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

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 accurate-mass 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.

Xylitol pentanitrate - Its characterization and analysis.

Xylitol is a polyhydric alcohol that may be nitrated to form an explosive (xylitol pentanitrate or XPN). Consequently, forensic and first response personnel may encounter XPN in post-blast residues or as a bulk material. Despite this, key analytical data for XPN that may be used in first response or forensic operations to aid its detection are not yet available in the literature. The present article provides infrared spectrometry, Raman spectrometry, nuclear magnetic resonance spectrometry, chromatography and mass spectrometry data in order to address this knowledge gap.

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

Gunshot residue (GSR) is a valuable form of forensic trace evidence in the investigation of firearms crime. The current gold-standard approach does not include the analysis of organic components of the residues, which may be a deficiency, particularly in cases where there is little to no inorganic gunshot residue (IGSR) present or its attribution to a firearm source is ambiguous. A solvent extraction method was used for the extraction of organic GSR (OGSR) from the most common sampling device used to collect IGSR (i.e., SEM stubs with double-sided carbon adhesive tape). It was found that extraction did not significantly disturb inorganic GSR present on stubs, which raises the possibility that a valuable, comprehensive tandem analysis of both organic and inorganic GSR may be implemented using a single and commonly used residue collection device. The organic extract was analysed using Ultra High Performance Liquid Chromatography coupled to an Ion Trap Mass Spectrometer using Electrospray Ionisation (UHPLC-ESI-MS/MS), with preliminary results indicating that organic components can be extracted and detected at levels appropriate to casework GSR analysis. Testing of traces collected from the hands of recent shooters showed detection of stabiliser compounds typical of OGSR, which were confirmed to be present in the test ammunition's propellant. Total analysis time is approximately 30min per specimen, including preparation, instrumental analysis and data review. As the first step in the examination of GSR stubs in relation to a shooting case, extraction of organics and analysing them for the presence of OGSR may bring two operational benefits. First, that approach may be a useful way to determine which stubs warrant priority examination for IGSR, and second, it offers the possibility of providing relatively rapid case information to investigators.