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采用液-液萃取与气相色谱-质谱联用测定复杂环境基质样品中的单质硫,研究萃取溶剂、色谱柱类型及炉温升温程序对分析方法的影响。实验结果表明:二硫化碳作为萃取溶剂好于四氯化碳。采用HP-1MS柱时,炉温在270℃恒温保持10min进行分析,单质硫峰形较好。采用HP-5MS柱,单质硫峰形及丰度均优于HP-1M S柱。该分析方法的线性范围为5—200mg/L,可决系数R2为0.9980,最低定量限0.106mg/L,测定5个5mg/L硫水混合液平行样的相对标准偏差为3.179%。生物脱硫反应器出水中单质硫测定结果表明,该检测方法是可行的。
Liquid-liquid extraction coupled with gas chromatography-mass spectrometry was used to determine elemental sulfur in complex environmental matrix samples. The effects of extraction solvent, column type and temperature program on the analytical method were studied. The experimental results show that carbon disulfide is better than carbon tetrachloride as extraction solvent. When HP-1MS column was used, the furnace temperature was maintained at 270 ° C for 10 min for analysis, and the elemental sulfur peak shape was better. HP-5MS column, elemental sulfur peak shape and abundance are better than the HP-1M S column. The linear range of the analytical method was 5-200mg / L, the coefficient of determination R2 was 0.9980, the lowest limit of quantification was 0.106mg / L. The relative standard deviation of 5 samples of 5mg / L sulfur water mixture was 3.179%. The determination results of elemental sulfur in the effluent of the biological desulfurization reactor show that the detection method is feasible.