title: Headspace-trap gas chromatography-mass spectrometry for determination of sulphur mustard and related compounds in soil.
abstract: Methods for trace determination of sulphur mustard (HD) and some related cyclic sulphur compounds in soil samples have been developed using headspace-trap in combination with gas chromatography-mass spectrometry (GC-MS). Two quite different types of soil were employed in the method optimisation (sandy loam and silty clay loam). Prior to analysis, water saturated with sodium chloride was added to the samples, at a water to soil ratio of 1:1. A detection limit of 3 ng/g was achieved for HD, while the cyclic sulphur compounds 1,4-thioxane, 1,3-dithiolane and 1,4-dithiane could be detected at 0.2-0.7 ng/g. The methods were validated in the concentration range from the limit of quantification (LOQ) to hundred times LOQ. The within assay precision at fifty times LOQ was 6.9-7.3% relative standard deviation (RSD) for determination of the cyclic sulphur compounds, and 15% RSD for determination of HD. Recoveries were in the range of 43-60% from the two soil types. As the technique requires very little sample preparation, the total time for sample handling and analysis was less than 1h. The technique was successfully employed for the determination of cyclic sulphur compounds in a sediment sample from an old dumping site for chemical munitions, known to contain HD degradation products.
authors.affiliation: Norwegian Defence Research Establishment (FFI), P.O. Box 25, NO-2027 Kjeller, Norway. Bent-Tore.Roen@ffi.no
authors.forename: Bent T
authors.initials: BT
authors.lastname: Røen
authors.forename: Erik
authors.initials: E
authors.lastname: Unneberg
authors.forename: John Aa
authors.initials: JA
authors.lastname: Tørnes
authors.forename: Elsa
authors.initials: E
authors.lastname: Lundanes
mesh_terms: D002619:Chemical Warfare Agents / Q000032:analysis* / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D009151:Mustard Gas / Q000032:analysis* / Q000737:chemistry; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity; D012965:Sodium Chloride / Q000737:chemistry; D012987:Soil / Q000032:analysis*; D012989:Soil Pollutants / Q000032:analysis* / Q000737:chemistry; D013457:Sulfur Compounds / Q000032:analysis* / Q000737:chemistry; D013696:Temperature
chemical_list: D002619:Chemical Warfare Agents; D012987:Soil; D012989:Soil Pollutants; D013457:Sulfur Compounds; D012965:Sodium Chloride; D009151:Mustard Gas