Investigation on sample preparation method of high purity indium sheet in analysis of conductor and non-conductor sample by direct current glow discharge mass spectrometry
TAN Xiu-zhen1, LI Yao1, LIN Qian-bin1, ZHU Liu1, DENG Yu-ning2
1. Guangdong First Rare Materials Co., Ltd., National Engineering and Technology Research Center of Scattered Metal, Qingyuan 511875, China; 2. Qingyuan First Materials Co.,Ltd., Qingyuan 511517, China
Abstract：After the thin sheet of high-purity indium was used as adhesive, proper sample was selected and pressed on In thin sheet. Then the content of impurity elements was determined by direct current glow discharge mass spectrometry (dc-GDMS) in three types of materials including bulk non-conductor of red phosphorus, powder non-conductor of Al2O3 and powder conductor of In2O3 and Lu2O3. The effects of sample mass and discharge parameter on matrix signal intensity and its stability were investigated. The optimized testing conditions were listed as follows: (1) for the bulk non-conductor sample of red phosphorus, the proper sample size was about 2mm×3mm×1mm; the sample was pressed on In sheet by hand-operated press machine; the discharge current was 1.5mA and the discharge voltage was 850V; (2) for the powder non-conductor sample of Al2O3, the diameter of Al2O3 powder pressed on In sheet was about 3mm; the discharge current was 1.7mA and the discharge voltage was 900V; (3) for the powder conductor samples of In2O3 and Lu2O3, the diameter of In2O3 and Lu2O3 powder pressed on In sheet was about 7-8mm; the discharge current was 1.8mA and the discharge voltage was 950V. The experimental method was applied for the determination of red phosphorus, Al2O3, In2O3 and Lu2O3 samples. The detection limit of impurity elements in red phosphorus was one order of magnitude lower than those in Al2O3. The relative standard deviation of five independent measurements of In2O3 was within 20%, and the determination results of most elements were basically consistent with those obtained by inductively coupled plasma mass spectrometry (ICP-MS). Although the determination results of Na, Al, Sn and Pb had relatively large difference, the order of magnitude was the same, which had no great influence on the grading of high-purity metal products. The determination results of rare earth elements in Lu2O3 were also basically consistent with those obtained by ICP-MS.
谭秀珍, 李瑶, 林乾彬, 朱刘, 邓育宁. 直流辉光放电质谱分析导体和非导体样品的高纯铟片制样方法研究[J]. 冶金分析, 2018, 38(9): 1-7.
TAN Xiu-zhen, LI Yao, LIN Qian-bin, ZHU Liu, DENG Yu-ning. Investigation on sample preparation method of high purity indium sheet in analysis of conductor and non-conductor sample by direct current glow discharge mass spectrometry. , 2018, 38(9): 1-7.
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