Mapping explosive residues on galvanized pipe bomb fragments using total vaporization solid phase microextraction (TV-SPME)

摘要

Solid phase microextraction (SPME) is a popular sampling technique whereby analytes are sorbed to a coated fiber and subsequently desorbed into an analytical instrument. In headspace SPME, analytes partition between the sample, the headspace above the sample, and the SPME fiber coating. In total vaporization SPME (TV-SPME), sample extracts are heated until both the solvent and analytes completely vaporize, whereupon the analytes partition between the vapor phase and the SPME fiber. In this study, TV-SPME using a polyethylene glycol fiber was coupled with fast gas chromatography/mass spectrometry to identify components of double-base smokeless powder (DBSP). Nitroglycerin (NG), diphenylamine (DPA) and ethyl centralite (EC) were separated in under 5 min. For NG, the optimal sample volume (70 μL), extraction temperature (60 °C) and extraction time (20 min) resulted in a method that was over twelve fold more sensitive than traditional liquid injection and with a detection limit below 1 ppb. This method was then used to quantify DBSP residue on post-blast debris from five galvanized steel pipe bombs. The mean concentration of NG on the fragments was 0.25 ppm (w/w). An average of 1.01 mg of NG was recovered from the devices. Finally, the distribution of NG could be “mapped” by tracking the original locations of each fragment within the device. These maps showed that the distribution of NG was far from uniform. In fact, the concentration of the NG on fragments originating from the end caps was several fold higher than in other locations. This finding can help guide the selection of bomb fragments for chemical analyses in real-world scenarios.