顶空固相微萃取气相色谱法测定浓海水中的氯酚  

Determination of Chlorophenols in Desalinated Seawater by Headspace Solid Phase Microextraction-Gas Chromatography

作　　者：刘静[1] 曾兴宇[1] 周东星[1] 赵静红[1] 潘献辉[1] Liu Jing;Zeng Xingyu;Zhou Dongxing;Zhao Jinghong;Pan Xianhui(Institute of Seawater Desalination and Multipurpose Utilization, State Oceanic Administration, Tianjin　300192, China)

机构地区：[1]国家海洋局天津海水淡化与综合利用研究所,天津300192

出　　处：《化学分析计量》2016年第4期31-34,共4页Chemical Analysis And Meterage

基　　金：海洋公益性行业科研专项经费项目(201305039);国家海洋局业务化项目(YWZC2015–03);海水淡化与综合利用创新服务平台–膜法海水淡化技术创新服务平台项目(cxsf2014–34–B)

摘　　要：建立浓海水中氯酚的顶空固相微萃取气相色谱法检测方法。采用顶空固相微萃取对海水淡化排放的浓海水样品中2，4，6- 三氯酚(2，4，6-TCP) 和五氯酚(PCP) 进行分离富集，气相色谱– 电子捕获检测器(μECD) 测定浓海水样品中2，4，6-TCP 和PCP 的含量。讨论了萃取时间、萃取温度、水样盐度等实验条件对富集效率的影响，确定了萃取时间为40 min，萃取温度为60℃。2，4，6-TCP，PCP 的质量浓度在0.500～20.0 μg／L 范围内与其色谱峰面积呈良好的线性关系，线性相关系数均大于0.999，2，4，6-TCP 和PCP 的检出限(2S／N) 分别为0.055，0.128 μg／L，测定结果的相对标准偏差为3.65%～11.4%(n=6)，加标回收率为73.5%～119.0%。该方法快速，灵敏度高，适合于浓海水中氯酚的分析。The method for determination of chlorophenol in concentrated seawater by headspace solid phase microextraction–gas chromatography was established. 2,4,6-trichlorophenol (2,4,6-TCP) and pentachlorophenol (PCP) in concentrated seawater were separated and enriched by using headspace solid phase microextraction(HS–SPME),and then determined by gas chromatography with an electron capture detector(μECD). Determination parameters such as extraction time,extraction temperature and salinity were discussed. 2,4,6-TCP and PCP were extracted at 60℃ for 40 min.The detection limits of 2,4,6-TCP and PCP were 0.055,0.128 μg/L, respectively. The mass concentration of 2,4,6-TCP and PCP was linear with its chromatographic peak areas in the range of 0.500–20.0 μg/L, the correlation coefficients were more than 0.999. The RSD of determination results was 3.65%–11.4%(n=6) for 2,4,6-TCP and PCP. The recovery was 73.5%–119.0%. The method is rapid, has high sensitivity, which is suitable for the analysis of chlorophenol in concentrated seawater.

关 键 词：顶空固相微萃取 气相色谱法 浓海水 2 4 6- 三氯酚 五氯酚 

分 类 号：O657.7[理学—分析化学]