Abstract:During the determination of niobium in steel by inductively coupled plasma atomic emission spectrometry (ICP-AES),the conventional analytical line of niobium (Nb 316.340 nm) is not available in many types of ICP-AES instruments.Therefore, it is necessary to select other available analytical lines.The determination of niobium in steel by ICP-AES was established using Nb 269.706 nm as the analytical line.The spectral interference was corrected by multi-component spectral fitting (MSF).The results showed that iron had spectral interference with Nb 269.706 nm,which deteriorated the linearity of calibration curve prepared by certified reference materials with different contents,thus seriously affecting the analysis accuracy.After correcting the spectral interference of iron with Nb 269.706 nm by MSF method,the linear correlation coefficient of calibration curve was 0.999 9.The limit of detection was 0.000 7%.The content of niobium in actual steel samples was determined according to the experimental method.The relative standard deviations (RSD, n=6) of measured results were between 1.4% and 11%. The recoveries were between 92% and 101%.The measured results of niobium in steel certified reference materials were consistent with the certified value, which proved the accuracy of this method.
[1] 杨作宏,陈伯春.谈微合金元素Nb、V、Ti在钢中的作用[J].甘肃冶金(Gansu Metallurgy),2000(4):20-22. [2] 田永生,丁美英.ICP-MS测定钢中铌[J].冶金分析,2012,32(增:化学分册):324-325. TIAN Yongsheng,DING Meiying.Determination of Nb in steels by ICP-MS[J].Metallurgical Analysis,2012, 32(Suppl.:Chemistry):324-325. [3] 张亮亮,吴锐红,聂海明,等.干扰系数校正-电感耦合等离子体原子发射光谱法测定镍基合金中铈[J].冶金分析,2021,41(4):73-80. ZHANG Liangliang,WU Ruihong,NIE Haiming,et al.Determination of cerium in nickel-based alloy by inductively coupled plasma atomic emission spectrometry with interference coefficient correction[J].Metallurgical Analysis,2021,41(4):73-80. [4] 于英杰,孙莹,马洪波.电感耦合等离子体原子发射光谱法测定铝硅活塞合金中镧铈镨钕钇[J].冶金分析, 2018,38(4):69-73. YU Yingjie,SUN Ying,MA Hongbo.Determination of lanthanum,cerium,praseodymium,neodymium and yttrium in aluminum-silicon piston alloy by inductively coupled plasma atomic emission spectrometry[J]. Metallurgical Analysis,2018,38(4):69-73. [5] 于媛君,亢德华,杨丽荣,等.电感耦合等离子体原子发射光谱法测定钢中钨钼铌方法标准的探讨[J].冶金分析,2018,38(7):73-79. YU Yuanjun,KANG Dehua,YANG Lirong,et al.Discussion on standard method for determination of tungsten, molybdenum and niobium in steels by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2018,38(7):73-79. [6] 吴超超,梁小红,叶玉锋,等.电感耦合等离子体原子发射光谱法测定钢中铌含量[J].南方金属,2017(4): 13-16. WU Chaochao,LIANG Xiaohong,YE Yufeng,et al.Determination of niobium in steel by inductively coupled plasma atomic emission spectrometry[J].Southern Metals,2017(4):13-16. [7] 杨忠梅,闫宏江,杨忠辉.电感耦合等离子体原子发射光谱法测定钢中低含量钒和铌[J].冶金分析,2006, 26(3):100-101. YANG Zhongmei,YAN Hongjiang,YANG Zhonghui.The determination of vanadium and niobium in steel by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2006,26(3):100-101. [8] 张桂竹,李国华.电感耦合等离子体原子发射光谱法测定高温合金和耐热不锈钢中铌时钒、钛、铬的光谱干扰及校正[J].冶金分析,2013,33(8):43-48. ZHANG Guizhu,LI Guohua.Spectral interference and correction of vanadium,titanium and chromium during the determination of niobium in high temperature alloy and heat-resistance stainless steel by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2013,33(8):43-48. [9] 邹智敏,郭宏杰,马洪波,等.多元光谱拟合-电感耦合等离子体原子发射光谱法测定含铌镍基高温合金中铜[J].冶金分析,2016,36(8):78-82. ZOU Zhimin,GUO Hongjie,MA Hongbo,et al.Determination of copper in niobium-bearing nickel-based superalloy by multi-component spectral fitting-inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2016,36(8):78-82. [10] 严子心,曲景奎,余志辉,等.多谱线拟合-电感耦合等离子体原子发射光谱法测定高纯镍中痕量钴[J].分析化学,2019,47(3):423-428. YAN Zixin,QU Jingkui,YU Zhihui,et al.Multi-spectral fitting-determination of trace cobalt in high purity nickel by inductively coupled plasma atomic emission spectrometry[J].Chinese Journal of Analytical Chemistry,2019,47(3):423-428.