The determination method of 12 major impurity elements in rodlike high-purity magnesium (including Al, Si, Ca, Cr, Mn, Fe, Ni, Cu, Zn, Sn, Pb and Bi) by glow discharge mass spectrometry (GD-MS) was established. The results showed that the discharge surface area of rodlike sample was small and the discharge was instable. When the discharge current was 47.0mA and the gas flow was 599mL/min, the matrix signal was stable. Meanwhile, the strength could meet the testing requirements. The pollution of Na, Fe and Ca on sample surface could be fully removed by pre-sputtering for 15min. The abundance of 27Al, 28Si, 52Cr, 55Mn, 56Fe, 58Ni, 63Cu, 64Zn, 208Pb and 209Bi was highest, and the analytical results were good under moderate resolution mode. Since 40Ar had interference with the determination of 40Ca, 44Ca was selected as the determination isotope and the analytical results were good under moderate resolution mode. 120Sn could be fully separated from 40Ar40Ar40Ar when the resolution was higher than 7960, so 120Sn was selected as isotope for determination under high resolution mode. Twelve impurity elements in rodlike high-purity magnesium were determined according to the experimental method. The relative standard deviations (RSD, n=5) were between 1.8% and 10.9%. The standard deviations (SD, n=5) of all analysis results were less than the repeatability limit specified in national standard method (GB/T 13748). The found results were compared with those obtained by inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES) with standard addition. The consistence of most elements was good. Since the relative sensitivity factor (RSF) of rodlike magnesium sample was different from the standard RSF, the determination results of Fe, Cu and Zn showed large difference. However, the determination results had no great influence on the purity grading of high-purity substance.
刘元元, 胡净宇. 辉光放电质谱法测定棒状高纯镁中12种杂质元素[J]. 冶金分析, 2018, 38(4): 16-21.
LIU Yuan-yuan, HU Jing-yu. Determination of twelve impurities in rodlike high-purity magnesium by glow discharge mass spectrometry. , 2018, 38(4): 16-21.
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