ICP-AES法同时测定高纯铅中八种杂质元素

摘要

分析比较了ICP-AES、吸光光度法和原子吸收法三种方法测定高纯铅中的八种杂质元素.结果表明原子吸收法和吸光光度法分析速度慢,且对个别含量低的元素检测灵敏度也较低.因此选择电感耦合等离子体原子发射光谱法检测高纯铅中的八种杂质元素.样品采用1∶3的HNO3溶解,用1∶1的H2S04沉淀,同时测定As、Sb、Cu、Sn、Bi、Cd、Zn、Fe的含量,并考察了谱线的干扰及背景扣除、酸度效应等因素的影响,优化了实验条件.该方法有较好的检出限,加标回收率为97.62％ ～ 100.42％,相对标准偏差(RSD)(n =11)为0.74％～2.32％,实现了高纯铅中八种杂质元素的快速测定.%In this paper,simultaneous determination of eight kinds of impurity elements in high purity lead by three methods,namely the ICP-AES method,the absorbance spectrophotometry method and the atomic absorption method,is analyzed and compared.The results show that the atomic absorption method and the spectrophotometry analysis are slow,and the sensitivity of lower limit for content of individual elements is low.ICP-AES is chosen to detect eight kinds of impurity elements in high purity lead.The sample is dissolved with 1 ∶ 3 nitric acid and precipitated with 1∶1 sulfuric acid.The contents of As、Sb、Cu、Sn,Bi、Cd,Zn and Fe are determined simultaneously,the spectrum interference and background subtraction,the acidity effect,and the influence factors examined,and the experimental conditions optimized.The method has good detection limit,the standard addition recovery being 97.62％ ～ 100.42％,the relative standard deviation (RSD)(n =11) being 0.74％ ～ 2.32％,thus a rapid determination of eight kinds of impurity elements in high purity lead is realized.