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固相萃取—气相色谱法检测水中的邻苯二甲酸酯

Determination of Phthalic Acid Ester in Water by Solid Phase Extraction-Gas Chromatography

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【作者】 廖艳余煜棉赖子尼齐素芳冯本秀

【Author】 Liao Yan~1,Yu Yumian~2,Lai Zini~3,Qi Sufang~2,Feng Benxiu~2 (1.School of Chemical and Environmental Engineering,Maoming College,Maoming Guangdong 525000,China;2.Test Center,Guangdong University of Technology,Guangzhou Guangdong 510090,China;3.Pearl River Fishery Research Institute,Pearl River Valley Fishery Ecological and Environmental Test Center under Agriculture Ministry,Guangzhou Guangdong 510380,China)

【机构】 茂名学院化工与环境工程分院广东工业大学测试中心农业部珠江流域渔业生态环境检测中心珠江水产研究所广东工业大学测试中心 广东茂名525000广东广州510090广东广州510380

【摘要】 利用固相萃取技术富集了水中4种邻苯二甲酸酯类(PAEs)化合物:邻苯二甲酸二甲酯(DM P)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)。借助均匀设计法及计算机回归建模优化技术对4种PAEs的固相萃取条件进行了设计与优化,得到的最佳固相萃取条件:洗脱剂配比(正己烷与丙酮的体积比)30∶1,洗脱体积2mL,洗脱速率4mL/m in,上样速率8mL/m in。富集后的试样用带电子捕获器的毛细管气相色谱仪检测,方法的线性范围为1~1 000μg/L(DMP,DEP),0.2~100μg/L(DBP,DEHP),线性回归方程的相关系数为0.997 0~1.000 0,检出限为0.02~0.4μg/L,4种PAEs的回收率为69%~117%,相对标准偏差为2.5%~9.5%。

【Abstract】 4 kinds of phthalic acid esters(PAEs)in water were enriched by solid phase extraction(SPE)technology,namely dimethyl phthalate(DMP),diethyl phthalate(DEP),dibutyl phthalate(DBP),di-2-ethylhexyl phthalate(DEHP).The optimum SPE conditions of the 4 PAEs were obtained by homogeneous design and computer regression modeling method,which are:the volume ratio of hexane to acetone 30 ∶1,eluent volume 2mL,eluent rate 4mL/min and sample rate 8mL/min.The enriched samples were determined using a capillary gas chromatograph with electron capture detector.The linear response of the proposed method are in the range of(1-1 000)μg/L(DMP、DEP)and 0.2-100μg/L(DBP、DEHP).The correlation coefficients of the linear regression equations are 0.997 0-1.000 0.The detection limit is(0.02-0.4)μg/L.The recoveries of the 4 PAEs are(69%-117%) and the relative standard deviations are(2.5%-9.5%).

  • 【文献出处】 化工环保 ,Environmental Protection of Chemical Industry , 编辑部邮箱 ,2006年03期
  • 【分类号】X832
  • 【被引频次】30
  • 【下载频次】527
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