氟化络合-ICP-MS法测定稀土金属中的难熔金属杂质元素Ta、Mo、W、Ti、Nb

Determination of Ta,Mo,W,Ti,Nb in rare earth metals by ICP-MS with the complexion of fluoricion

针对稀土金属中难熔金属杂质元素Ta、Mo、W、Ti、Nb在HCl或HNO3中不易溶解的性质,本文在前人工作基础上,采用HF络合-ICP-MS结合的方法,有效地将上述元素溶解在溶液中,并利用ICP-MS高灵敏度和多元素同时测定的优势,成功建立了稀土金属中难熔金属杂质元素Ta、Mo、W、Ti、Nb的测定方法.其操作过程较传统化学方法简便,灵敏度也更高.本文分析了氢氟酸的络合过程,试验了稀土氟化物沉淀对被测元素的吸附作用和内标法的校正作用.方法检出限在0.3～1.5 ng/mL,测定下限0.0005%～0.0010%,回收率在89.2%～118.9%,相对标准偏差为4.6%～9.7%.

Ta, Mo, W, Ti, Nb, the refractory impurity elements, in RE metals are dissolved thoroughly with the addition of fluoric acid, and then determined by ICP-MS. The operation process is simpler and more timesaved than that of respective traditional chemical methods. This method is highly sensitive with detection limits of 0.3 - 1.5 ng/mL. The recoveries and precisions are between 89.2% - 118.9% and 4.6% -9.7%, respectively.