顶空固相微萃取气相色谱-火焰光度法测定废水中烷基硫醇化合物  

Headspace Solid Phase Microextraction Combined with Gas Chromatography/Flame Photometric Detection for Analysis of Alkylthiols in Wastewater

作　　者：冯琳[1,2] 董入源[1] 黄玉明[1] 

机构地区：[1]西南大学化学化工学院,三峡库区生态环境教育部重点实验室,重庆400715 [2]重庆师范大学化学学院,重庆400047

出　　处：《分析化学》2009年第4期563-567,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.20477033);863计划(No.2008AA062312)资助项目

摘　　要：建立了顶空固相微萃取(HS-SPME)-气相色谱法测定人工湿地废水中烷基硫醇化合物的分析方法。详细研究了萃取参数如萃取涂层、萃取时间、萃取温度、样品体积、盐效应及样品pH值等对HS-SPME萃取乙硫醇(EtSH)、2-甲基-2-丙硫醇(Me-PrSH)、1-丙硫醇(1-PrSH)、2-丙硫醇(2-PrSH)、1-丁硫醇(1-BuSH)及环戊硫醇(CycloPeSH)(内标)的影响。富集的硫醇化合物经DB-VRX毛细管色谱柱分离,FPD检测。在优化的实验条件下,测定乙硫醇、2-甲基-2-丙硫醇、1-丙硫醇、2-丙硫醇、1-丁硫醇的线性范围介于0.12～16.21μg/L之间;检出限(3σ)介于0.97～22.11ng/L之间。以环戊硫醇为内标物质,将本法用于废水中硫醇化合物的测定,获得满意结果。A headspace solid phase microextraction combined with gas chromatography/flame photometric detection（FPD） has been developed for the analysis of alkyhhiols in wastewater from constructed wetlands. The effect of various extraction parameters such as extraction coatings, extraction time, temperature, sample volume, salt effect, sample pH value on the extraction of alkyhhiols, namely, ethanethiol（EtSH） , 2-methyl- 2-propanethiol（ Me-PrSH ）, 1 -propanethiol （ 1 -PrSH ）, 2-propanethiol （ 2-PrSH ）, 1 -butanethiol （ 1 -BUSH ） and cyclopentanethiol（CycloPeSH） were investigated and optimized. The enriched alkylthiols were separated by DB-VRX capillary column and detected by FPD. Under the optimized conditions, the linear dynamic ranges for EtSH, Me-PrSH, 1-PrSH, 2-PrSH, 1-BUSH were in the range of 0.12 - 16.21 μg/L. The detection limit （3σ） for the studied five alkylthiols was 0.97 -22.11 ng/L. By using CycloPeSH as internal standard, the proposed method has been successfully applied to the analysis of alkylthiols in wastewater from constructed wetlands with satisfactory results.

关 键 词：气相色谱 顶空固相微萃取 烷基硫醇化合物 人工湿地 

分 类 号：X832[环境科学与工程—环境工程]