液-液萃取与气相色谱-质谱联用测定环境样品中的单质硫  

Determination of Elemental Sulfur in Environmental Samples by Liquid-Liquid Extraction Coupled with GC-MS

作　　者：刘卫国[1,2] 梁存珍[2] 於俊杰[3] 韩超南[2] 

机构地区：[1]武汉理工大学资源与环境工程学院,武汉市洪山区珞狮路122号430070 [2]北京石油化工学院环境工程系 [3]环境保护部环境与经济政策研究中心

出　　处：《光谱实验室》2012年第3期1403-1406,共4页Chinese Journal of Spectroscopy Laboratory

基　　金：北京科技新星计划资助项目(2008B25);环保部公益性行业科研专项(200909054);环境治理与调控技术北京市优秀教学团队资助项目(PHR201107213)

摘　　要：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。A sensitive method was developed for the determination of elemental sulfur in complex environmental matrixes via the liquid-liquid extraction method followed by gas chromatography-mass spectrometry（GC-MS）.Effects of extraction solvents,chromatography column and heating oven temperature programme on the determination were investigated.The results showed that：as a solvent for the elemental sulfur extraction,CS2 was better than CCl4.For HP-1MS column,there was a better peak shape of elemental sulfur at the oven temperature of 270 ℃ constant for 10 min,while both the peak shape and the sensitivity from HP-5MS column were better than that from HP-1MS column.The linear range for elemental sulfur was 5—200mg/L with the coefficient of determination R2 of 0.9980,and the minimum limit of quantitation was 0.106mg/L.The relative standard deviation for the determination of five replicates of 5mg/L elemental sulfur in water was 3.179%.The method has been applied to determining elemental sulfur in biological desulfurization reactor effluent with good results.

关 键 词：单质硫 液液萃取 气相色谱-质谱法 生物脱硫反应器 

分 类 号：O657.63[理学—分析化学]