation analysis

Knowing that the shots were made with the right hand ra-

dionuclides identified in the irradiated samples from car-

tridges 7.65 mm-Seriana using “P.Beretta” pistol, 82BB and 38-

SP-GECOusing “S&W” revolver are: 153Smor 153Gd, 141Ce, 151Cr,198Au, 131Ba, 82Br, 122Sb, 124Sb, 59Fe, 65Zn, 182Ta, 24Na, and 140La.

GammaCounting detected from elements in the envelope and

blank support vary between 2.29 10þ2 and 3.87 10þ4.

By comparing samples containing shot's residues with

blank GSP and an aluminum envelope, a significant increases

of counting was observed from antimony (122Sb, 124Sb), iron

(59Fe), Barium (131Ba) and to a lesser degree from Brome (82Br).

Net counting shows that only the elements (131Ba, 82Br,122Sb, 124Sb, and 59Fe) can be differentiated from impurities

found on blank support and in envelope:

- 131Ba: 5.05 10þ2 and 1.76 10þ2, respectively Net counting of

shots GSR detected on IRH and ERH from the cartridge

7.65 mm SERIANA so Barium was detected in samples

SERIANA only.

- 82Br: 1.29 10þ3 and 6.33 10þ2 respectively net counting of

GSR detected on the IRH and ERH and from the cartridge

Fig. 2 e Samples taken after firing tests (LCPS/SDPST/DPJ/

DGSN).

Fig. 3 e The water channel and “White swab” (LCPS/SDPST/DPJ/DGSN).

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SERIANA 7.65 and 3.82 10þ2 and 1.04 10þ3 respectively

detected on IRH and ERH Bromine the 38-SP GECO car-

tridge, so Bromine is slightly higher in gunshot residue

Seriana Geco.

- 122Sb: 1.48 10þ5 and 6.33 10þ4 net counting of GSR detected

respectively on the IRH and ERH from the cartridge SERI-

ANA 7.65 mm, and 4.22 10þ4 and 4.90 10þ4respectively

detected on the IRH and ERH from the cartridge 38 SP-Geco.

So Antimony (122Sb) is greater by a factor 40 in the samples

from Seriana Geco.

- 124Sb: 2.74 10þ4 and 1.21 10þ4 net counting of GSR respec-

tively deteted on IRH and ERH from cartridge 7.65 mm

Seriana, and 7.5 10þ3 and 9.76 10þ3 respectively detected on

IRH and ERH from cartridge 38-SP GECO.

- 59Fe: 1.18 10þ3 and 5.04 10þ2 respectively net counting GSR

detected on IRH and ERH from the cartridge SERIANA

7.65 mm, and 2.74 10þ2 on IRH from 38 SP cartridge Geco.

Due to its high sensitivity, the INAA technique could detect

Barium, Antimony, Zinc, Bromine and Iron in most samples,

although these elements are present in trace amounts in the

graphite support. Because it does not interact with the

neutron, the graphite is an ideal matrix for the INAA tech-

nique. Graphite is therefore not a source of interference for

the determination of trace residues from shots. However, Lead

as an element of the GSR is not detectable by INAA because its

reaction with the neutron produces a radionuclide with very

short half life (T1/2 ¼ 800 ms).

Moreover, trace elements detected in samples taken from a

hand does not necessarily mean that they are from GSR.

Therefore, INAA technique is unable to identify the origin of

trace elements.

3.2. Scanning electron microscopy coupled with X-ray

microanalysis

The morphological (visual) results showed a nodular specific

morphology of metal particles Pb, Ba and Sb resulting from

gunshot residue. These photos (Fig. 5 and Fig. 6) obtained from

GECO cartridge SP-38 External Right Hand were taken from

SEM/EDS of Algiers central scientific laboratory of police.

3.2.1. Analytical identification (chemical composition)

3.2.1.1. K-means classification of GSR supports. EDAX analysis

identifying the elemental chemical composition contributes

as a second identification to confirm a significant presence of

ballistic gunshot residue and detect every wrong positives due

to pollution sources (Romolo&Margot, 2001). Application of k-

means on the GSR shows five (05) classes for each type of

weapon.

� Pistol (semi-automatic), “P.Beretta”-7.65 mm-82BB, using

national ammunition; Seriana: The registration of a high

concentration of GSR particles on different supports

Fig. 4 e g spectra of GSR after firing ammunition Geco38 SP/ELH obtained by NAA.

Fig. 5 e Morphologie of PbBaSb, obtained from GECO

cartridge SP-38 External Right Hand HV: 10.0 kV; mag:

20,000£; W: 11 mm; spot: 3.5; det: DualBSD.


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especially on the matrix ERH (class 1) indicating a signifi-

cant presence of unique particles PbBaSb and BaSb

(Wallace & McQuillan, 1984; Wolten, Nesbitt, & Calloway,

1979; Wolten, Nesbitt, Calloway, Loper, & Jones, 1979), is

explained: triggering the shooting carried out by the right

hand which its outer face was close to the ejection port

(first exit smoke) without forgetting the barrel of a gun

(second exit smoke) is close to the ERH matrix which

operates (in our case) the ballistic shot.Q5

Contamination of other matrices ELH, RH, LH and AP

(classes 3 and 5) must be considered. internal Matrices IRH

and ILH (class 2 and 4) may be subject to contamination

(Table 1).

� Shotgun, Saint Etienne-16 using national ammunition;

Onex: The registration of a high concentration of unique,

particles including PbBaSb and BaSb (Wallace &McQuillan,

1984; Wolten, Nesbitt, & Calloway, 1979; Wolten, Nesbitt,

Calloway, Loper, et al., 1979) and especially on the matrix

ELH (class 3) is explained by: supports the gun barrel with

the left hand whose outer face (ELH) is close to the muzzle

(only exit of the smoke). The absence of GSR particles on

thematrix ERH (class 1) is explained by the fact that there is

no ejection port, which implies no exhaust smoke near the

hand that operates the ballistic shot, also the matrix ERH

operating the fire is distant from the muzzle.

The Contamination of other matrices LH, RH, and PA (class

1 and 5) should be considered (Basu, 1982; Garofano et al.,

1991). The same observation for the matrices IRH and ILH

(class 2 and 4) as the P.Beretta-82BB pistol, using 7.65 mm

Seriana cardridge. (Table 2).

� Revolver, Smitt & Wesson using foreign ammunition, 38

SP-Geco: The registration of a very high concentration of

GSR particles on different revealing supports especially on

thematrix ERH (class 1) indicating a significant presence of

unique particles PbBaSb and BaSb (Wallace & McQuillan,

1984; Wolten, Nesbitt, & Calloway, 1979; Wolten, Nesbitt,

Calloway, Loper, et al., 1979), is explained by the release

of the shot made by the right hand whose outer face was

close to the barrel (exit of the smoke between the barrel

and the cylinder), not to mention that the barrel of a

revolver is close to the hand operating the ballistic shot.

The last meeting of the two criteria regarding the evacua-

tion of waste powders with the power of 38SP cartridge

amplified the concentration of particles of ballistic gunshot

residue on the right hand that powered the shot.

The Contamination of other matrices ELH, RH, PA and LH

(class 3 and 5) must be considered (Basu, 1982; Garofano

et al., 1991). The same for IRH and ILH (class 2 and 4)

matrices as weapons previously studied (Table 3).

� Automatic rifle, Kalachnikov using National ammunition

7.62 � 39 mm-Seriana: The registration of a high concen-

tration of GSR particles on different revealing supports

especially on matrices, ERH, RH, LH and ELH (Class 1, 3, 4

and 5) indicating a significant presence of unique particles

PbBaSb and BaSb (Wallace & McQuillan, 1984; Wolten,

Nesbitt, & Calloway, 1979; Wolten, Nesbitt, Calloway,

Loper, et al., 1979) is explained by: the support of the gun

barrel with the left hand, whose the external face ELH

(class 1) was close to the muzzle (first exit of smoke) and

triggering the firing performed by the right hand close to

the ejection opening (second outlet of smoke). The pres-

ence of significant GSR on RH and LH matrices (class 4 and

5) is justified by the spread of smoke coming out of the

muzzle and the ejection opening, knowing that the length

of the barrel of the Kalashnikov is less important than the

shotgun one's.

The Contamination of the matrix PA (class 5) must be

considered (Basu, 1982; Garofano et al., 1991). The same is

noted for IRH and ILH matrices (class 2) than previous

weapons (Table 4).

Fig. 6 e Morphologie of PbBaSb, obtained from GECO

cartridge SP-38 External Right Hand, HV: 10.0 kV; mag:

20 000£; W: 11 mm; spot: 3.5; det: ETD.

Table 1e Spatial distribution of GSR particles using Pistol,Beretta, 82BB, 7.65 mm and Seriana local ammunition.

Particules MDE MDI MGE MGI MD MG PA

PbBaSb 48 19 14 06 05 04 04

BaSb 22 28 19 20 33 19 08

PbSb 13 14 16 04 07 05 04

Sb 13 10 17 09 486 307 04

PbBa 07 06 01 02 / / /

Ba 18 13 07 15 49 54 07

Pb 91 80 98 53 58 38 14

BaCaSi / 02 01 01 10 / 02

Table 2 e Spatial distribution of GSR particles usingShotgun, Saint-Etienne, 16 and Onex local ammunition.


PbBaSb / / 30 / 03 02 /

BaSb / 12 18 02 03 03 02

PbSb / 03 161 12 08 09 03

Sb / 519 378 421 103 632 43

PbBa / / 03 / / / /

Ba / 01 03 06 06 04 02

Pb / 03 237 25 16 57 23

BaCaSi / 08 52 21 06 07 01


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4. Discussion

There exists, on the hands and clothing effects, a presence of a

large number ofmetal particles of composition: (PbBaSb, BaSb,

PbSb, Sb, PbBa, Ba, Pb, BaCaSi, SbS, BaS, Ti, Fe, Sn, SnSb, Ca,

Cu, Bi, KCl, Ni and CuZn). This minerals offers an information

about the cartridge parts composition (bullet alloy, case alloy,

case mineral container and cartridge cap composition). This

presence is confirmed by the morphological specificity of

these particles, namely PbBaSb which have a spheroid shapes

with nodules due to recent contacts with the particles lodged

inside the bore due to antecedent fire or also due at the

diffusion between a small spheroids and a large spheroids

(Basu, 1982). Given their compositions and their morphol-

ogies, these particles constitute a formal indication of the

presence of ballistic shots residues. In this context, it follows

that collected samples, helped to highlight a more important

and significant presence of metal particles on the telltale

places, classified in a procession of mineral particles ordered

according to their importance (Wallace & McQuillan, 1984;

Wolten, Nesbitt, & Calloway, 1979; Wolten, Nesbitt,

Calloway, Loper, et al., 1979). The spatial distribution of resi-

dues of shots, depending on the weapon is used, and espe-

cially on the hand that operates the shooting (near the

ejection outlet) and the hand holding the gun barrel close to

the exhaust gas locations (Garofano et al., 1991; Syvitski, 1991).

The presence of mineral particles on the adjacent person

warns of the risks of cross-contamination (Garofano et al.,

1991).

5. Conclusion

Neutron Activation Analysis assess with high sensitivity the

traces of antimony (Sb), Barium (Ba), Bromine (Br) and iron (Fe)

on the graphite sampling support. Unfortunately, Lead which

is a key element in the composition of GSR is undetectable by

INAA. This allows to say that the revelation of GSR using only

INAA is insufficient. In addition, the technique is unable to

decide whether these elements come from a GSR or another

source of pollution.

The results of analysis and expertise gunshot residues by

environmental scanning electron microscopy technique, al-

lows us to make the following conclusions:

SEM/EDX is a non-destructive method, it eliminates sam-

ple preparation, no need to be metallized (for non-conductive

specimens).

The combination of mineral particles contained in the

composition of gunshot residues, gives us an idea about the

sources and itinerary of mineral elements by visual identifi-

cation towards the origin.

The analysis, point by point and line by line allows scan-

ning the entire matrix. The mineral particles detected are

numbered and classified, which allows us to revisit specific or

suspicious particles. This revision reform false positive or

false negative results, because controlling revisited particles is

done by visual analysis of the particle and the chemical

analysis of the elemental composition.

On the whole, we can say that the environmental ESM/EDX

is the most suitable among the techniques studied for this

type of investigation. It will keep unchanged the sample

which can be a key to maintain legal proof.

Acknowledgments

First author wishes to thank his superiors; M. Feragh Ali and

M. Zekri Mohammed for their support, also to thank his col-

legues; MM. Benyell�es S., M. Asseli B., M. Tahraoui M. for their

cooperation in the test firing, without forget M. Magnouch,

responsible of CRND for providing a help to analyze.

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Table 3 e Spatial distribution of GSR particles usingRevolver, Smitt & Wesson, 38 SP and Geco foreignammunition.


PbBaSb 256 154 02 17 05 / 07

BaSb 20 21 01 13 03 03 /

PbSb 40 17 02 05 01 / /

Sb 02 17 / 09 / / 01

PbBa 58 09 01 05 04 04 /

Ba 09 / 01 01 03 / /

Pb 645 333 25 125 46 03 07

BaCaSi 71 08 / 09 / 04 01

Table 4 e Spatial distribution of GSR particles usingAutomatic rifle KALACHNIKOV, 7.62 £ 39 mm andSeriana local ammunition.


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Study of gunshot residue by NAA and ESEM/EDX using several kinds of weapon and ammunition

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Transcript of Study of gunshot residue by NAA and ESEM/EDX using several kinds of weapon and ammunition