CAPILLARY COLUMN ELECTRON-IMPACT AND AMMONIA CHEMICAL-IONIZATION GAS-CHROMATOGRAPHIC MASS-SPECTROMETRIC AND GAS-CHROMATOGRAPHIC TANDEM MASS-SPECTROMETRIC ANALYSIS OF MUSTARD HYDROLYSIS PRODUCTS

Capillary column GC-MS and GC-MS-MS, under electron impact (EI) and ammonia chemical ionization (CI) conditions, were used to detect and identify longer-chain sulfur vesicant hydrolysis products. Interpretation of the MS data enabled the characterization of the partial and fully hydrolysed products of 2-chloroethyl (2-chloroethoxy)ethyl sulfide, bis(2-chloro-ethylthio)ethane (sesquimustard) and bis[(2-chloroethylthio)ethyl] ether before and after trimethylsilyl derivatization. EI data were generally lacking in significant molecular ion information while those obtained during ammonia CI contained valuable (M + H)+ and/or (M + NH4)+ molecular ion information. The usefulness of this approach to degradation product analysis was demonstrated during the 3rd United Nations Conference on Disarmament Technical Group on Instrumentation Round Robin Analytical Exercise held in 1991. Both thiodiglycol and thiodiglycol sulfone. the mustard degradation compounds spiked onto concrete samples circulated to fifteen international laboratories. were confirmed during capillary column GC-MS and GC-MS-MS analysis of the samples.