Abstract：In the pre-furnace inspection, the rapid and accurate determination of La and Ce contents in the middle-low alloy steel is of great significance to promote the development of rare earth steel. The internal calibration samples was prepared with high-frequency induction remelting furnace. La 433.37 nm (level 1) and Ce 413.76 nm (level 1) were selected as the analytical lines for La and Ce, respectively, and Fe 273.1 nm (level 1) was used as the internal standard line. Thus, a method for determination of La and Ce in middle-low alloy steel by spark discharge atomic emission spectrometry was established. The experiments of integration time and pre-combustion time were conducted. The optimized analytical conditions were listed as follows: the integration time was 8 s, and the pre-combustion time was 6 s. Under the optimized experimental conditions, the interference coefficient method was employed for calibration, and the calibration curve was prepared. The linear correlation coefficients of La and Ce were 0.997 4 and 0.997 0, respectively. The limits of detection for La and Ce were 0.000 033% (mass fraction, the same below) and 0.000 33%, respectively. The contents of La and Ce in middle-low alloy steel sample of X80 were determined according to the proposed method. The relative standard deviations (RSD, n=10) of determination results were 5.5% for La and 3.5% for Ce. The comparative tests were also conducted with inductively coupled plasma mass spectrometry (ICP-MS) and inductively coupled plasma atomic emission spectrometry (ICP-AES), and the results were consistent.
[1] ZHU J,LIN G T,ZHANG Z H,et al.The martensitic crystallography and strengthening mechanisms of ultra-high strength rare earth H13 steel[J].Materials Science and Engineering:A,2020,797:140139. [2] TORCHANE L.Influence of rare earths on the gas nitriding kinetics of 32CrMoNiV5 steel at low temperature[J].Surfaces and Interfaces,2021,23:101016. [3] 杨健,李婷婷.稀土处理的无取向硅钢夹杂物控制研究进展[J].钢铁,2022,57(7):1-15. YANG Jian,LI Tingting.Research progress on inclusion control of non-oriented silicon steel with REM treatment[J].Iron & Steel,2022,57(7):1-15. [4] 董瀚,廉心桐,胡春东,等.钢的高性能化理论与技术进展[J].金属学报,2020,56(4):558-582. DONG Han,LIAN Xintong,HU Chundong,et al.High performance steels:the scenario of theory and technology[J].Acta Metallurgica Sinica,2020,56(4):558-582. [5] CHEN Rongchun,WANG Zhigang,ZHU Fusheng,et al.Effects of rare-earth micro-alloying on microstructures,carbides,and internal friction of 51CrV4 steels[J].Journal of Alloys and Compounds,2020,824:153849. [6] ZHANG Yue,XIAO Jun,LIANG Juhua,et al.Effect of rare earth elements on the segregation behavior and microstructure of super austenitic stainless steel[J].Journal of Materials Research and Technology,2022,19(7):20-29. [7] 胡洪澳,杨吉春,富晓阳.痕量稀土对Super304不锈钢冲击性能的影响[J].中国稀土学报,2022,https://kns.cnki.net/kcms/detail/11.2365.tg.20220425.0905.002.html. HU Hongao,YANG Jichun,FU Xiaoyang.Effect of trace rare earth on impact properties of super 304 stainless steel[J].Journal of the Chinese Society of Rare Earths,2022,https://kns.cnki.net/kcms/detail/11.2365.tg.20220425.0905.002.html. [8] WANG Changgang,MA Rongyao,ZHOU Yangtao,et al.Effects of rare earth modifying inclusions on the pitting corrosion of 13Cr4Ni martensitic stainless steel[J].Journal of Materials Science and Technology,2021,93(12):232-243. [9] ZHANG Jing,SU Chunming,CHEN Xianpei,et al.First-principles study on pitting corrosion of Al deoxidation stainless steel with rare earth element(La) treatment[J].Materials Today Communications,2021,27:102204. [10] YANG Chaoyun,LUAN Yilun,LI Dianzhong,et al.Very high cycle fatigue behavior of bearing steel with rare earth addition[J].International Journal of Fatigue,2020,131:105263. [11] 赵允琦,于明明,肖俊杰,等.偶氮胂-Ⅲ分光光度法测定废弃荧光粉中稀土总量[J].现代矿业,2021,37(1):248-250. ZHAO Yunqi,YU Mingming,XIAO Junjie,et al.Determination of total rare earths in the waste phosphors by spetrpohotometry with arsenazo-Ⅲ[J].Modern Mining,2021,37(1):248-250. [12] 黄永飞.偶氮氯膦-mA分光光度法测定钢中的稀土总量[J].宝钢技术,1997(5):49-52. HUANG Yongfei.Determination of total rare earths in steel with chlorophosphonazo-mA spectrophotometry[J].Baosteel Technology,1997(5):49-52. [13] 朱悦然,李佳,赵文怡,等.草酸盐质量法测定铁矿石中稀土总量[J].金属功能材料,2022,29(2):46-50. ZHU Yueran,LI Jia,ZHAO Wenyi,et al.Determination of total rare earth in iron ore by oxalate gravimetric method[J].Metallic Functional Materials,2022,29(2):46-50. [14] 龙旭东,高立红,张红,等.EDTA滴定法测定稀土铝中间合金中稀土总量[J].冶金分析,2020,40(4):70-75. LONG Xudong,GAO Lihong,ZHANG Hong,et al.Determination of total rare earths in intermediate alloy of rare earth aluminum by EDTA titration[J].Metallurgical Analysis,2020,40(4):70-75. [15] 王宴秋,张建军,刘钢耀.等离子体质谱法测定钢中镧、铈、镨、钕、钐[J].包钢科技,2019,45(6):91-94. WANG Yanqiu,ZHANG Jianjun,LIU Gangyao.Determination of lanthanum,cerium,praseodymium,neodymium and samarium in steel with inductively coupled plasma mass spectrum[J].Science and Technology of Baotou Steel,2019,45(6):91-94. [16] 任慧.ICP-AES法测定钢中的铈[J].化学分析计量,2012,21(4):53-55. REN Hui.Determination of Ce in steel by ICP-AES[J].Chemical Analysis and Meterage,2012,21(4):53-55. [17] 中华人民共和国国家质量监督检验检疫总局.JJF 1343—2012 标准物质定值的通用原则及统计学原理[S].北京:中国标准出版社,2012. [18] 中华人民共和国国家质量监督检验检疫总局.JJG 768—2005 发射光谱仪[S].北京:中国标准出版社,2005. [19] 中华人民共和国国家质量监督检验检疫总局.GB/T 24234—2009 铸铁 多元素含量的测定 火花放电原子发射光谱法(常规法)[S].北京:中国标准出版社,2009.
