ABSTRACT
An automated thermal desorption (ATD)-gas chromatography-mass spectrometry method was developed for the analysis of selected chemical warfare (CW) agents. Suitable methods were developed for analytes of high volatility to low volatility. The less volatile CW agents required the purchase and installation of a high-temperature valve upgrade kit allowing valve temperatures of up to 260 degrees C to be reached. The limit of detection was 50 ng on the tube for most CW agents in full scan. Chloropicrin exhibited some temperature dependence, with detection limits improving as ATD temperatures were decreased below 150 degrees C. A sample storage trial was undertaken to establish the most suitable storage environment for CW agents adsorbed onto Tenax TA. Temperature and time of storage were found to influence recovery of analytes with best recoveries being observed after 1 day storage in a freezer (-12 degrees C). This method was evaluated during a trial of procedures for sampling and identification of chemical agents at Porton Down, UK. Sulfur mustard was detected downwind of a simulated exploded munition.
Subject(s)
Chemical Warfare Agents/analysis , Gas Chromatography-Mass Spectrometry/methods , Hot Temperature , Retrospective StudiesABSTRACT
Thiodiglycol (TDG) is the predominant hydrolysis product of the chemical warfare agent sulfur mustard. The extraction of TDG was investigated using pressurised liquid extraction and the results compared for a variety of different solvents and soils. TDG was analysed underivatised by gas chromatography with flame photometric detection. A mixture of methanol-water (9:1), proved to be the most efficient extracting solvent for TDG at a temperature of 150 degrees C and 10 MPa.
