Determination of 16 rare earth elements in graphite ore by inductively coupled plasma mass spectrometry with microwave digestion
LI Xiaojing1,2, HU Yanqiao1,2, ZHANG Jinming1,2, RAN Zhuo1,2, ZHAO Liangcheng1,2, JIN Qian*1,2
1. Hebei Research Center for Geoanalysis,Baoding 071051,China; 2. Hebei Key Laboratory of Mineral Resources and Ecological Environment Monitoring,Baoding 071051,China
Abstract：The determination of rare earth elements in graphite ore is of great significance in evaluating resource value, protecting the environment, and scientific research. In experiments, the samples were treated by high-temperature microwave digestion in HNO3-HF-HClO4-H2SO4 system. The collision mode was used with helium (He) flow rate of 4-5 mL/min. 45Sc, 89Y, 139La, 140Ce, 141Pr, 146Nd, 147Sm, 153Eu, 157Gd, 159Tb, 163Dy, 165Ho, 166Er, 169Tm, 172Yb, and 175Lu were selected as the isotopes to be measured. Sc, Y, La, Ce and Pr were corrected using Rh, and Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu were corrected using Re. The multi-atomic ion interference of 157Gd, 153Eu, 159Tb and 169Tm was corrected by the interference correction equation. The method for the determination of 16 rare earth elements in graphite ore by electrical coupled plasma mass spectrometry (ICP-MS) with microwave digestion was established. Under the optimized experimental conditions, the linear correlation coefficients of calibration curves of rare earth elements were between 0.999 7 and 1.000 0. The limits of detection were between 0.002 6 and 0.065 μg/g, and the limits of quantification were between 0.008 7 and 0.22 μg/g. The contents of 16 rare earth elements in graphite ore standard substances for composition analysis were determined according to the experimental method for 15 times in parallel. The relative standard deviations (RSD, n=15) of determination results were all less than 3.5%. The mixed standard working solution of rare earth elements were added based on 0.5-2 fold of element content for the spiked recovery tests, and the recoveries were between 90% and 105%. 16 rare earths in graphite ore sample were analyzed according to the experimental method, and the measurement results were basically consistent with those obtained by ashing-mixed acid dissolution-ICP-MS method.
李晓敬, 胡艳巧, 张金明, 冉卓, 赵良成, 金倩. 微波消解-电感耦合等离子体质谱法测定石墨矿中16种稀土元素[J]. 冶金分析, 2024, 44(8): 18-26.
LI Xiaojing, HU Yanqiao, ZHANG Jinming, RAN Zhuo, ZHAO Liangcheng, JIN Qian. Determination of 16 rare earth elements in graphite ore by inductively coupled plasma mass spectrometry with microwave digestion. , 2024, 44(8): 18-26.
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