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出 处:《质谱学报》2011年第4期216-221,共6页Journal of Chinese Mass Spectrometry Society
基 金:国家科技支撑计划(2006BAF07B02)资助
摘 要: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0.12~0.50μg/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。The trace-impurities in high purity tungsten were determined by inductively cou- pled 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 condi- tions 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 ptg/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.
关 键 词:电感耦合等离子体质谱(ICP-MS) 反应池技术 高纯钨 杂质元素
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