酸消解-能量色散X射线荧光光谱法测定铜及铜合金中铜  

Determination of copper in copper and copper alloy by acid digestion and energy dispersive X-ray fluorescence spectrometry

作　　者：刘志英 李明茂[2] 刘奇 王丽丽 章新亮 袁江山 LIU Zhiying;LI Mingmao;LIU Qi;WANG Lili;ZHANG Xinliang;YUAN Jiangshan(Yingtan Institute of Inspection,Testing and Certification,Yingtan 335000,China;Jiangxi University of Science and Technology,Ganzhou 341000,China)

机构地区：[1]鹰潭市检验检测认证院,江西鹰潭335000 [2]江西理工大学,江西赣州341000

出　　处：《冶金分析》2023年第11期39-44,共6页Metallurgical Analysis

基　　金：江西省市场监督管理局科技项目(GSJK202124);江西省科技厅重大科技研发专项(20213AAE01007)。

摘　　要：为了解决能量色散X射线荧光光谱法(EDXRF)测定铜及铜合金中铜含量误差大的问题,试验采用酸分解的方法前处理样品,用标准溶液配制铜标准溶液系列,以铜的质量浓度为横坐标、荧光强度为纵坐标绘制校准曲线,建立了酸消解-能量色散X射线荧光光谱法测定铜及铜合金中铜含量的方法。采用正交试验考察了酸分解中的润湿用水量、盐酸用量、硝酸用量、反应后处理几个重要因素,确定了最优酸消解条件。按照实验方法测定4个铜及铜合金标准物质中铜,结果的相对标准偏差(RSD,n=13)为0.32%~0.68%,测定值和认定值一致性良好。分别采用实验方法与标准方法GB/T 5121.1—2008对4类铜产品中铜进行测定,结果表明测试结果一致性良好。方法能较好克服基体效应,解决了相匹配的固体标样难配齐的问题,能满足日常检验要求。In order to solve the problem of large error during the determination of copper content in copper and copper alloys by energy dispersive X-ray fluorescence spectroscopy(EDXRF),the sample was pretreated by acid decomposition in experiments.The copper standard solution series were prepared with standard solution.The calibration curve was drawn with the mass concentration of copper as the abscissa and the fluorescence intensity as the ordinate.A method for the determination of copper in copper and copper alloys by EDXRF after acid digestion was established.The effects of wetting water consumption,hydrochloric acid dosage,nitric acid dosage and post-reaction treatment on the determination were investigated by orthogonal tests,and the optimal acid digestion conditions were obtained.The contents of copper in four copper and copper alloy CRMs were determined according to the experimental method.The relative standard deviations(RSD,n=13)of determination results were between 0.32%and 0.68%.The measured values were weill consistent with the certified values.The contents of copper in four copper products were determined according to the experimental method and GB/T 5121.1-2008,and it was found that the test results were consistent.The proposed method could well overcome the matrix effect and solve the matching problem of solid standard sample.This method could meet the requirements of daily inspection.

关 键 词：酸消解 能量色散X射线荧光光谱法(EDXRF) 铜及铜合金 铜 正交试验 

分 类 号：O657.34[理学—分析化学] TF03[理学—化学] TF811[冶金工程—冶金物理化学]