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液-液萃取与气相色谱-质谱联用测定环境样品中的单质硫
引用本文:刘卫国,梁存珍,於俊杰,韩超南.液-液萃取与气相色谱-质谱联用测定环境样品中的单质硫[J].光谱实验室,2012,29(3):1403-1406.
作者姓名:刘卫国  梁存珍  於俊杰  韩超南
作者单位: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;北京石油化工学院环境工程系 北京市大兴区黄村镇清源北路19号 102617
2. 北京石油化工学院环境工程系 北京市大兴区黄村镇清源北路19号 102617
3. 环境保护部环境与经济政策研究中心 北京市西城区西直门南小街115号 100029
基金项目:北京科技新星计划资助项目,环保部公益性行业科研专项,环境治理与调控技术北京市优秀教学团队资助项目
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。

关 键 词:单质硫  液液萃取  气相色谱-质谱法  生物脱硫反应器

Determination of Elemental Sulfur in Environmental Samples by Liquid-Liquid Extraction Coupled with GC-MS
LIU Wei-Guo , LIANG Cun-Zhen , YU Jun-Jie , HAN Chao-Nan.Determination of Elemental Sulfur in Environmental Samples by Liquid-Liquid Extraction Coupled with GC-MS[J].Chinese Journal of Spectroscopy Laboratory,2012,29(3):1403-1406.
Authors:LIU Wei-Guo  LIANG Cun-Zhen  YU Jun-Jie  HAN Chao-Nan
Affiliation:b a(College of Resources and Environmental Engineering,Wuhan University of Science and Technology,Wuhan 430070,P.R.China)b(Department of Environmental Engineering,Beijing Institute of Petrochemical Technology,Beijing 102617,P.R.China)c(Policy Research Center for Environment and Economy,Minstry of Environmental Protection,Beijing 100029,P.R.China)
Abstract: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.
Keywords:Elemental Sulfur  Liquid-Liquid Extraction  GC-MS  Biological Desulfurization Reactor
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