Norwegian Defence Research Establishment (FFI), P.O. Box 25, NO-2027 Kjeller, Norway.
J Chromatogr A. 2010 Apr 2;1217(14):2171-8. doi: 10.1016/j.chroma.2010.01.088. Epub 2010 Feb 6.
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.
采用顶空捕集与气相色谱-质谱联用（GC-MS）方法，开发了用于土壤样品中硫芥（HD）和一些相关环状硫化合物痕量测定的方法。该方法优化中使用了两种截然不同类型的土壤（沙壤土和粉质壤土）。在分析之前，将饱和氯化钠的水按水与土壤 1:1 的比例加入到样品中。HD 的检测限达到 3ng/g，而环状硫化合物 1,4-噻恶烷、1,3-二硫戊环和 1,4-二噻烷可以在 0.2-0.7ng/g 时被检测到。该方法在定量下限（LOQ）到 100 倍 LOQ 的浓度范围内进行了验证。在 50 倍 LOQ 时，环状硫化合物测定的日内精密度为相对标准偏差（RSD）6.9-7.3%，HD 测定的 RSD 为 15%。两种土壤类型的回收率在 43-60%范围内。由于该技术需要很少的样品制备，因此样品处理和分析的总时间不到 1 小时。该技术成功地用于测定已知含有 HD 降解产物的化学弹药旧倾卸场沉积物样品中的环状硫化合物。
