Determination of sixteen trace impurity elements in high- purity nickel by glow discharge mass spectrometry
YANG Hai-an1,2, LUO Shun1,2, YAN Yu-xin1,2 ,LIU Ying-bo1,2
1. Kunming Metallurgy Research Institute, Kunming 650031,China; 2. National Non- Ferrous Metal Products Quality Supervision and Inspection Center, Kunming 650031, China
Abstract：Total sixteen trace impurity elements (including silicon, phosphorus, sulfur, manganese, iron, cobalt, zinc, arsenic, cadmium, antimony, tin, lead, bismuth, magnesium, aluminum and copper) in high-purity nickel were directly determined by glow discharge mass spectrometry (GD-MS) without the preparation of calibration curve using certified reference materials. The optimal instrumental parameters for the analysis of high-purity nickel were obtained and the methods for the adjustment of parameters were summarized. The pollution of sodium, calcium and iron introduced by sample pretreatment could be completely eliminated by setting the pre-sputtering time of 20 min. The highest abundance (24Mg,27Al,28Si,31P,114Cd,32S,209Bi,75As,55Mn,56Fe,59Co,63Cu,121Sb,208Pb) were used as analytical isotopes under moderate resolution mode to reduce the mass spectra interference of isotopes. However, zinc and tin were an exception. Although abundance of 64Zn and 120Sn was the highest , but their mass spectra peaks overlapped with those of 36Ar14N16O and 82Se36Ar. Therefore, separable mass spectra peak and lower abundance 66Zn and 118Sn were selected for analytical isotopes in the test. The proposed experimental method was used to the analysis of three high-purity nickel samples and the determination values of sixteen trace impurity elements were consistent with the reference values and those obtained by inductively coupled plasma mass spectrometry (ICP-MS). The precision became better with the increase of elemental content. The relative standard deviation (RSD) was less than 10% when the content of element was in the level of μg/g.
杨海岸,罗 舜,闫豫昕,刘英波. 辉光放电质谱法测定高纯镍中16种痕量杂质元素[J]. 冶金分析, 2015, 35(5): 1-6.
YANG Hai-an, LUO Shun, YAN Yu-xin ,LIU Ying-bo. Determination of sixteen trace impurity elements in high- purity nickel by glow discharge mass spectrometry. , 2015, 35(5): 1-6.
Gijbels R, Van Straaten M, Bogaerts A. Mass spectrometric analysis of inorganic solids: GDMS and other methods [J]. Adv. Mass Spectrom. , 1995, 13: 241- 256.
[16]
赵墨田,曹永明,陈刚,等. 无机质谱概论 [M]. 北京:化学工业出版社,2006.
[17]
刘红,李爱嫦,李继东. 辉光放电质谱法测定高纯铟中痕量元素 [J]. 分析实验室(Chinese Journal of Analysis Laboratory),2012,31(5):10-12.
[18]
徐常昆,周涛,赵永刚. 辉光放电质谱应用和定量分析 [J]. 岩矿测试(Rock and Mineral Analysis),2012,31(2):47-56.
