电感耦合等离子体质谱法测定高纯钨中15种痕量杂质元素

摘要

The trace-impurities in high purity tungsten were determined by inductively coupled plasma mass spectrometry (ICP-MS). The interferences for K, Ca, Fe and Si produced by polyatomic ions were eliminated by H2 reaction technology. Under the optimized conditions of measured isotopes and internal standard elements, the acid and matrix effects were investigated, and the method for the analysis of 15 trace-impurities in high purity tungsten was established. Determination limits obtained ranged between 0. 12 and 0. 50 μg/g for this fifteen impurities. The accuracy of the method was evaluated by recovery measurements on spiked samples, and good recovery results (96. 1%-110. 6%) with precision(RSD) of less than 8% were achieved. The method was used for the analysis of high purity tungsten bar and power. The result showed that the method was suitable for the analysis of 4N-5N high purity tungsten products.%采用电感耦合等离子体质谱(ICP-MS)法测定高纯钨中杂质元素含量；应用H2反应池技术消除复合离子对K、Ca、Fe和Si等元素的干扰；考察了溶液酸度、基体效应等条件对测定结果的影响；以内标校正法补偿基体效应,优化选择了测定同位素和内标元素,最终建立高纯钨中15种杂质元素含量的测定方法.方法测定下限介于0.12～0.50 μg/g,加标回收率在96.1％～110.6％之间,相对标准偏差小于8％.采用该方法测定高纯钨条和钨粉两种实际样品,可以满足4N～5N高纯钨的测定.