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出 处:《分析试验室》2011年第7期18-21,共4页Chinese Journal of Analysis Laboratory
基 金:国家科技支撑计划;科研用高纯无机试剂核心单元物质及共性关键技术的研究与开发项目(2006BAF07B02)资助
摘 要:采用反应池技术消除了复合离子对Ca、Fe和Si等元素的干扰,以内标校正法直接测定了其它9种元素。优化选择了测定同位素和内标元素,考察了基体效应对测定结果的影响,建立了电感耦合等离子体质谱测定了高纯钼中12种杂质元素含量的方法。方法测定下限介于0.10~0.37μg/g之间,加标回收率为93%~105%,RSD<10%。对钼粉和钼条两个实际样品进行了分析,测定结果表明,方法可满足4N~5N高纯钼产品的测定要求。The interferences for Ca,Fe and Si produced by polyatomic ions were eliminated by H2 reaction technology and the other 9 impurities were determined directly by internal standard correction method.Under the optimized conditions of measured isotopes and internal standard elements,the matrix effects were investigated and the method for the analysis of 12 trace-impurities in high purity molybdenum was established.Determination limits obtained ranged between 0.10 and 0.37 μg/g for this 12 impurities.The accuracy of the method was evaluated by recovery measurements on spiked samples,and good recovery results(93-105%) with precision of less than 10% were achieved.The method was used for the analysis of high purity molybdenum bar and power,which proved that this method was suitable for the analysis of 4N^5N high purity molybdenum products.
关 键 词:电感耦合等离子体质谱法 反应池技术 高纯钼 杂质元素
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