Determination of 73 trace impurity elements in high purity lutetium oxide by radio frequency glow discharge mass spectrometry
JIANG Wei1,2, SUN Na1,2, XU Na*1,2, LI Ping1,2, XIE Min1,2
1. National Center of Quality Testing and Inspection for Tungsten and Rare Earth Products,Ganzhou 341000,China; 2. JiangXi Institute of Tungsten and Rare Earth,Ganzhou 341000,China
Abstract：The existing method for the detection of lutetium oxide cannot cover the detection of whole elements, and also cannot meet the determination requirements of super trace elements. Therefore, a method for the determination of 73 impurity elements in high-purity lutetium oxide by pressed powder pellet-radio frequency glow discharge mass spectrometry(RF-GD-MS) was established. The intensity of matrix signal was controlled to 0.30 nA or higher. The flow rate of discharge gas was 0.8 mL/min, the radio frequency power was 38 W, and the pre-sputtering time was 20 min. RF-GD-MS was applied for the determination of 73 trace impurity elements in high-purity lutetium oxide samples, and the found results were compared with those obtained by direct current glow discharge mass spectrometry (DC-GD-MS). It was found that the determination results of two methods had good consistency when the content of impurity elements was in range of 0.01-2 mg/kg. In other words, the measurement results of impurity elements in same sample were not affected by the light source, i.e., direct current or radio frequency. But RF-GD-MS had higher sensitivity and lower limit of detection compared with DC-GD-MS. The limit of detection of some impurity elements could reach 0.001 mg/kg for RF-GD-MS method, while the limit of detection for DC-GD-MS could only reach 0.05 mg/kg. The limits of detection were in range of 0.001-0.39 mg/kg, and the limits of quantification were in range of 0.005-1.30 mg/kg. The proposed method was applied to the determination of 73 trace impurity elements in high-purity lutetium oxide samples. The results showed that the relative standard deviations(RSD,n=7) were within 10% for the impurity elements with content (mass fraction, similarly hereinafter) higher than 1 mg/kg. For the impurity elements with content in range of 0.1-1 mg/kg, the RSDs were within 20%. For the impurity elements with content lower than 0.1 mg/kg, the RSDs were within 30%. Some representative elements in high-purity lutetium oxide samples were determined according to the experimental method. The found results were compared with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) in national standard methods (GB/T 12690 series) and GB/T 18115.15-2010. For the elements with content of 1 mg/kg, the determination results of two methods were consistent.
蒋威, 孙娜, 徐娜, 李平, 谢敏. 射频辉光放电质谱法测定高纯氧化镥中73种痕量杂质元素[J]. 冶金分析, 2023, 43(1): 16-24.
JIANG Wei, SUN Na, XU Na, LI Ping, XIE Min. Determination of 73 trace impurity elements in high purity lutetium oxide by radio frequency glow discharge mass spectrometry. , 2023, 43(1): 16-24.
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