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小铅试金富集-ICP-MS法测定地球化学样品中的铂和钯

         

摘要

为了对地球化学样品中铂族元素快速、准确地进行分析测试,在实验的基础上,建立了小铅试金富集-电感耦合等离子体质谱(ICP-MS)法测定地球化学样品中铂和钯的方法.以碱式碳酸铅代替氧化铅,以硝酸银为铂钯捕集剂,取样量为10 g时,试金配方具有较宽的使用范围;灰吹后的银合粒经硝酸溶解后以盐酸沉淀分离银,可有效去除测定干扰元素;采用ICP-MS可准确测定试液中的铂钯含量.方法加标回收率符合要求,对标准样品的测定结果与推荐值相符,适用于批量化探样品中痕量(0.1 ng/g)的铂和钯的分析.%A combined technique of the fire assay and inductively coupled plasma mass spectrometry (ICP-MS) was established to analysize the platinum group elements in geochemical samples. The application range of the technique would be extended by using basic lead carbonate to replace lead oxide and silver nitrate as collector of platinum and palladium, when the sampling amount was 10 g. Silver alloy produced after ash blowing was dissolved in nitric acid, and then silver was separated as AgCl precipitate by adding HCl to the solution with an intention to eliminate the interference of silver in the following ICP-MS measurements for platinum and palladium. The recovery rate of the labeled elements met the relevant requirements. The result of the standard sample was consistent with the recommended value. This analysis technique can be used for the analysis of trace (0.1 ng/g) platinum and palladium in batch geochemical samples.

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