顶空固相微萃取-GC/FPD测定废水中二甲基硫和二甲基二硫  

Headspace Solid Phase Microextraction Combined with GC/FPD for Dimethylsulfide and Dimethyldisulfide Determination in Wastewater

作　　者：董入源[1,2] 冯琳[1,2,3] 黄玉明[1,2] 

机构地区：[1]西南大学化学化工学院,重庆400715 [2]三峡库区生态环境教育部重点实验室,重庆400715 [3]重庆师范大学化学学院,重庆400047

出　　处：《西南大学学报（自然科学版）》2010年第5期126-130,共5页Journal of Southwest University(Natural Science Edition)

基　　金：863计划(2008AA06Z312);重庆市科技攻关资助项目(2009AB7028)

摘　　要：建立了顶空固相微萃取(HS-SPME)和气相色谱/火焰光度法(GC/FPD)联用测定人工湿地废水中二甲基硫和二甲基二硫的方法.研究了萃取纤维头的种类、萃取温度、pH值、离子强度、样品量等对HS-SPME的影响.载气为高纯氮气,流速为1.5mL/min,色谱柱为DB-VRX毛细管柱(1.4μm,60m×0.25mm),柱温:始温50℃,以8℃/min升至120℃保持2min后,以6℃/min升至180℃保持3min;在优化的实验条件下,测定二甲基硫和二甲基二硫的线性范围分别是1060～13780ng/L和159～4240ng/L,检出限分别为1020ng/L和140ng/L;相对标准偏差小于7%;废水样品加标回收率分别为85%～114%和105%～113%,用于实际水样分析获得满意结果.A new method based on combined application of headspace solid phase microextraction（HS-SPME）and gas chromatography/flame photometric detection（FPD）is proposed in this paper for the determination of dimethyl sulfide and dimethyl disulfide in wastewater from constructed wetlands.In our experiment,various parameters,including type of fibers,extraction temperature,pH,ionic strength and sample volume,were investigated for optimization of HS-SPME performance for dimethylsulfide and dimethyldisulfide.The DB-VRX capillary column（1.4 μm,60 m×0.25 mm）was used for separation of dimethylsulfide and dimethyldisulfide with 1 mL /min of high purity nitrogen as carrier gas by GC.The initial oven temperature was 50 ℃,then was programmed at a rate of 8 ℃ /min until 120 ℃,holding 2 min,and then at a rate of 6 ℃ /min until 180 ℃,holding the final temperature for 3 min.The enriched targets were detected by FPD.Under the optimized conditions,the linear dynamic ranges were 1 060-13 780 and 159-4 240 ng/L and the detection limits（3σ）were 1 020 ng/L and 140 ng/L for dimethylsulfide and dimethyldisulfide,respectively.The relative standard deviations for the determination of the compounds studied were less than 7%.By using dimethyl sulphide as internal standard,the proposed method was successfully applied to the analysis of dimethylsulfide and dimethyldisulfide in wastewater and their recoveries were in the range of 85%-114% and 105%-113%,respectively.

关 键 词：顶空固相微萃取 气相色谱-火焰光度法 烷基硫 人工湿地 

分 类 号：X502[环境科学与工程—环境工程]