Retrospective detection and identification of chemical warfare agents (CWAs) is important from the verification point of view of the Chemical Weapons Convention. In the present work, a novel method for determination of CWAs and their markers in water has been described. It is based on a single drop micro extraction (SDME) of analytes and gas chromatography/mass spectrometric identification. Extraction conditions, such as solvent selection, agitation, extraction time, and salt content, were found to have significant influence on SDME. The conditions optimized for extraction of CWAs were 1 microL CH2Cl2/CCl4 (3:1 v/v), 30-min extraction time, 300-rpm stirring rate, and with or without NaCl addition. Under optimized conditions, comparison of SDME, solid-phase microextraction, and liquid-liquid extraction was also made. The limit of detection by SDME ranged from 75 to 10 microg L(-1) at a signal-to-noise ratio of 10:1.

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This communication describes the synthesis and gas chromatography/mass spectrometric (GC/MS) analysis of N,N-dialkylphosphoramidic dihalides and alkylphosphonic difluorides, which are synthones of nerve agents. The study was undertaken with a view to developing a spectral database of these compounds for verification purposes of the Chemical Weapons Convention (CWC). The modified synthetic approach reported here has advantages over traditional syntheses in terms of time and yield. GC/MS analysis of these synthones yielded electron ionization (EI) mass spectra and, based on these spectra, generalized fragmentation routes are proposed that rationalize most of the characteristic ions.

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