Characterization of residual gunpowder recovered from articles of clothing utilizing thermal desorption GC/MS

Applications | 2018 | ShimadzuInstrumentation
GC/MSD, Thermal desorption, GC/SQ
Industries
Other
Manufacturer
Shimadzu

Significance of the topic

Gunshot residue (GSR) contains a complex mixture of organic and inorganic particles generated during firearm discharge. While scanning electron microscopy has traditionally focused on inorganic elements, the organic fraction—comprising propellant stabilizers, lubricants and combustion by-products—provides critical forensic information. Thermal desorption GC/MS offers a solvent-free, sensitive approach to detect these minute organic residues on various substrates, enhancing the toolkit available to crime laboratories.

Objectives and study overview

This study evaluates the application of thermal desorption GC/MS to recover and characterize organic GSR from 9 mm cartridge casings and clothing textiles. The goal is to compare this approach with conventional methanol extraction, assessing its ability to detect a broad range of stabilizers and accelerants without extensive sample preparation.

Methodology and instrumentation

A consistent lot of 9 mm ammunition was discharged and residues collected from (1) bulk gunpowder dissolved in methanol, (2) swabs of spent casings, and (3) swabs of chest and sleeve regions on clothing worn during firing. One microliter of each methanolic extract was loaded onto Tenax thermal desorption tubes. Tubes were desorbed at 250 °C onto a cold trap maintained at –20 °C, then rapidly heated to transfer analytes into a GC column. Full-scan mass spectrometry was performed over m/z 50–500 using a Shimadzu thermal desorption GC/MS system. Compound identities were confirmed via NIST17 library searches.

Main results and discussion

Thermal desorption GC/MS chromatograms revealed distinct organic profiles for gunpowder, spent casings and clothing swabs. Major residue compounds included nitroglycerin, carbazole, glycine, trimethylbenzene isomers, benzaldehyde, 2-furaldehyde and 2-pyrrolidinone. Quantitative area counts were significantly higher in casing samples compared to clothing, reflecting transfer efficiency and sampling delays. The technique successfully detected key stabilizers and accelerants that may be under-represented in traditional solvent methods.

Benefits and practical applications

  • Minimized solvent usage and reduced sample preparation time.
  • Enhanced sensitivity for diverse organic GSR constituents.
  • Non-destructive sampling preserves evidentiary value.
  • Applicability to substrates such as fabrics and metal casings.
  • Compatibility with existing forensic GC/MS workflows for rapid screening.

Future trends and potential applications

  • Development of portable thermal desorption GC/MS systems for field deployment.
  • Integration with high-resolution mass analyzers for improved compound identification.
  • Advanced sorbent materials to boost low-level residue capture.
  • Implementation of machine learning algorithms for pattern recognition in GSR profiles.
  • Expansion to security screening scenarios and on-site forensic analysis.

Conclusion

Thermal desorption GC/MS represents a robust, efficient method for organic GSR analysis, delivering enhanced sensitivity and streamlined sample preparation. Its ability to recover critical stabilizers and accelerants underscores its value for forensic casework, with future advancements poised to broaden its applicability.

Reference

  1. Dalby O, Butler D, Birkett JW. Analysis of gunshot residue and associated materials—a review. Journal of Forensic Sciences. 2010;55:924–943.
  2. Benito S, Abrego Z, Sánchez A, Unceta N, Goicolea MA, Barrio RJ. Characterisation of organic gunshot residues in lead-free ammunition using a new sample collection device for LC–QTOF MS. Forensic Science International. 2015;246:79–85.
  3. Weyermann C, Belaud V, Riva F, Romolo FS. Analysis of organic volatile residues in 9 mm spent cartridges. Forensic Science International. 2009;186:29–35.
  4. Reid L, Chana K, Bond JW, Almond MJ, Black S. Stubs versus swabs? A comparison of gunshot residue collection techniques. Journal of Forensic Sciences. 2010;55:753–756.

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