王水水浴消解-电感耦合等离子体质谱法测定土壤中的硒  

Determination of Selenium in Soil by Inductively Coupled Plasma-Mass Spectrometry with Aqua Regia Digestion in Water Bath

作　　者：薛静 安帅 汪寅夫[1] 高慧莉 史佳铭 XUE Jing;AN Shuai;WANG Yin-fu;GAO Hui-li;SHI Jia-ming(Shenyang Centre of Geological Survey,China Geological Survey,Shenyang 110032,China;Liaoning Nonferrous Geological Exploration Institute Co.LTD,Shenyang 110121,China)

机构地区：[1]中国地质调查局沈阳地质调查中心,辽宁沈阳110032 [2]辽宁省有色地质勘查总院有限责任公司,辽宁沈阳110121

出　　处：《岩矿测试》2020年第5期720-725,共6页Rock and Mineral Analysis

摘　　要：随着富硒产品关注度越来越高,对土壤中硒含量测定的研究也越来越受到人们的重视。应用传统电感耦合等离子体质谱法(ICP-MS)测定土壤样品中的硒时,受到的基体效应和多原子离子干扰比较显著,准确测定硒含量的难度较大。本文建立了采用50%王水-沸水浴消解体系,ICP-MS测定土壤样品中硒含量的方法,实验中采用动能歧视模式(KED)消除质谱干扰,选用103 Rh元素作为在线加入内标以消除仪器信号漂移。用该方法对有证土壤标准物质进行分析,其结果均在不确定度范围内,测定值与认定值的相对误差介于-2.01%~2.99%之间,相对标准偏差(RSD)小于6.60%,检出限为0.012μg/g,测定下限为0.048μg/g。应用该方法与国家环境保护标准方法(HJ680—2013)对20个土壤实际样品进行比对分析,其结果基本一致。该方法适合于分析测定地质等行业大批量土壤样品中的硒。BACKGROUND:With more and more attention being paid to selenium-rich products,the study on the determination of selenium content in soil has become more significant.The accurate determination is difficult due to the serious interference of the matrix effect and polyatomic ion when determining selenium in soil samples by inductively coupled plasma-mass spectrometry(ICP-MS).OBJECTIVES:To establish a method for accurate determination of Se in soil.METHODS:The content of selenium in soil samples was determined by ICP-MS with 50%aqua regia-boiling water digestion.Kinetic energy discrimination mode(KED)was adopted to eliminate mass spectrum interference,and the 103Rh element was selected as the internal standard for on-line addition to eliminate instrument signal drift.RESULTS:The results of the analysis of certified soil standard materials were consistent with those of certified standard materials within the uncertainty.The results showed that the relative errors(REs)of this method were between-2.01%and 2.99%,the relative standard deviation(RSD)was less than 6.60%,the detection limit was 0.012μg/g,and the minimum quantitative detection limit was 0.048μg/g.The method was applied to analyze 20 soil samples,and the results were consistent with those obtained by national environmental protection standard HJ680—2013.CONCLUSIONS:The study results are suitable for the determination of selenium in large numbers of soil samples from the geological industry.

关 键 词：水浴消解 土壤 硒 电感耦合等离子体质谱法 动能歧视模式 

分 类 号：O657.63[理学—分析化学] S151.93[理学—化学]