高纯五氧化二钒样品在硝酸氢氟酸(4+1)混合液中经微波消解处理,采用电感耦合等离子体质谱法测定样品溶液中15种杂质元素(钛、硅、铝、铬、镍、铜、铅、砷、磷、铁、锰、钙、镁、钾、钠)的含量。采用内标法消除基体的影响。方法的检出限(3s/k)在0.03~0.89 μg·L-1之间。方法的加标回收率在90.0%~113%之间,相对标准偏差(n=8)小于5.0%。五氧化二钒5号样品中8种杂质元素的测定值与石墨炉原子吸收光谱法进行核对,测得结果互相符合。

The sample of vanadium pentoxide was treated with a mixture of HNO3 and HF (4+1) by microwave assisted digestion, and contents of 15 impurity elements ( i.e. Ti, Si, Al, Cr, Ni, Cu, Pb, As, P, Fe, Mn, Ca, Mg, K and Na ) in the sample solution were determined by ICPMS. The matrix interference was eliminated by internal standard method. Detection limits (3s/k) of the method found were in the range of 0.03-0.89 μg·L-1. Tests for recovery were made by standard addition method, giving values of recovery in the range of 90.0%-113% and RSD′s (n=8) found were less than 5.0%. Contents of 8 impurity elements in sample 5# were checked by GFAAS method, consistent values were obtained.