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液液萃取—GC-MS法同时测定石化废水中双酚A和邻苯二甲酸二乙酯
引用本文:陈婷婷,席宏波,周岳溪,章丽萍.液液萃取—GC-MS法同时测定石化废水中双酚A和邻苯二甲酸二乙酯[J].化工环保,2018,38(6):744-749.
作者姓名:陈婷婷  席宏波  周岳溪  章丽萍
作者单位:1. 中国矿业大学(北京)化学与环境工程学院,北京 100083;2. 中国环境科学研究院 水污染控制技术研究中心,北京 100012;3. 中国环境科学研究院 环境基准与风险评估国家重点实验室,北京 100012
基金项目:国家水体污染控制与治理科技重大专项课题(2017ZX07402-002)
摘    要:建立了液液萃取(LLE)—气相色谱-质谱(GC-MS)法同时测定石化废水中双酚A(BPA)和邻苯二甲酸二乙酯(DEP)的新方法,对液液萃取条件进行了优化。最佳的液液萃取条件为:萃取剂为乙酸乙酯,水样调成酸性(pH<2),每次加入萃取剂0.1 mL/mL、盐析剂NaCl 0.1 g/mL,萃取次数为6次,每次萃取时间为2 min。实验结果表明:在质量浓度1~100 mg/L的范围内,BPA和DEP测定标准曲线的线性关系良好;BPA和DEP的检出限(LOD)分别为5.18 μg/L和0.89 μg/L,定量限(LOQ)分别为17.11 μg/L和2.96 μg/L,回收率为81.4 %~124.9 %,相对标准偏差(RSD)(n=7)小于5.5 %。

关 键 词:液液萃取  气相色谱-质谱  环境雌激素  双酚A  邻苯二甲酸二乙酯  同时测定  
收稿时间:2018-02-02

Simultaneous determination of bisphenol A and diethyl phthalate in petrochemical wastewater by liquid-liquid extraction - gas chromatography-mass spectrometry
CHEN Tingting,XI Hongbo,ZHOU Yuexi,ZHANG Liping.Simultaneous determination of bisphenol A and diethyl phthalate in petrochemical wastewater by liquid-liquid extraction - gas chromatography-mass spectrometry[J].Environmental Protection of Chemical Industry,2018,38(6):744-749.
Authors:CHEN Tingting  XI Hongbo  ZHOU Yuexi  ZHANG Liping
Institution:1. School of Chemical and Environmental Engineering,China University of Mining and Technology (Beijing),Beijing 100083,China;2. Research Center of Water Pollution Control Technology,Chinese Research Academy of Environmental Sciences,Beijing 100012,China;3. State Key Laboratory of Environmental Criteria and Risk Assessment,Chinese Research Academy of Environmental Sciences,Beijing 100012,China
Abstract:A method of liquid-liquid extraction(LLE)coupled with gas chromatography-mass spectrometry (GC-MS)for simultaneous determination of bisphenol A(BPA)and diethyl phthalate (DEP)environmental estrogens in petrochemical wastewater was developed,and the conditions of LLE were optimized. The best conditions of LLE were as follows:the extraction solvent ethyl acetate,the sample pH made acidic (pH<2),the extractant added by 0.1 mL/mL each time,salting-out agent NaCl 0.1 g/mL,6 times of extraction ,and each extraction time 2 min. The experimental results indicated that:In the range of mass concentration was 1-100 mg/L for BPA and DEP,the linearity of their standard curves are good;the limits of detection (LODs)and limits of quantitative (LOQs)were 5.18,17.11 μg/L for BPA and 0.89,2.96 μg/L for DEP,and the average recoveries were in the range of 81.4 %-124.9 % with the relative standard deviation (RSD)less then 5.5% (n=7).
Keywords:liquid-liquid extraction (LLE)  gas chromatography-mass spectrometry (GC-MS)  environmental estrogen  bisphenol A (BPA)  diethyl phthalate (DEP)  simultaneous detection  
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