Determination of scandium in high purity rare earths and their oxides by inductively coupled plasma mass spectrometry
FAN Xiaolong1,2, BAO Xiangchun*1,2
1. State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization of Baotou Research Institute of Rare Earths,Baotou 014030,China; 2. Ruike National Engineering Research Center of Rare Earth Metallurgy and Function Materials,Baotou 014030,China
Abstract：With the extensive application of high purity rare earths and their oxides in industrial production, the requirements for their purity are increased gradually. Therefore, it is necessary to accurately determine the content of scandium in high purities rare earths and their oxides. After the sample was dissolved with 10 mL of HNO3 and 3-5 drops of H2O2, a determination method of scandium in high purity rare earths and their oxides by inductively coupled plasma mass spectrometry (ICP-MS) was established with 133Cs as the internal standard and 2%(V/V) HNO3 as the determination medium. High purity yttrium oxide, high purity lanthanum oxide, high purity praseodymium oxide, high purity europium oxide, high purity holmium oxide and high purity ytterbium oxide were selected from the light, medium and heavy rare earths to prepare the matrix solutions with matrix mass concentrations of 0.20, 0.50, 0.70 and 1.00 mg/mL, respectively, and scandium standard solution was added to make sure that the mass concentrations of scandium oxide were all at 10.00 ng/mL. The relationship between these matrix mass concentrations in the range of 0.20-1.00 mg/mL and the signal intensity of scandium was investigated. The results showed that there was a good linear relationship between the signal intensity of scandium and matrix concentration with linear correlation coefficients all not less than 0.97, indicating that the matrix effects were negligible. The changes in signal intensity of internal standard of cesium and rhodium with scandium were investigated at different matrix concentrations. The results showed that the reduction degree of cesium signal intensity was basically the same as that of scandium, so 10.00 ng/mL of cesium was selected as the internal standard to correct the content of scandium. The results showed that when the mass concentration of scandium was in the range of 1.00-100.00 ng/mL, the correlation coefficient of calibration curve was greater than 0.999 5, the detection limit of this method was 0.045 μg/g, the limit of quantification was 0.15 μg/g. The proposed method was applied in determination of scandium (The results of high purity rare earth oxides are expressed in scandium oxide) in samples of high purity lanthanum, high purity lanthanum oxide, high purity europium oxide and high purity ytterbium oxide, and the relative standard deviations (RSD, n=11) were between 6.2% and 7.9%. The contents of scandium in samples of high purity lanthanum, high purity samarium, high purity ytterbium, high purity yttrium oxide, high purity lanthanum oxide, high purity praseodymium oxide, high purity europium oxide, high purity holmium oxide and high purity ytterbium oxide were determined by the proposed method. The recoveries were between 96% and 104%, and the results were basically consistent with standard addition method.
范小龙, 包香春. 电感耦合等离子体质谱法测定高纯稀土及其氧化物中钪[J]. 冶金分析, 2023, 43(9): 14-20.
FAN Xiaolong, BAO Xiangchun. Determination of scandium in high purity rare earths and their oxides by inductively coupled plasma mass spectrometry. , 2023, 43(9): 14-20.
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