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Molybdenum in Gunshot Residue: Experimental Evidences and Detection Challenges in the Presence of Lead and Sulfur

Published online by Cambridge University Press:  07 May 2021

Felice Nunziata
Affiliation:
Dipartimento di Matematica e Fisica, Università degli studi della Campania Luigi Vanvitelli, viale Lincoln 5, 81100Caserta, Italy
Francesco Saverio Romolo*
Affiliation:
Dipartimento di Giurisprudenza, Università degli studi di Bergamo, via Moroni 255, 24127Bergamo, Italy
Bryan Burnett
Affiliation:
Meixa Tech, 1624 Debann Road, Cardiff-by-the-Sea, CA92007, USA
Luigi Manna
Affiliation:
Arma dei Carabinieri, Reparto Investigazioni Scientifiche di Parma, Parco Ducale 3, 43125Parma, Italy
Stefano Orsenigo
Affiliation:
Arma dei Carabinieri, Reparto Investigazioni Scientifiche di Parma, Parco Ducale 3, 43125Parma, Italy
Matteo Donghi
Affiliation:
Arma dei Carabinieri, Reparto Investigazioni Scientifiche di Parma, Parco Ducale 3, 43125Parma, Italy
*
*Author for correspondence: Francesco Saverio Romolo, E-mail: francescosaverio.romolo@unibg.it
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Abstract

Inorganic gunshot residue (GSR) analysis is carried out by scanning electron microscopy/energy-dispersive X-ray spectroscopy (SEM/EDS) in many forensic laboratories. Characteristic GSR often consists of lead–barium–antimony, commonly associated with sulfur. The strength of forensic GSR evidence increases when unusual elements are found in residues collected both from the suspect and from the discharged firearm. The presence of molybdenum in GSR, due to the use of MoS2 lubricants in firearms, is experimentally demonstrated here for the first time. The most intense molybdenum X-ray emissions are MoL peaks at 2.3 keV which overlap with PbM and SK families due to the poor resolution of EDS detectors. When Pb, S, and Mo are allegedly present in the same particle, the reliability of automatic EDS routines is at risk. Missing identifications or false detections and exclusions may then occur. Molybdenum should be considered as detected only if MoK emissions meet the peak-to-background ratio minimum requirements. A strategy to spot Mo-containing residues is described, based on the automated search of MoS2, using a new “Sulfur only” class added to the classification scheme, followed by careful manual review of all GSR particles at an acceleration voltage of 30 kV. Our proposal improves commonly adopted forensic procedures currently followed in casework.

Type
Materials Science Applications
Copyright
Copyright © The Author(s), 2021. Published by Cambridge University Press on behalf of the Microscopy Society of America

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References

ASTM E1588-16 (2016). Standard guide for gunshot residue analysis by scanning electron microscopy/energy dispersive X-ray spectrometry. In Book of Standards, Vol. 14.02. West Conshohocken: ASTM International. doi:10.1520/E1588-16.Google Scholar
ASTM E1588-20 (2020). Standard practice for gunshot residue analysis by scanning electron microscopy/energy dispersive X-ray spectrometry. In Book of Standards, Vol. 14.02. West Conshohocken: ASTM International. doi: 10.1520/E1588-20.Google Scholar
Blakey, LS, Sharples, GP, Chana, K & Birkett, JW (2018). Fate and behaviour of gunshot residue—A review. J Forensic Sci 63(1), 919.CrossRefGoogle ScholarPubMed
Boyle, P, Humphrey, A & Courtney, M (2012). Quantifying friction effects of molybdenum disulfide, tungsten disulfide, hexagonal boron nitride, and Lubalox as bullet coatings. US DoD Research Report ADA568594. Available at https://apps.dtic.mil/sti/citations/ADA568594 (last accessed November 16, 2020).Google Scholar
Brede, U, Hagel, R, Redecker, KH & Weuter, W (1996). Primer compositions in the course of time: From black powder and SINOXID to SINTOX compositions and SINCO booster. Propellants, Explos, Pyrotech 21, 113117.CrossRefGoogle Scholar
CFG (2020). Catalogo Generale CFG 2020. Prodotti tecnici la per manutenzione professionale e il fai da te. p. 63. Available at https://www.cfg.it/cataloghi/Catalogo%20Generale%20CFG%202020.pdf (last accessed March 17, 2021).Google Scholar
Charles, S, Nys, B & Geusens, N (2011). Primer composition and memory effect of weapons—Some trends from a systematic approach in casework. Forensic Sci Int 212, 2226.10.1016/j.forsciint.2011.05.001CrossRefGoogle ScholarPubMed
Costa, AR, Motta, LC, Destefani, CA, Rodrigues, RRT, do Espirito Santo, KS, Aquije, GMFV, Boldrini, R, Athayde, GPB, Carneiro, MTWD & Romao, W (2016). Gunshot residues (GSR) analysis of clean range ammunition using SEM/EDX, colorimetric test and ICP-MS: A comparative approach between the analytical techniques. Microchem J 129, 339347.CrossRefGoogle Scholar
Dalby, O, Butler, D & Birkett, JW (2010). Analysis of gunshot residue and associated materials—A review. J Forensic Sci 55(4), 924943.CrossRefGoogle ScholarPubMed
Donghi, M, Orsenigo, S, Niewoehner, L, Barth, M, Fiocchi, C & Pomi, A (2019). A new ammunition for forensic needs: FIOCCHI-RIS. Forensic Chem 13, 100159.CrossRefGoogle Scholar
French, J & Morgan, R (2015). An experimental investigation of the indirect transfer and deposition of gunshot residue: Further studies carried out with SEM–EDX analysis. Forensic Sci Int 247, 1417.CrossRefGoogle ScholarPubMed
French, J, Morgan, R & Davy, J (2014). The secondary transfer of gunshot residue: An experimental investigation carried out with SEM-EDX analysis. X-ray Spectrom 43(1), 5661.CrossRefGoogle Scholar
French, JC, Morgan, RM, Baxendell, P & Bull, PA (2012). Multiple transfers of particulates and their dissemination within contact networks. Sci Justice 52(1), 3341.CrossRefGoogle ScholarPubMed
Goldstein, JI, Newbury, DE, Joy, DC, Lyman, CE, Echlin, P, Lifshin, E, Sawyer, L & Michael, JR (2003). Scanning Electron Microscopy and X-ray Microanalysis, 3rd ed. New York: Springer Science + Business Media LLC.CrossRefGoogle Scholar
Gunaratnam, L & Himberg, K (1994). The identification of gunshot residue particles from lead-free Sintox ammunition. J Forensic Sci 39(2), 532536.CrossRefGoogle Scholar
Harris, A (1995). Analysis of primer residue from CCI Blazer® lead free ammunition by scanning electron microscopy/energy dispersive X-ray. J Forensic Sci 40(1), 2730.CrossRefGoogle Scholar
Izraeli, ES, Tsach, T & Levin, N (2014). Optimizing FEG-SEM combined with an SDD EDX system for automated GSR analysis. X-ray Spectrom 43(1), 2937.CrossRefGoogle Scholar
Kazimirov, VI, Zorin, AD & Zanozina, VF (2006). Application of X-ray fluorescence analysis to investigation of the composition of gunshot residues. J Appl Spectrosc 73(3), 359365.CrossRefGoogle Scholar
Laflèche, DJN, Brière, SJJ, Faragher, NF & Hearns, NGR (2018). Gunshot residue and airbags: Part I. Assessing the risk of deployed automotive airbags to produce particles similar to gunshot residue. J Can Soc Forensic Sci 51, 4857.CrossRefGoogle Scholar
Lindsay, E, McVicar, MJ, Gerard, RV, Randall, ED & Pearson, J (2011). Passive exposure and persistence of gunshot residue (GSR) on bystanders to a shooting: Comparison of shooter and bystander exposure to GSR. J Can Soc Forensic Sci 44(3), 8996.CrossRefGoogle Scholar
Luten, R, Neimke, D, Barth, M & Niewoehner, L (2018). Investigating airborne GSR particles by the application of impactor technology. Forensic Chem 8, 7281.CrossRefGoogle Scholar
Maitre, M, Kirkbride, KP, Horder, M, Roux, C & Beavis, A (2017). Current perspectives in the interpretation of gunshot residues in forensic science: A review. Forensic Sci Int 270, 111.CrossRefGoogle ScholarPubMed
Newbury, DE (2009). Mistakes encountered during automatic peak identification of minor and trace constituents in electron-excited energy dispersive X-ray microanalysis. Scanning 31(3), 91101.CrossRefGoogle ScholarPubMed
Newbury, DE & Ritchie, NWM (2015). Performing elemental microanalysis with high accuracy and high precision by scanning electron microscopy/silicon drift detector energy-dispersive X-ray spectrometry (SEM/SDD-EDS). J Mater Sci 50, 493518.CrossRefGoogle Scholar
Rijnders, MR, Stamouli, A & Bolck, A (2010). Comparison of GSR composition occurring at different locations around the firing position. J Forensic Sci 55(3), 616623.CrossRefGoogle ScholarPubMed
Ritchie, NWM (2011). Standards-based quantification in DTSA-II—Part I. Microsc Today 19(5), 3036.CrossRefGoogle Scholar
Romanò, S, De Giorgio, F, D'Onofrio, C, Gravina, L, Abate, S & Romolo, FS (2020). Characterisation of gunshot residues from non-toxic ammunition and their persistence on the shooter's hands. J Leg Med 134, 10831094.CrossRefGoogle ScholarPubMed
Romolo, FS, Bailey, MJ, De Jesus, J, Manna, L & Donghi, M (2019). Unusual sources of Sn in GSR. An experimental study by SEM and IBA. Sci Justice 59(2), 181189.CrossRefGoogle ScholarPubMed
Romolo, FS & Margot, P (2001). Identification of gunshot residue: A critical review. Forensic Sci Int 119(2), 195211.CrossRefGoogle Scholar
Romolo, FS, Stamouli, A, Romeo, M, Cook, M, Orsenigo, S & Donghi, M (2017). An experimental study about the presence of selenium in inorganic gunshot residues (GSR). Forensic Chem 4, 5160.CrossRefGoogle Scholar
Torre, C, Mattutino, G, Vasino, V & Robino, C (2002). Brake linings: A source of non-GSR particles containing lead, barium, and antimony. J Forensic Sci 47(3), 494504.CrossRefGoogle ScholarPubMed
von Hertz, E & Rathsburg, H (1932). Priming composition. US Patent 1889116. Available at https://www.uspto.gov/ (last accessed November 15, 2020).Google Scholar
Winer, WO (1967). Molybdenum disulfide as a lubricant: A review of the fundamental knowledge. Wear 10(6), 422452.CrossRefGoogle Scholar
Zeichner, A, Levin, N & Springer, E (1991). Gunshot residue particles formed by using different types of ammunition in the same firearm. J Forensic Sci 36(4), 10201026.CrossRefGoogle Scholar