微波消解—电感耦合等离子体原子发射光谱法测定铂金首饰中的汞、铅、镉、铬、砷  

Determination of Hg,Pb,Cd,Cr,As in platinum jewelry by microwave digestion- inductively coupled plasma atomic emission spectrometry

作　　者：张凤霞[1,2,3] 刘海彬[1,2] 王萍[1,2,3] 黄准[1,2] 

机构地区：[1]国家黄金钻石制品质量监督检验中心 [2]山东省计量检测重点实验室 [3]山东省社会公正计量行

出　　处：《黄金》2014年第12期70-73,共4页Gold

基　　金：山东省质量技术监督局科研项目资助(2011KY02)

摘　　要：建立了试样经微波消解后采用电感耦合等离子体原子发射光谱法（ ICP－AES）测定铂金首饰中汞、铅、镉、铬、砷的分析方法。对试样的微波消解条件、基体和谱线干扰等进行了研究，对比了微波密闭消解法与传统分（消）解法的条件。其结果表明：在150℃温度下，以王水为消解试剂，试样在密闭容器中消解25 min可以完全溶解；消解液用ICP－AES测定时，通过选择合适的分析谱线可避免基体和光谱干扰；不同元素的检出限为0．006～0．15 mg／kg，回收率为98％～117％，RSD为0．04％～1．17％；Pt 900和Pt 950首饰对应消解时间分别为传统法的1／6～1／8，总分析流程均大大缩短，微波消解前处理方法具有简便、快捷、回收率高、精密度高的优点。该方法适用于铂金首饰中汞、铅、镉、铬、砷元素的测定。An analysis method for determination of Hg ,Pb,Cd,Cr,As in platinum jewelry by inductively coupled plasma atomic emission spectrometry （ ICP-AES） after microwave digestion was proposed .The conditions of sample microwave digestion ,interference of matrix and spectral line were investigated .The dissolved conditions of the proposed method were compared with the traditional method .The results showed that the sample could be fully dissolved in aqua regia by microwave digestion for 25 min in closed container at 150 ℃.During determination of the digestion solution by ICP-AES,the interference of matrix and spectrum could be avoided by selecting proper analytical lines .The de-tection limit was 0.006 -0.15 mg/kg.The recovery rate was 98 %-117 % and relative standard deviation was 0 .04 %-1 .17 %.Results showed that digestion time of the Pt 900 and Pt 950 jewelry was 1/6 and 1/8 times of the traditional method respectively .The microwave digestion method is simple ,rapid with high recovery rate and accuracy and is applicable for the determination of Hg ,Pb,Cd,Cr,As in platinum jewelry .

关 键 词：微波消解 电感耦合等离子体原子发射光谱法 铂金首饰 汞 铅 镉 铬 砷 

分 类 号：O657.31[理学—分析化学]