TATP in post explosion exhibits was reported earlier to be best recovered from vapor phase. A typical procedure includes its adsorption on Amberlite XAD-7, elution with acetonitrile and analysis by GC/MS. In this work, improved recovery of TATP from the vapor phase was achieved by SPME using PDMS/DVB fiber and immediate sampling to GC/MS. The recovery of TATP by SPME was compared with headspace and with adsorption on Amberlite XAD-7 by spiking onto filter paper put in a 100 mL beaker. The limit of detection of TATP was 6.4 ng in these conditions, few orders magnitude more than in the other tested methods. Recovery of TATP in the presence of various solvents was also studied. Acetone, water, and mixtures of water:alcohols (1:1) were found to reduce the recovery of TATP. Using SPME, TATP has been identified in dozens of post-explosion cases.
Experiments were conducted to collect gunpowder (propellant) residues from shooters' clothing by vacuum and to analyze them by gas chromatography/thermal energy analyzer (GC/TEA), ion mobility spectrometry (IMS), and gas chromatography/mass spectrometry (GC/MS). The residues were collected on fiberglass and Teflon filters using the portable vacuum sampler, all supplied with the IMS instrument. Several solvents were examined for the extraction of the propellant components from the filters. The extracts were centrifuged and/or filtered, concentrated by evaporation, and analyzed without any additional clean-up procedure. Based on the results of the study, an operational method for analysis of gunpowder residues was introduced into casework without changing the present operational technique for gunshot (primer) residue (GSR) analysis on clothing implemented by the Israel Police. In the modified method, the clothing is first sampled by double-side adhesive-coated aluminum stubs (the tape-lift method) for GSR analysis (the existing method), followed by vacuum collection for propellant residue examination. The issue of interpretation of the analytical results is discussed.
A sensitive, specific and simple color test for the improvised explosive urea nitrate is described. It is based on the formation of a red pigment upon the reaction between urea nitrate and p-dimethylaminocinnamaldehyde (p-DMAC) under neutral conditions. Urea itself, which is the starting material for urea nitrate, does not react with p-DMAC under the same conditions. Other potential sources of false positive response e.g., common fertilizers, medications containing the urea moiety and various amines, do not produce the red pigment with p-DMAC. Exhibits collected from 10 terrorist cases have been tested with p-DMAC. The results were in full agreement with those obtained by instrumental techniques including GC/MS, XRD and IR.
[reaction: see text] TATP gives rise to two separable conformations because the barrier for interconversion between them is relatively high at room temperature. This kind of behavior is rare in cyclic organic systems and is the result of poor overlap in the "flip-flop" transition state. The crystal structure of the analogous tricyclohexanone triperoxide also indicates the presence of two conformers.
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