Tandem detection of organic and inorganic gunshot residues using LC–MS and SEM-EDS

Bonnar, Callum; Moule, Eliza C.; Lucas, Nick; Seyfang, Kelsey E.; Dunsmore, Robert P.; Popelka-Filcoff, Rachel S.; Redman, Kahlee; Kirkbride, K. Paul

doi:10.1016/j.forsciint.2020.110389

Cited by 20 publications

(17 citation statements)

References 32 publications

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“…For the elemental analysis of small samples, scanning electron microscopy-energy-dispersive X-ray spectroscopy (SEM-EDS) [13], X-ray fluorescence (XRF) [14,15], laser ablation-inductively coupled plasma-mass spectrometry (LA-ICP-MS) [16,17], and laserinduced breakdown spectroscopy (LIBS) [18,19] have been used in forensic science. SEM-EDS simultaneously allows the observation of micro-samples and elemental analysis of the primary components.…”

Section: Introductionmentioning

confidence: 99%

“…SEM‐EDS simultaneously allows the observation of micro‐samples and elemental analysis of the primary components. However, it is a destructive method because it involves carbon deposition onto the samples and, because its lower limits of detection (LLDs) are ~0.1%, it is often unsuitable for detecting trace elements in silk fibers [13]. Laboratory XRF is unsuitable for the trace element analysis of silk single fibers due to problems associated with maintaining an incident X‐ray beam that is both sufficiently thin and intense [15].…”

Section: Introductionmentioning

confidence: 99%

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Nondestructive discrimination of red silk single fibers using total reflection X‐ray fluorescence spectrometry and synchrotron radiation X‐ray fluorescence spectrometry

Komatsu

Takahara

Matsuda

et al. 2021

Journal of Forensic Sciences

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In a strangulation case, when a necktie is used as a murder weapon, the dyed silk single fiber becomes an important evidence sample to solve the crime. Dyed silk single fibers contain elements, such as Cr and Co, which are obtained from dyeing using metal mordants. Currently, there are no nondestructive and sufficiently sensitive elementary analytical methods for the forensic analysis of single fibers. Therefore, in this study, eight commercially available red silk samples were collected and used for total reflection X-ray fluorescence (TXRF) and synchrotron radiation X-ray fluorescence (SR-XRF) spectrometry. Benchtop TXRF detected both S in the silk protein and Cl and Ca, which are elements absorbed from the environment by silkworms, but also Cr, which is a dyeing derivative for metal mordants. The presence of Cr and Zn, in addition to the Zn/Cr signal intensity ratios, was reported to be particularly useful identifiers. In SR-XRF, the presence of Cr, Co, Zn, and Br and the Zn/Cr signal intensity ratios were reported to be useful discriminating indicators. In this study, the nondestructive discrimination capabilities of TXRF and SR-XRF measurements for the samples were found to be 85.7% and 100%, respectively. Therefore, we propose a combination of TXRF and SR-XRF as a new nondestructive single fiber identification method for forensic science. Moreover, if partial destruction of a single fiber is allowed, the observation of the cross section and micro-Fourier-transform infrared spectroscopy measurements is useful for identifying red silk fibers.

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Section: Introductionmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 99%

Nondestructive discrimination of red silk single fibers using total reflection X‐ray fluorescence spectrometry and synchrotron radiation X‐ray fluorescence spectrometry

Komatsu

Takahara

Matsuda

et al. 2021

Journal of Forensic Sciences

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“…Black et al demonstrated that sufficient SP material could be extracted from the surface of such a stub with a droplet of organic solvent to enable analysis of OGSR compounds by direct analysis in real-time mass spectrometry. Further evaluation of this stub-and-droplet extraction approach has shown successful detection of SP residues on the hands of a recent shooter using hyphenated liquid chromatography and mass spectrometry, without disruption to particles of IGSR present on the stub surface . While OGSR examination is unlikely to fully replace the prevailing method of choice for shooting investigations (i.e., IGSR examination), there are potentially many benefits to carrying out the analysis of OGSR traces in addition to the analysis of IGSR.…”

Section: Introductionmentioning

confidence: 99%

“…Further evaluation of this stub-and-droplet extraction approach has shown successful detection of SP residues on the hands of a recent shooter using hyphenated liquid chromatography and mass spectrometry, without disruption to particles of IGSR present on the stub surface. 24 While OGSR examination is unlikely to fully replace the prevailing method of choice for shooting investigations (i.e., IGSR examination), there are potentially many benefits to carrying out the analysis of OGSR traces in addition to the analysis of IGSR. When compared to assessing IGSR alone, OGSR may increase the total mass of crime-related trace for detection, provide a greater amount of orthogonal chemical information, and help analysts discriminate between types of ammunition and nonfirearm sources of GSR-like material.…”

Section: ■ Introductionmentioning

confidence: 99%

“…For the third aspect of this study, the simple and rapid extraction process reported by Black et al 23 was used as it offered the greatest potential for simple integration into current forensic operations and does not interfere with IGSR deposits. 24 The authors explicitly recognize that there are additional considerations regarding analysis of OGSR recovered from hands such as sampling efficiency, persistence, transfer, and interferences that affect the forensic interpretation of OGSR evidence for legal purposes. These are not explored in the current work, in favor of focusing on the performance of the instrument itself.…”

Section: ■ Introductionmentioning

confidence: 99%

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Armed with the Facts: A Method for the Analysis of Smokeless Powders by Ambient Mass Spectrometry

Bonnar

Popelka-Filcoff

Kirkbride

2020

J. Am. Soc. Mass Spectrom.

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The work presented here follows several others in investigating what capabilities, if any, ambient mass spectrometry might have toward the analysis of compounds commonly associated with smokeless propellant powders. This family of instrumental techniques has attracted curiosity from the field of forensic science due to its desirable properties such as rapid collection of information-rich data, combined with minimal requirements for sample mass and preparation. Experiments were conducted with a "Direct Sample Analysis" ion source integrated with a time-of-flight mass spectrometer. The ionization behaviors of nitroglycerin, methyl and ethyl centralite, akardite, diphenylamine, nitrosodiphenylamine, and nitrated diphenylamine derivatives were investigated specifically, with accuratemass data presented for each. Diphenylamine standards were used to demonstrate the performance of this instrument, which exhibited good response linearity across 1 order of magnitude and sub-nanogram detection limits. Thirty smokeless powder extracts, recovered from ammunition potentially in circulation within Australia, were analyzed to determine whether the technique is appropriate for rapid analysis of smokeless powder particles. Results demonstrated that the technique might be applied to compare individual particles with each other or to a database. Such a capability may be of value in the examination of explosive devices containing smokeless powder, postblast residues therefrom, or muzzle discharge from a close-range shooting. However, when efforts were made to detect residues from the hands of a volunteer shooter, only some returned positive results, and a high background signal from the sample collection stub indicates that detection using this instrument is thus far insufficiently reliable.

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The relevance of gunshot residues in forensic science

Minzière

Gassner

Gallidabino

et al. 2022

WIREs Forensic Science

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Gunshot residues (GSR) are routinely exploited by forensic scientists in the investigation of firearm-related events. While many new techniques are daily reported in the literature for the analysis of GSR, there is still a significant lack of data on the transfer, persistence, and prevalence of GSR. Such fundamental knowledge is essential to fully exploit the information potential of GSR for investigation or in Court. This article provides an overview of the relevant questions related to GSR, more particularly to infer about the trace's origin (i.e., is it from a firearm discharge?) and the activity that caused transfer (e.g., primary, secondary, or subsequent transfer). GSR production and composition will be briefly described, considering both inorganic and organic components. Then, the available knowledge about the primary transfer, the secondary transfer, and the persistence of GSR will be outlined, as well as the prevalence (background level) of the targeted elements and/or compounds in the environment, more particularly on the hands of people unrelated to firearm incidents. Finally, the methods developed for the collection, analysis, and interpretation of GSR will be discussed. A holistic approach combining fundamental forensic science knowledge about GSR transfer, persistence, and prevalence together with other available information is discussed as a path forward to increase the relevance and value of the GSR trace in practice.

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Tandem detection of organic and inorganic gunshot residues using LC–MS and SEM-EDS

Cited by 20 publications

References 32 publications

Nondestructive discrimination of red silk single fibers using total reflection X‐ray fluorescence spectrometry and synchrotron radiation X‐ray fluorescence spectrometry

Nondestructive discrimination of red silk single fibers using total reflection X‐ray fluorescence spectrometry and synchrotron radiation X‐ray fluorescence spectrometry

Armed with the Facts: A Method for the Analysis of Smokeless Powders by Ambient Mass Spectrometry

The relevance of gunshot residues in forensic science

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