高效液相色谱法测定间苯二甲酸中微量3-CBA的研究
Determination of trace 3-CBA in phthalic acid by high-performance liquid chromatography
王敏1
作者信息
- 1. 中石化北京燕山分公司 北京 102500
- 折叠
摘要
间苯二甲酸(PIA)中间羧基苯甲醛(3-CBA)的含量,是直接判断产品品质等级的重要指标之一.主要探索了选用合适的色谱柱、检测器波长、流动相配比,确定了典型色谱操作条件,建立了高效液相色谱法测定PIA中3-CBA的方法.结果表明,3-CBA含量在0～100mg/kg时,外标法测定3-CBA含量的线性相关系数大于0.999,线性良好,标准溶液的重复性测定结果小于5%,加标回收率在96.0%～103.8%之间.分别采用液相色谱法和极谱法对标准样品进行测定,检测结果相似,没有明显差异,表明该方法的准确度和精密度良好.
Abstract
The content of m-carboxybenzaldehyde(3-CBA)in isophthalic acid(PIA)is one of the important indicators for directly judging the quality level of products.Exploring the selection of appropriate chromatographic columns,detector wavelengths,and mobile phase ratios,typical chromatographic operating conditions were determined and a high-performance liquid chromatography method was established to determine 3-CBA in PIA.The results showed that when the content of 3-CBA was between 0 and 100mg/kg,the linear correlation coefficient of the external standard measured 3-CBA content was greater than 0.999,indicating good linearity.The repeatability of the standard solution was less than 5%,and the recovery rate of the added standard was between 96.0%and 103.8%.The standard samples were measured using liquid chromatography and polarography respectively,and the detection results were similar without significant differences,indicating that the accuracy and precision of the method were good.
关键词
PIA/3-CBA/液相色谱/极谱法/外标Key words
PIA/3-CBA/Liquid chromatography method/Polarographic method/External standard method引用本文复制引用
出版年
2024
NETL
NSTL
万方数据