火花放电原子发射光谱法测定中低合金钢中镧和铈  

Determination of lanthanum and cerium in medium-low alloysteel by spark discharge atomic emission spectrometry

作　　者：赵梦莹 徐永林 王姗姗 秦汉成 杨志强 鞠新华 ZHAO Mengying;XU Yonglin;WANG Shanshan;QIN Hancheng;YANG Zhiqiang;JU Xinhua(Shougang Group Company Limited Research Institute of Technology,Beijing 100043,China)

机构地区：[1]首钢集团有限公司技术研究院,北京100043

出　　处：《冶金分析》2023年第9期35-40,共6页Metallurgical Analysis

摘　　要：在炉前检验中,快速、准确测定中低合金钢中La、Ce元素含量,对推进稀土添加中低合金钢的开发具有重要意义。采用高频感应重熔炉制备内部校准样品,选择La 433.37nm(1级)、Ce 413.76nm(1级)作为La和Ce的分析线,Fe 273.1nm(1级)作为内标线,建立了火花放电原子发射光谱法测定中低合金钢中La、Ce含量的方法。对积分时间、预燃时间等进行试验,优化后分析条件如下:积分时间为8s,预燃时间为6s。在优化的实验条件下,采用干扰系数法进行校正,绘制校准曲线,其线性相关系数为0.9974(La)和0.9970(Ce);方法检出限为0.000033%(La,质量分数,下同)和0.00033%(Ce)。按照实验方法测定中低合金钢X80样品中La和Ce,结果的相对标准偏差(RSD,n=10)为5.5%和3.5%;并用电感耦合等离子体质谱法(ICP-MS)和电感耦合等离子体原子发射光谱法(ICP-AES)进行比对试验,结果相一致。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 433.37nm(level 1)and Ce 413.76nm(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 8s,and the pre-combustion time was 6s.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 0.9974and 0.9970,respectively.The limits of detection for La and Ce were 0.000033%(mass fraction,the same below)and 0.00033%,respectively.The contents of La and Ce in middle-low alloy steel sample of X80were 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.

关 键 词：火花放电原子发射光谱法 中低合金钢 镧 铈 

分 类 号：O657.31[理学—分析化学] TF031[理学—化学]