色谱

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气相色谱-质谱法测定饮用水中的卤乙酸

汪昆平1,2,邓荣森1,李伟民1,王涛1

  

  1. 1.Key Laboratory of the Three Gorges Reservoir Region’s Eco-Environment of Ministry of Education, Chongqing University, Chongqing 400045, China; 2.Chengdu Army Institute of Science Research and Engineering Design, Kunming 650031, China
  • 收稿日期:2004-12-23 修回日期:2005-11-21 出版日期:2006-01-30 发布日期:1987-09-25
  • 通讯作者: 邓荣森

Analysis of Haloacetic Acids in Drinking Water by Gas Chromatography-Mass Spectrometry

WANG Kunping1,2, DENG Rongsen1, LI Weimin1, WANG Tao1   

  1. 1.Key Laboratory of the Three Gorges Reservoir Region’s Eco-Environment of Ministry of Education, Chongqing University, Chongqing 400045, China; 2.Chengdu Army Institute of Science Research and Engineering Design, Kunming 650031, China
  • Received:2004-12-23 Revised:2005-11-21 Online:2006-01-30 Published:1987-09-25

摘要:

参照美国EPA Method 552.3方法中的液-液微萃取、酸化甲醇衍生化技术,以高纯水代替甲基叔丁基醚(MTBE)做溶剂配制标准贮备液,采用气相色谱/质谱联用技术对饮用水中的卤乙酸(HAAs)进行测定。结果表明:在所确立的检测条件下,样品分析时间短,内标、HAAs组分峰在谱图上能够得到很好的分离。低、中、高3个浓度水平的加标水样的HAAs回收率为82%~103%。该方法的检测限:二氯乙酸为0.72 μg/L、三氯乙酸为0.44 μg/L。用水做溶剂配制的标准贮备液在4 ℃条件下贮存时,贮存时间为2个月。

关键词: 卤乙酸, 气相色谱/质谱, 衍生化 , 饮用水

Abstract:

Based on liquid-liquid micro-extraction and acidic methanol derivatization methods from EPA Method 552.3, a gas chromatographic-mass spectrometric (GC-MS) method has been studied for determining haloacetic acid (HAAs) in drinking water using ultrapure water instead of methyl tert-butyl ether (MTBE) as solvent for preparing standard stock solution. The results showed that the peaks of 1,2-dibromo propane (internal standard) and HAAs were separated very well. With the improved method, the recoveries for HAAs (82%-103%) were high at concentrations ranging from 5 to 80 μg/L, the detection limits for dichloroacetic acid (DCAA) and trichloroacetic acid (TCAA) were 0.72 and 0.44 μg/L. With the improved method, the runtime could be also significantly reduced without compromising the analytical resolutions. It is also demonstrated that the stock standard was stable under storage for 2 months at 4 ℃.

Key words: derivatization , drinking water, haloacetic acids, gas chromatography-mass spectrometry (GC-MS)