1. AECC Beijing Institute of Aeronautical Materials, Beijing 100095, China; 2. Beijing Key Laboratory of Aeronautical Materials Testing and Evaluation,Beijing 100095, China; 3. Beijing Tongzhou District Quality Inspection and Inspection of Agricultural Products, Beijing 101149, China
Abstract：Nickel-based high temperature alloys were widely used in hot end components of aero-engines. The purity of main raw material (high-purity nickel) had important influence on the properties of alloys. Therefore, the content of trace elements in high-purity nickel should be determined and controlled. Proper isotopes were selected to overcome the mass spectral interference. The calibration curves were prepared by standard addition method to eliminate the matrix effect. The flow rate of auxiliary gas was optimized. The contents of calcium and arsenic were determined at high resolution mode, while the contents of other elements were determined at middle resolution mode. The determination method of 25 trace elements (magnesium, aluminum, phosphorus, calcium, manganese, iron, copper, zinc, gallium, germanium, arsenic, selenium, silver, cadmium, indium, tin, antimony, tellurium, gold, mercury, thallium, lead, bismuth, thorium and uranium) in high-purity nickel by high resolution inductively coupled plasma mass spectrometry was established. Under the optimized experimental conditions, the linear correlation coefficients of calibration curves were all higher than 0.999. The limits of detection of method ranged from 0.003 μg/L to 0.15 μg/L. The limits of quantification were in range of 0.010-0.50 μg/L. The contents of trace elements in three high-purity nickel samples (purity of 99.99%) were determined according to the experimental method. Meanwhile, the recovery test with different gradients was conducted with one high-purity nickel sample. The results showed that relative standard deviations (RSD, n=8) of determination values were between 3.5% and 9.7%. The recoveries were between 90% and 110%. The certified reference material of pure nickel was determined according to the experimental method, and the results were basically consistent with the standard values. The contents of 25 impurity elements in high-purity nickel sample were determined according to the experimental method, and the results were compared with the glow discharge mass spectrometry. It was found that the determination results of two analytical methods were consistent.
[1] 孙晓峰,金涛,周亦胄,等.镍基单晶高温合金研究进展[J].中国材料进展,2012,31(12):1-11. SUN Xiaofeng,JIN Tao,ZHOU Yizhou,et al.Research progress of nickel-base single crystal superalloys[J].Materials China,2012,31(12):1-11. [2] 姜周华,张新法,刘福斌,等.镍基高温合金生产用原材料有害杂质的控制[J].钢铁,2017,52(9):1-9. JIANG Zhouhua,ZHANG Xinfa,LIU Fubin,et al.Harmful impurities control of raw material used in Ni-based superalloy production[J].Iron and Steel,2017,52(9):1-9. [3] 中国人民解放军总装备部,国防科技工业标准化研究中心.GJB 8781.17—2015 高温合金痕量元素分析方法第10部分:石墨炉原子吸收光谱法测定硒含量[S].北京:总装备部军标出版发行部,2016. [4] 蒙益林.石墨炉原子吸收直接法测量钢中的微量Pb、Sb元素[J].分析试验室(Chinese Journal of Analysis Laboratory),2008,27(Suppl.):430-433. [5] 李庆美,朱纪夏.电感耦合等离子体原子发射光谱法测定低合金钢中酸溶硼[J].冶金分析,2013,33(10):77-80. LI Qingmei,ZHU Jixia.Determination of acid-soluble boron in low alloy steel by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2013,33(10):77-80. [6] 周桂海,梁峙,胡宏卫.电感耦合等离子体原子发射光谱法测定低合金钢中痕量铌[J].理化检验(化学分册),2016,52(10):1211-1213. ZHOU Guihai,LIANG Zhi,HU Hongwei.ICP-AES Determination of trace amount of niobium in low alloy steel[J].Physical Testing and Chemical Analysis(Part B:Chemical Analysis),2016,52(10):1211-1213. [7] 中国人民解放军总装备部,国放科技工业标准化研究中心.GJB 8781.16—2015 高温合金痕量元素分析方法第16部分:电感耦合等离子体质谱法测定硼、钪、镓、银、铟、锡、锑、铈、铪、铊、铅和铋含量[S].北京:总装备部军标出版发行部,2016. [8] 张洁,阳国运.电感耦合等离子体质谱法测定金矿石中金[J].冶金分析,2018,38(11):18-23. ZHANG Jie,YANG Guoyun.Determination of gold ore by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2018,38(11):18-23. [9] 靳兰兰,王秀季,李会来,等.电感耦合等离子体质谱技术进展及其在冶金分析中的应用[J].冶金分析,2016,36(7):1-14. JIN Lanlan,WANG Xiuji,LI Huilai,et al.Progress in inductively coupled plasma mass spectrometry technology and its application in metallurgical analysis[J]. Metallurgical Analysis,2016,36(7):1-14. [10] 钟胜贤,卢现友,刘景麟.电感耦合等离子体质谱法测定磷酸铁锂中杂质元素[J].冶金分析,2015,35(3):19-24. ZHONG Shengxian,LU Xianyou,LIU Jinglin,et al.Determination of impurity elements in lithium iron phosphate by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2015,35(3):19-24. [11] 余兴,李小佳,王海舟.辉光放电质谱法测定高温合金中的痕量元素[J].冶金分析,2004,24(增l):152-156. YU Xing,LI Xiaojia,WANG Haizhou.Determination of trace elements in superalloy by glow discharge mass spectrometry[J].Metallurgical Analysis,2004,24(zl):152-156. [12] 李兵,梁帮宏,苏冬萍,等.HR-ICP-MS测定高纯镍金属中的微量元素杂质[J].化学分析与研究,2019,3(7):1397-1400. LI Bing,LIANG Banghong,SU Dongping,et al.Determination of trace elements in high purity nickel metal by HR-ICP-MS[J].Chemical Research and Application,2019,3(7):1397-1400. [13] 朱莉,张毅,纪红聆.高分辨电感耦合等离子体质谱法测定含铜不锈钢中痕量磷[J].理化检验(化学分册),2020,56(3):332-335. ZHU Li,ZHANG Yi,JI Hongling,et al. Determination of trace phosphorus in copper-containing stainless steel by high resolution inductively coupled plasma mass spectrometry[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis),2020,56(3):332-335. [14] 李兵,梁帮宏,苏冬萍,等. HR-ICP-MS 测定高纯镍金属中的微量元素杂质[J].化学研究与应用,2019,31(7):1398-1400. LI Bing,LIANG Banghong,SU Dongping,et al.Determination of trace elements in high purity nickel metal by HR-ICP-MS[J].Chemical Research and Application,2019,31(7):1398-1400.
