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本文采用电感耦合等离子体质谱法(ICP-MS)测定高纯铼酸铵中19种痕量杂质元素,应用屏蔽炬技术消除了56ArO+等多原子离子对Fe、Ca、K等元素的干扰,讨论了质谱干扰和锥的接口效应,优化采样时间,研究了铼酸铵的基体效应,采用在线样品标准加入法消除基体效应。各元素的方法定量下限(15σ)为0.014~0.63μg/g,对样品加标0.4μg/g的回收率在85%~112%之间。方法适用于纯度为99.999%的高纯铼酸铵中痕量杂质元素的测定。
In this paper, inductively coupled plasma mass spectrometry (ICP-MS) was used to determine 19 kinds of trace impurities in high purity ammonium rhenium formate. Shielding torch technology was used to eliminate the interference of 56ArO + and other polyatomic ions on Fe, Ca, K and other elements. The mass spectrometry interference and cone interface effect were optimized, and the sampling time was optimized. The matrix effect of ammonium rhenium was studied. The matrix effect was eliminated by the online sample standard addition method. The lower limit of quantification (15σ) of each element was 0.014 ~ 0.63μg / g, and the recoveries of spiked samples 0.4μg / g ranged from 85% to 112%. The method is suitable for the determination of trace impurity elements in high purity ammonium rhenate with a purity of 99.999%.