Analysis of thiodiglycol in urine of victims of an alleged attack with mustard gas.

A procedure for the semi-quantitative determination of thiodiglycol, a metabolite of the vesicant mustard gas, in urine has been developed. Thiodiglycol was converted into mustard gas using concentrated HCl at temperatures close to 100 degrees C. The headspace of the solution containing mustard gas, was trapped on an adsorption tube filled with Tenax-GC which was subsequently analyzed by gas chromatography/mass spectrometry. Using 10 mL of urine, a detection limit of a few ng/mL of thiodiglycol was achieved. The procedure was applied to urine samples obtained from Iranian patients who were the alleged victims of an attack by chemical warfare agents (probably mustard gas). A number of control samples were investigated as well. Thiodiglycol was found in the urine of the Iranian patients in concentrations varying between 3 and 140 ng/mL. However, the detection of thiodiglycol in concentrations up to 55 ng/mL in control samples excluded the unambiguous verification of the use of mustard gas against the Iranian patients.

Chemical warfare agents: verification of compounds containing the phosphorus-methyl linkage in waste water.

The chemical analysis of the waste water from plants that manufacture chemicals is a nonintrusive method for confirming a suspected violation of the prohibition against the production of chemical warfare agents. The chemical structure of most nerve gases is related to that of methylphosphonic acid, whereas most organo-phosphorus pesticides have the phosphoric acid structure. On the basis of this characteristic difference, a procedure has been developed in which the presence of a nerve gas, its decomposition products, or its starting materials in waste water (Rhine River and Meuse River water) is reflected by the appearance of methylphosphonic acid as a breakdown product after hydrolysis. This acid is concentrated and converted into a volatile compound by methylation. After cleanup, the ester may be separated from related compounds by gas chromatography and is detected by means of a specific detector for phosphorus. The detection limit of nerve gases by this procedure is approximately 1 nanomole per liter of water. The scope and limitations of the method are discussed.