Nitrogen mustards analytical methods

A number of modifications/improvements to methods for the analysis of metabolites of sulfur and nitrogen mustards, and hydrolysis products of nerve agents, have been reported in a special issue of the Journal of Analytical Toxicology, 28 (5) (2004) pp. 305-392. 

Figure 4.9 Degradation products of Nitrogen Mustard N-methyldiethanolamine (MDEA), N-ethyldiethanolamine (EDEA) and triethanolamine (TEA) [31]. Reprinted from Executive Summary of Chemical Warfare Agents and their Hydrolysis Products from the US EPA Standardized Analytical Methods and GC-MS Analytical Method for the Analysis of Chemical Warfare Agent Degradation Products listed in the EPA Standardized Analytical Methods US EPA, Theodore A. Haigh...

Wils et al. (25,26) previously reported an entirely different approach to TDG analysis. TDG in urine was converted back to sulfur mustard by treatment with concentrated HC1. The sample treatment is less straightforward than the methods described above, but analysis as sulfur mustard is facile. Urine, plus 2H8-TDG as internal standard, was cleaned up by elution through two C18 cartridges. Concentrated HC1 was added and the sample stirred and heated at 120 °C. Nitrogen was blown over the solution and sulfur mustard isolated from the headspace by adsorption onto Tenax-TA. The method was used to detect TDG in urine from casualties of CW attacks (see below). A disadvantage of this method is that it may convert metabolites other than TDG to sulfur mustard. This is supported by the detection of relatively high levels of analytes in urine from control subjects. Vycudilik (27) used a similar procedure, but recovered the mustard by steam distillation and extraction. 

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