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以电感耦合等离子体质谱法(ICP-MS)测定了高纯铼中26种杂质元素含量。应用反应池技术消除了复合离子对K、Ca、Fe等元素的干扰,采用干扰方程校正技术消除了Re氧化物对Tl的质谱重叠干扰,未受干扰的其它杂质元素采用内标校正法直接测定。考察了溶液酸度、基体效应等条件对测定的影响,优化选择了测定同位素和内标元素。方法测定下限介于0.12～5.0μg/g,加标回收率在90%～110%之间,相对标准偏差小于10%。方法可以满足4N5高纯铼的测定。
The content of 26 kinds of impurity elements in high purity rhenium was determined by inductively coupled plasma mass spectrometry (ICP-MS). The use of reaction cell technology to eliminate the interference of complex ions on K, Ca, Fe and other elements, the use of interference equation correction technology to eliminate Re oxide Tl overlap of mass spectrometry interference, other undisturbed impurities directly measured by internal standard method . The effects of solution acidity, matrix effect and other conditions on the determination were investigated, and the determination of isotope and internal standard elements was optimized. The lower limit of determination was between 0.12 and 5.0 μg / g, the spiked recoveries were between 90% and 110%, and the relative standard deviations were less than 10%. The method can meet the determination of 4N5 high purity rhenium.