常压混酸溶矿—电感耦合等离子体发射光谱法测定铌钽

Dissolution with mixed acids under normal pressure-determination of niobium and tantalum by inductively coupled plasma atomic emission spectrometric

混酸溶解矿石样品,在酒石酸介质中,用电感耦合等离子体发生光谱法(ICP-AES)测定溶液中的铌钽。该方法p(Nb_2O_5)和p(T_2O_5)在0～20μg/mL时,铌钽原子发射光谱强度与浓度呈良好的直线关系,Nb、Ta标准曲线相关系数R分别为0.999 9和0.999 7。检出限分别为0.023μg/mL和0.072μg/mL。本方法测定标准样品,测定值与认定值相符。对实际样品分析,Nh、Ta的相对标准偏差(n=6)分别为0.42%～2.3%和1.8%～3.3%,加标回收率均为97%～103%。适合地质找矿、选冶等领域的样品测试。

The ore samples were dissolved by mixed acids and then determined the niobium and tantalum in tartaric acid by inductively coupled plasma atomic emission spectrometry （ICP- AES）. The emission spectral intensity of niobium and tantalum showed linear relationship with the concentration when p （ Nb2O5 ） and p （ Ta2O5 ） in the range of 0 - 20 μg/mL and the correlation coefficients of calibration curve for niobium and tantalum were 0. 999 9 and 0. 999 7. The detection limits for niobium and tantalum were 0. 023 μg/mL and 0. 072 μg/mL. The method was applied to the analysis of standard sample, and the results were consistent with the certified values. The relative standard deviations （RSD, n = 6） were 0.42% -2. 3% and 1.8% - 3.3% for niobium and tantalum, and the recovery rate was 97% - 102% to actual samples. The method is suitable for sample test in geological prospecting and metallurgy.