高分辨电感耦合等离子体质谱仪测定电子级没食子酸中的金属杂质含量  

Determination of metal impurity content in electronic grade gallic acid by High-Resolution inductively coupled plasma mass spectrometry

作　　者：常燕 高一鸣 魏王慧 王勇 曹建雄 李春华[1] ChangYan;Gao Yiming;WeiWanghui;Wang Yong;Cao Jianxiong;Li Chunhua(Shanghai Institute of Measurement and Testing Technology)

机构地区：[1]上海市计量测试技术研究院

出　　处：《上海计量测试》2024年第6期8-11,共4页Shanghai Measurement and Testing

基　　金：国家市场监督管理总局科技计划(2022MK027、2023MK029)。

摘　　要：通过研究前处理方法和质谱干扰消除方案,建立了基于硝酸氧化消解—高分辨电感耦合等离子体质谱法(HR-ICP-MS)测定电子级没食子酸中多种痕量金属杂质(Na、Pb、Mg、Al、Ca、Cr、Mn、Fe、Ni、Cu、Zn和K)的分析方法。利用标准加入法校正基体效应,12种元素的校正曲线的相关系数均大于0.999,方法检出限为0.041~0.76μg/kg,测试精密度优于5%,加标回收率在92.2%~109.3%之间,满足集成电路用没食子酸的质量要求。By studying the pre-treatment methods and mass spectrometry interference elimination schemes,an analytical method based on nitric acid oxidation and high-resolution inductively coupled plasma mass spectrometry(HR-ICP-MS)was established to determine multiple trace metal impurities(Na,Pb,Mg,Al,Ca,Cr,Mn,Fe,Ni,Cu,Zn,and K)in electronic-grade gallic acid.The matrix effect was corrected using the standard addition method,and the correlation coefficients of the calibration curves for the 12 elements were all greater than 0.999.The method detection limits were from 0.041-0.76μg/kg,the test precision was better than 5%,and the recovery rates of spiked samples ranged from 92.2%to 109.3%,meeting the quality requirements for integrated circuit use of gallic acid.

关 键 词：电子级没食子酸 金属杂质 高分辨电感耦合等离子体质谱法 标准加入法 硝酸氧化消解 

分 类 号：O65[理学—分析化学]