王水水浴消解-电感耦合等离子体质谱(ICP-MS)法测定地质样品中镉、硒和银  

Determination of Cadmium,Selenium and Silver in Geological Samples by Inductively Coupled Plasma Mass Spectrometry(ICP-MS)with Aqua Regia Bath Digestion

作　　者：何袖辉 段文 王银剑 高鑫磊 黎宏新 王志凯 冯俊 HE Xiuhui;DUAN Wen;WANG Yinjian;GAO Xinlei;LI Hongxin;WANG Zhikai;FENG Jun(Kunming Natural Resources Comprehensive Survey Center of China Geological Survey,Kunming,Yunnan 650100,China;Technology Innovation Center for Analysis and Detection of the Element Speciation and Emerging Contaminants,China Geological Survey,Kunming,Yunnan 650100,China)

机构地区：[1]中国地质调查局昆明自然资源综合调查中心,昆明650100 [2]中国地质调查局元素形态与新污染物检验检测技术创新中心,昆明650100

出　　处：《中国无机分析化学》2025年第5期683-689,共7页Chinese Journal of Inorganic Analytical Chemistry

基　　金：中国地质调查局地质调查项目(DD20243335);云南省农业联合专项面上项目(202101BD070001-107)。

摘　　要：地质样品中镉、硒和银的测定对于了解地质体系的成因和演化具有重要意义,采用王水溶样(1+1)-电感耦合等离子体质谱(ICP-MS)法测定地质样品中Cd、Se和Ag,考察了干扰元素Zr、Nb、Mo和Sn对Ag、Cd、Se的干扰消除问题。在样品消解阶段最主要难溶干扰元素Zr、Sn和Nb等的提取率可以有效控制在较低水平,而Ag、Cd、Se的提取趋于完全,在样品预处理阶段实现了待测元素和干扰元素的有效分离,减少了多原子离子和同量异位数的干扰。在测试中使用内标元素Rh校正基体效应和信号漂移,用KED模式消除质谱干扰。Cd、Se和Ag的方法检出限分别为0.008、0.012和0.014μg/g,对不同含量样品12次测定的相对标准偏差RSD为4.3%~7.6%,Δlg C小于0.1。测定国家一级标准物质,准确度和精密度都能优于规范要求,工作效率得到较大的提高,实现了绿色环保的高效分析。The determination of cadmium(Cd),selenium(Se),and silver(Ag) in geological samples is crucial for understanding the genesis and evolution of geological systems.In this study,aqua-regia-soluble sample(1+1)-inductively coupled plasma mass spectrometry(ICP-MS) was employed to determine Cd,Se,and Ag,aiming to explore the elimination of interference from elements such as zirconium(Zr),niobium(Nb),molybdenum(Mo),and tin(Sn) on Ag,Cd and Se.During the sample digestion stage,the extraction rates of key interfering elements,such as insoluble Zr,Sn and Nb,were effectively controlled at a low level,while the extraction of Ag,Cd,and Se tended to be complete.In the sample pretreatment stage,the effective separation of the target elements from the interfering elements was achieved,reducing the interference.In the testing process,the internal standard element rhodium(Rh) was used to correct the matrix effect and signal drift,and the kinetic energy discrimination(KED) mode was adopted to eliminate spectral interference.The detection limits of Cd,Se,and Ag were determined to be 0.008,0.012,and 0.014 μg/g,respectively.The relative standard deviation(RSD) for 12 measurements of samples with different contents ranged from 4.3% to 7.6%,and the ΔlgC value was less than 0.1.When this method was applied to the determination of national first-class certified reference materials,it demonstrated better accuracy and precision than the standard requirements,significantly improving work efficiency and achieving efficient and environmentally-friendly analysis.

关 键 词：ICP-MS 王水水浴消解 AG CD SE 

分 类 号：O657.63[理学—分析化学]