一种测定3,3′,4,4′-联苯四甲酸二酐纯度的新方法
A New Method for Determination of Purity of 3,3′,4,4′-Biphenyl-tetracarboxylic Dianhydride
摘 要
试验结果表明在HPLC分析中,3,3′,4,4′-联苯四甲酸二酐(简写作BPDA)难以与其合成中的副产品联苯四甲酸(简写作BPTA)相互分离,而且在流动相通过色谱柱的过程中,由于BPDA与流动相之间产生水解反应又增加了一些BPTA.因此HPLC法测定BPDA纯度误差较大.为此,提出用碱滴定法分析滴定BPDA的醇解及水解产物,根据两者所耗氢氧化钠标准溶液体积之差按文中所给出的公式算得样品中BPDA的含量(即其纯度),与BPDA共存的杂质BPTA对滴定无干扰.在分析纯度为99.58%的BPDA样品时,算得测定值的相对偏差为0.29%.
纯度
3,3′,4,4′-联苯四甲酸二酐
醇解反应
水解反应
Alkalimetry
Purity
3,3′,4,4′-Biphenyltetracarboxylic dianhydride
Alcoholysis
Hydrolysis以3,3′,4,4′-
Abstract
It was shown that in HPLC analysis,3,3′,4,4′-biphenyltetracarboxylic dianhydride (BPDA in short) was hardly to be separated from the by-product 3,3′,4,4′-biphenyltetracarboxylic acid (BPTA in short),and in addition,some more BPTA was produced by hydrolysis of BPDA with the mobile phase when passing through the chromatographic column.Hence,results with significant errors were obtained by determination of purity of BPDA by HPLC.It was proposed that the purity of BPDA can be determined by alkalimetric titration of products of alcoholysis and hydrolysis of BPDA with NaOH standard solution separately,and the content of BPDA (i.e.,its purity) calculated from the difference of volume of the titrant used as shown by the given formula.The presence of the impurity,BPTA,did not interfere with the determination.In the analysis of a sample of BPDA having its purity of 99.58%,the value of relative deviation found was 0.29%.
中图分类号 O657
所属栏目 工作简报
基金项目
收稿日期 2008/4/28
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备注张金芳(1972-),女,安徽全椒人,讲师,硕士,从事分析化学教学与研究.
引用该论文: ZHANG Jin-fang,LI Shan-mao,LIU Guo-hong,CHEN Chuan-zhi. A New Method for Determination of Purity of 3,3′,4,4′-Biphenyl-tetracarboxylic Dianhydride[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(5): 524～525
张金芳,李善茂,刘国宏,陈传治. 一种测定3,3′,4,4′-联苯四甲酸二酐纯度的新方法[J]. 理化检验－化学分册, 2009, 45(5): 524～525
被引情况:
【1】虞锐鹏,陈尚卫,朱松,王明堂,王红春, "反相高效液相色谱法测定抗氧化剂硫代二丙酸双十二醇酯",理化检验－化学分册 47, 572-573(2011)
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参考文献
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【3】穆瑞才,邓国才,刘歆颖,等.均苯四甲酸二酐产品的反相高校液相色谱分析[J].分析化学,1996,24(9):1114-1114．
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【5】KITAI M,KATSURO Y,KAWAMURA S.Method for dimerization of aromatic halide compounds: US,4900843[P].1990-02-12．
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