电感耦合等离子体质谱法测定硫酸镍中痕量铊

Determination of trace thallium in nickel sulfate by inductively coupled plasma mass spectrometry

为了进一步提升新能源工业生产领域中痕量铊元素的分析准确性,使用iCAPRQ型电感耦合等离子体质谱(ICP-MS)建立了一种测试硫酸镍中铊含量的方法。对该方法引入的质谱仪干扰进行了分析,提出了采用“干扰离子动能歧视消除模式(KED)”分析模式、控制可溶解固体总量(TDS)和引入铑、铼内标等降低干扰的方法。确定了前处理条件中可溶解固体总量和溶解温度分别为0.2%与210℃。方法验证结果表明:该方法的检出限为0.0036 ng/mL,精密度测试中相对标准偏差(RSD)为1.3%-2.5%,加标回收率为98.4%-100.8%。在实验室间比对中,RSD为0-5.7%,再现性良好。该测试方法简单、快速、准确度高,可广泛适用于硫酸镍产业链的铊含量监控。

In order to further improve the analytical accuracy of trace thallium in the field of new energy industrial produc-tion,this paper established a method to determine the content of thallium in nickel(Ⅱ)sulfate using iCAP RQ type ICP-MS.The interference of mass spectrometer introduced by this method was analyzed,which could be reduced by using inter-ference ion kinetic energy discrimination elimination mode(KED)analysis mode,controlling the total dissolved solids(TDS)and introducing rhodium and rhenium internal standards.The total amount of soluble solids and the dissolution tem-perature in the pretreatment conditions were determined to be 0.2%and 210℃,The method validation results showed that the detection limit of the method was 0.0036 ng/mL,the RSD of the precision test was 1.3%-2.5%,and the recovery rate was 98.4%-100.8%.In the comparison between laboratories,the RSD was 0-5.7%,and the reproducibility was good.The method was simple,rapid,and highly accurate,and could be widely used in the monitoring of thallium content in the nickel sulfate industry chain.