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建立了用电感耦合等离子体-质谱法(ICP-MS)测定纯铪或氧化铪中的Mg、Al、Si、P、Ca、Ti、V、Cr、Mn、Fe、Ni、Co、Cu、Zn、As、Zr、Nb、Mo、Cd、Sn、Sb、Ta、W、Pb和Bi等25种杂质元素含量的方法。铪金属室温条件下混酸溶解后可直接进样分析,氧化铪采用微波消解,辅助溶解后用ICP-MS测定。利用建立的方法,对铪及氧化铪中的杂质元素进行测定,加标回收率为86%—120%。各金属杂质含量均为10ng/mL的混合标准溶液平行7次进样的相对标准偏差均小于5%。方法操作简便、快速,检出限低,能够满足纯度为99.99%的铪金属或氧化铪中杂质分析的需要。
The determination of Mg, Al, Si, P, Ca, Ti, V, Cr, Mn, Fe, Ni, Co and Cu in pure hafnium or hafnium oxide by inductively coupled plasma mass spectrometry (ICP- Zn, As, Zr, Nb, Mo, Cd, Sn, Sb, Ta, W, Pb and Bi. Hafnium metal mixed solution at room temperature can be dissolved directly into the sample analysis, hafnium oxide by microwave digestion, assisted dissolution after determination by ICP-MS. Using the established method, the impurity elements in hafnium and hafnium oxide were determined, and the recoveries were in the range of 86% -120%. The relative standard deviations (RSDs) of seven parallel injections of mixed standard solutions with 10 ng / mL of each metal impurity were all less than 5%. The method is simple, rapid, and low in detection limit. It can meet the need of impurity analysis in hafnium metal or hafnium oxide with the purity of 99.99%.