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.
An improved synthesis of a family of amino acids that contain omega-aminoalkyl groups and of a new family containing omega-carboxyalkyl groups linked to the alpha-amine is described. The synthesis was performed by alkylation of suitably monoprotected alkylenediamines and protected omega-amino acids with triflates of alpha-hydroxy acid esters. The reaction proceeded with inversion of configuration yielding optically pure products. The N(alpha)-(omega-aminoalkyl)amino acids and N(alpha)-(omega-carboxyalkyl)amino acids were orthogonally protected to allow their incorporation into peptides by solid-phase peptide synthesis (SPPS) methodology.
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.
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