Abstract：During the determination of trace Mg, K, Ca, Cr and Fe in high purity niobium pentoxide by inductively coupled plasma mass spectrometry (ICP-MS), these impurity elements could not be accurately determined due to the high background equivalent concentrations (BECs) which were caused by the serious mass spectral interferences. After the sample was treated by microwave digestion with HF-HNO3 system and the matrix effect was corrected by the standard addition method, an analysis method of 25 trace impurity elements (including Mg, K, Ca, Cr, Fe, etc) in high-purity niobium pentoxide by ICP-MS was established with matrix mass concentration at 500μg/mL. The results indicated that BECs of Na, Mg, Al, K, Ca, Cr, Fe, Cu, Co, Ni and Mn were obviously improved in 500μg/mL niobium pentoxide matrix solution by the shield torch cool plasma technology. Particularly, the improvement effect of BECs of Mg, K, Ca, Cr and Fe were the most significant, which were reduced from 56.5-194ng/mL at normal mode to 0.012-0.203ng/mL at cool plasma mode. The reagent blank could be effectively reduced by the electronic-grade HF and HNO3 purified in laboratory by sub boiling distillation. The linear correlation coefficients of calibration curves of elements were all higher than 0.9990. The detection limits of elements in this method were in the range of 0.001-0.010μg/g, and the low limits of determination were between 0.003μg/g and 0.033μg/g. The contents of 25 impurity elements in high purity niobium pentoxide sample were determined according to the experimental method. The results showed that the relative standard deviations of determination results (RSD, n=11) were between 0.9% and 12.7%, and the spiked recoveries were between 91% and 111%. The proposed method was applied for the analysis of two batches of actual ultra-pure niobium pentoxide samples (the purity was 99.999%). The results were basically consistent with those obtained by GD-MS.
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