Preparation and Analysis of Samples for the Third Round Robin VerificationExercise

摘要

For the third international Round Robin verification exercise executed in thefall of 1991 the TNO-Prins Maurits Laboratory prepared the samples consisting of rubber, paint and concrete. These materials, which were selected to represent samples taken during an inspection at a military facility, were spiked with mustard gas and related vesicants as well as with decomposition products of mustard gas. Diesel fuel and an aromatic white spirit were added as a chemical background. In addition to a description of the spiked materials, details about the coding and transportation of the samples are presented. A number of procedures was developed for the analysis of the samples. Rubber, which was spiked with mustard gas and its disulphide, could either be analysed by extraction with a nonpolar solvent or by thermodesorption. The latter procedure had advantages for the analysis by gas chromatography-mass spectrometry (GC-MS). Paint was spiked with sesquimustard (Q) and dimustard ether (T). Determination of these compounds was based on extraction with a nonpolar solvent, followed by spectrometric analysis (GC-MS, NMR). Concrete was spiked with two polar decomposition products of mustard gas viz. thiodiglycol and its sulphone. Extraction with water followed by analysis with thermospray-liquid chromatography-mass spectrometry (TSP-LC-MS) turned out to be the best method for the quantitative determination. All compounds added were rather stable in the materials. After a period of 7 weeks they could still be recovered with reasonable or even good efficiencies. Mustard Gas, Samples, Rubber, Paint, Concrete.