Determination of zirconium,niobium,hafnium,tantalum and rare earth elements in geological sample by inductively coupled plasma mass spectrometry with sodium peroxide alkali fusion
SUN Menghua1,2, ZHU Yongxiao1,2, ZHAO Ye*1,2, CHEN Qingzhi1,2, SONG Fan1,2, SUN Kaixi1,2
1. Hebei Research Center for Geoanalysis,Baoding 071051,China; 2. Hebei Provincial Key Laboratory of Mineral Resources and Ecological Environment Monitoring,Baoding 071051,China
Abstract：The determination of Zr,Nb,Hf,Ta, and rare earth elements in geological samples has important significance for exploration and utilization of rare earth mineral resources as well as the geological environment researches such as geochemistry and petrogenesis. The sample was melted with Na2O2 at 750 ℃ for 8 min followed by leaching with boiling water. After filtration, the hydroxide precipitates were dissolved with HCl-H2O2 mixed solution in stages. The interferences of oxides or hydroxides of light rare earth elements with heavy rare earth elements were overcome by selecting He collision cell mode and interference correction equation. Rh was used to correct Zr, Nb, Sc, Y, La, Ce, Pr, Nd and Sm, and Re was used to correct Hf, Ta, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu. Consequently,a method for simultaneous determination of Zr, Nb, Hf, Ta and rare earth elements in geological sample was established by inductively coupled plasma mass spectrometry(ICP-MS). Under the optimized experimental conditions, the linear correlation coefficients of calibration curves of 20 elements were all not less than 0.999 2. The limits of detection were in range of 0.03-2.69 μg/g, and the limits of quantitation were in range of 0.09-8.07 μg/g. The contents of Zr, Nb, Hf, Ta and rare earth elements in certified reference materials of stream sediment and rock were determined according to the proposed method, and the relative errors (RE) between the results and certified values were all not more than 6.7%, which could meet the allowable limit requirements of relative error in industry standard of DZ/T 0130-2006. The relative standard deviations (RSD, n=12) were all not more than 4.8%. The proposed method was applied for determination of Zr, Nb, Hf, Ta and rare earth elements in soil, stream sediment and rock samples, and the RSDs (n=6) of determination results were between 0.5% and 4.8%.
孙孟华, 朱永晓, 赵烨, 陈庆芝, 宋凡, 孙凯茜. 过氧化钠碱熔-电感耦合等离子体质谱法测定地质样品中锆铌铪钽和稀土元素[J]. 冶金分析, 2024, 44(9): 35-44.
SUN Menghua, ZHU Yongxiao, ZHAO Ye, CHEN Qingzhi, SONG Fan, SUN Kaixi. Determination of zirconium,niobium,hafnium,tantalum and rare earth elements in geological sample by inductively coupled plasma mass spectrometry with sodium peroxide alkali fusion. , 2024, 44(9): 35-44.
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