Determination of the total amount of sixteen rare earth elements and its component in uhligite by inductively coupled plasma mass spectrometry
LIU Yan1,2,3, YAO Mingxing*1,2,3, ZHANG Liping1,2,3, FAN Lei1,2,3, ZHANG Hongli1,2,3, WANG Tiantian1,2,3
1. Zhengzhou Institute of Multipurpose Utilization of Mineral Resources, CAGS, Zhengzhou 450006, China; 2. Key Laboratory for Polymetallic Ores' Evaluation and Utilization, MNR, Zhengzhou 450006, China; 3. Key Laboratory of Comprehensive Utilization of Gold Resource in Henan Province, Zhengzhou 450006, China
Abstract：Zirconium and titanium with high temperature resistance and high hardness exist in uhligite. It is difficult to decompose the sample completely by conventional acid solution method, and the sample is easily adhered onto the crucible during the treatment by alkali fusion. The sample was melted with sodium carbonate and boric acid. The interference of heavy rare earth elements by the oxides or hydroxides of light rare earth elements was overcome by kinetic energy discrimination (KED) collision cell mode and interference coefficient correction method. Consequently, an analysis method of the total amount of sixteen rare earth elements and its component in uhligite, including scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, was established by inductively coupled plasma mass spectrometry(ICP-MS) with 50 ng/mL 185Re as internal standard. Six methods for sample decomposition were compared, including open acid solution with hydrochloric acid-nitric acid-hydrofluoric acid-perchloric acid, closed acid solution with nitric acid-hydrofluoric acid, microwave digestion with hydrofluoric acid, fusion with sodium peroxide-sodium hydroxide, fusion with borax, and fusion with sodium carbonate-boric acid. The results showed that the flux of sodium carbonate and boric acid exhibited the optimal decomposition effect on the sample. The matrix effect was reduced by sample dilution to control matrix concentration of 0.20 mg/mL and internal standard correction method. The experiments showed that the linear correlation coefficients of calibration curves of rare earth elements were between 0.999 1 and 1.000 0. The limit of detection was between 0.000 1 and 0.008 4 μg/g, and the limit of quantification was between 0.000 5 and 0.042 0 μg/g. The total amount of sixteen rare earth elements and its component in certified reference materials of zirconium ore with similar composition to uhligite were determined according to the experimental method. The results were basically consistent with the certified values. The proposed method was applied in the determination of uhligite sample. The relative standard deviations (RSDs, n=8) of determination results were between 1.2% and 4.0%. The reveries were between 94% and 110%, which could meet the allowable limit of recovery in range of 90%-110% in Part III of the national geological and mineral industry standard of DZ/T 0130-2006.
刘闫, 姚明星, 张丽萍, 樊蕾, 张宏丽, 王甜甜. 电感耦合等离子体质谱法测定锆钛矿中16种稀土元素分量及其总量[J]. 冶金分析, 2022, 42(3): 19-25.
LIU Yan, YAO Mingxing, ZHANG Liping, FAN Lei, ZHANG Hongli, WANG Tiantian. Determination of the total amount of sixteen rare earth elements and its component in uhligite by inductively coupled plasma mass spectrometry. , 2022, 42(3): 19-25.
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