称量定容-ICP-AES法测定纯铁中痕量铝、铬、铜、锰、镍和硅

详细信息    查看全文 | 推荐本文 |

英文篇名：Determination of trace Al,Cr,Cu,Mn,Ni,Si in pure iron by ICPAES with mass dilution method 作者：李帆 ; 杨春晟 ; 丁妍 ; 叶晓英 英文作者：LI Fan;YANG Chun-sheng;DING Yan;YE Xiao-ying;AECC Beijing Institute of Aeronautical Materials;Beijing Key Laboratory of Aeronautical Materials Testing and Evaluation;Aviation Key Laboratory of Science and Technology on Materials Testing and Evaluation; 关键词：ICP-AES ; 称量定容 ; 纯铁 ; 痕量元素 英文关键词：ICP-AES;;Mass dilution method;;Iron;;Trace elements 中文刊名：FXSY 英文刊名：Chinese Journal of Analysis Laboratory 机构：中国航发北京航空材料研究院检测研究中心;航空材料检测与评价北京市重点实验室;材料检测与评价航空科技重点实验室; 出版日期：2019-04-15 11:27 出版单位：分析试验室 年：2019 期：v.38 基金：国家重点研发计划(2016YFB0701401)资助 语种：中文; 页：FXSY201905007 页数：6 CN：05 ISSN：11-2017/TF 分类号：36-41

摘要

纯铁样品5. 000 g用HCl(1+1)溶液9 mL和3 mL硝酸溶解,采用称量定容方法定容至50 g。采用电感耦合等离子体发射光谱法测定其中痕量铝、铬、铜、锰、镍和硅元素,选择的分析谱线依次为Al 396. 152 nm,Cr 267. 716 nm和359. 348 nm,Cu 324. 754 nm和327. 396 nm,Mn293. 306 nm和257. 610 nm,Ni 221. 647 nm和351. 505 nm,Si 212. 412 nm和288. 158 nm。通过样品标准加入法求出样品中杂质元素含量后重新建立工作曲线,上述元素的质量分数在0. 0005%～0. 01%之间与其发射强度呈线性关系,方法的检出限在0. 00002%～0. 0002%之间,以空白样品为基体进行加标回收实验,所得回收率在84. 0%～121%之间,相对标准偏差(RSD)在0. 6%～30%之间。测定了纯铁标准物质中质量分数在0. 003%～0. 44%的分析元素,测量值与标准值基本一致,相对标准偏差(RSD)在1. 0%～15%之间。
        5. 000 g sample was dissolved with 9 m L of HCl( 1 + 1) and 3 m L of HNO3 solution and the solution was diluted to 50 g. Trace amounts of Al,Cr,Cu,Mn,Ni and Si in the solution were determined by ICP-AES. Analytical spectral lines of Al 396. 152 nm,Cr 267. 716 nm and359. 348 nm,Cu 324. 754 nm and 327. 396 nm,Mn 293. 306 nm and 257. 610 nm,Ni 221. 647 nm and 351. 505 nm,Si 212. 412 nm and 288. 158 nm for the determination of the 6 elements,respectively. Linear relationships between emission intensity and mass fraction of the elements were obtained in the range of 0. 0005%-0. 01%,with detection rage of 0. 00002%-0. 0002%. On the base of blank sample,the recoveries were in the range of 84. 0%-121%,with RSD in the range of0. 6%-30%. Iron standard substances were determined with the RSD in the range of 1. 0%-15%.

引文

[1] Dong S Z. Chin J Spectrosc Lab,1993,10(4):27董淑珍.光谱实验室,1993,10(4):27
    [2] Li X Y,He X L. Metallurg Anal,1996,16(4):45李新友,何新礼.冶金分析,1996,16(4):45
    [3] Yang S Y. Metallurg Anal,1987,7(3):63杨似燕.冶金分析,1987,7(3):63
    [4] Yu J R,Cui Z J. Chinese J. Anal. Chem.,1983,11(8):612于金润,崔贞姬.分析化学,1983,11(8):612
    [5] Wen X D,Cao H Y,Yang Y. Res Iron Steel,2008,36(4):45闻向东,曹宏燕,杨芸.钢铁研究,2008,36(4):45
    [6] Geng L J,Mao J W,Liu X W,et al. Metallurg Anal,2008,28(6):72耿丽君,毛敬伟,刘信文等.冶金分析,2008,28(6):72
    [7] Chen S,Yan Y,Zhong X H,et al. Metallurg Anal,2004,24(5):36陈胜,鄢艳,钟秀怀等.冶金分析,2004,24(5):36
    [8] Nie L Q,Ji H L. Metallurg Anal,2008,28(10):19聂玲清,纪红玲.冶金分析,2008,28(10):19
    [9] Huang M,Fang Z,He H Z,et al. Chin. J. Anal. Lab.,2011,30(9):96黄梅,方智,何会珍等.分析试验室,2011,30(9):96
    [10] Sun D Y,He L W,Xie D. Chin. J. Anal. Lab.,2014,33(7):855孙东亚,何丽雯,谢安.分析试验室,2014,33(7):855
    [11] Yuan H L,Cui F H,Ye Y,et al. Chin. J. Anal. Lab.,2016,35(1):38袁华丽,崔芙红,叶莹等.分析试验室,2016,35(1):38
    [12] Yu X Z,Shen J P,Sun J,et al. Chin. J. Anal. Lab.,2016,35(2):197余晓志,沈杰平,孙剑等.分析试验室,2016,35(2):197