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液相色谱法测定环氧氯丙烷工业中间体中的己二酸
引用本文:谯应召,华威,张思宝,李洪宽,马金凤.液相色谱法测定环氧氯丙烷工业中间体中的己二酸[J].化学分析计量,2013(6):53-55.
作者姓名:谯应召  华威  张思宝  李洪宽  马金凤
作者单位:[1]山东省化工研究院,济南250014 [2]山东爱纳分析仪器技术服务中心,济南250014
摘    要:建立了液相色谱仪测定环氧氯丙烷工业中间体中己二酸含量的方法。样品采用甲醇-10mm01/L磷酸缓冲液(体积比5:95)溶液提取,C18固相萃取柱净化,紫外检测器检测,外标法定量。己二酸在100~2000mg/L范围内线性良好,相关系数大于0.9999,按10s/Ⅳ计算,己二酸定量限为25.0mg/kg。添加回收率为91.1%~112.2%.测定结果的相对标准偏差为4.7%~7.9%(n=5)。该方法简单快速,回收率高,重现性好,满足工业分析要求。

关 键 词:己二酸  环氧氯丙烷工业中间体  液相色谱法

Determination of Adipic Acid in Epoxy Chloropropane Industrial Intermediates by Liquid Chromatography
Qiao Yingzhao,Hua Wei,Zhang Sibao,Li Hongkuan Shandong Chemical Industry Research Institute,Jinan,China Ma Jinfeng.Determination of Adipic Acid in Epoxy Chloropropane Industrial Intermediates by Liquid Chromatography[J].Chemical Analysis And Meterage,2013(6):53-55.
Authors:Qiao Yingzhao  Hua Wei  Zhang Sibao  Li Hongkuan Shandong Chemical Industry Research Institute  Jinan  China Ma Jinfeng
Institution:Qiao Yingzhao, Hua Wei, Zhang Sibao, Li Hongkuan ( Shandong Chemical Industry Research Institute, Jinan 250014, China ) Ma Jinfeng ( Shandong Ai' na Analysis Instrument Technology Service Center, jinan 250014, China )
Abstract:A method for determination of adipic acid in epoxy chloropropane industrial intermediates by liquid chromatography was established. The sample was extracted by methanol-10 mmol/L phosphate buffer and cleaned up with C18 solid-phase, then analyzed by UV detector and quantified by the external standard method. Good linear relation was obtained in the range of 100-2 000 mg/L with the correlation coefficient more than 0.999 9, the limit of quantitation was 25.0 mg/kg(10S/N). The recoveries was 91.1%-112.2% with RSD of 4.7%-7.9%(n=5). The method is simple and fast with high recovery rate, good reproducibility, and meets the demand of industrial analysis.
Keywords:adipic acid  epoxy chloropropane industrial intermediates  liquid chromatography
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