电感耦合等离子体-质谱法测定纯铪或氧化铪中的25种杂质元素

Determination of 25 Impurities Elements in Pure Hafnium or Hafnium Dioxide by ICP-MS

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 method for the determination of the contents of 25 kinds trace impurities elements in pure hafnium or hafnium dioxide,such as Mg,Al,Si,P,Ca,Ti,V,Cr,Mn,Fe,Ni,Co,Cu,Zn,As,Zr,Nb,Mo,Cd,Sn,Sb,Ta,W,Pb and Bi,by inductively coupled plasma mass spectrometry（ICP-MS） was established.Hafnium metal can be directly analyzed after the dissolved by mixed acid in room temperature,while hafnium dioxide should be assisted by microwave digestion before the determination by ICP-MS.The spiked recoveries in the range of 86%—120% was obtained to determine the impurities elements in hafnium or hafnium dioxide according to the established method.The relative standard deviations（RSDs） were less than 5% for calculation of the seven consecutive injections of 10ng/mL standard mixtures.The method is simple and fast with low detection limit,that can meet the need for impurity analysis of 99.99% hafnium or hafnium dioxide.