Abstract：Based on the established calibration curve by the manufacturer, some factors affecting the determination process of glow discharge atomic emission spectrometry were discussed. Thus, the determination of multiple elements in high manganese steel was realized. The experiments showed that the following aspects should be paid attention in order to guarantee the analysis accuracy: (1) one spectral tracing must be performed every day before any standardization or analysis. On the one hand, the sample for tracing should be iron-based sample with uniform content; on the other hand, the exit slit position of the glow spectrometer could be adjusted to the optimal position through spectral tracing, thus ensuring the light passage with maximum strength. (2) The sampling must be strictly conducted according to the requirements in GB/T20066-2006 to make sure that samples were free of inclusions, cracks, stomata, oil contamination, dust and oxides. (3) The sample preparation was referred to GB/T4336-2016 and GB/T22368-2008. Both sides of the prepared samples should be flat. The analytical surface should be carefully polished to ensure smoothness and cleanness without pollution. (4) The purity and flow rate of argon should be guaranteed: the purity was above 99.999% and the pressure was 280kPa. (5) Although the drift correction would not change every day, one drift correction should be conducted every day before any standardization or analysis. Three certified reference materials of high manganese steel were analyzed according to the optimized experimental methods. The found results of each element were consistent with the certified values. The errors were all within the allowable deviation of the certified reference materials. The relative standard deviation (RSD, n=11) were between 0.81% and 9.7%
胡维铸, 赵广东, 牟英华, 隋月斯, 杨维秀. 辉光放电原子发射光谱法测定高锰钢中多元素的影响因素探讨[J]. 冶金分析, 2019, 39(6): 54-59.
HU Wei-zhu, ZHAO Guang-dong, MU Ying-hua, SUI Yue-si, YANG Wei-xiu. Discussion of influence factors on determination of multiple elements in high manganese steel by glow discharge optical emission spectrometry. , 2019, 39(6): 54-59.
李树索,陈希杰.高锰钢的发展与应用[J].矿山机械,1998(3):70-71.LI Shu-suo,CHEN Xi-jie.Development and application of high manganese steel[J].Mining & Processing Equipment,1998(3):70-71.
孙红英.直读光谱法测定高锰钢中的锰及不确定度评估[J].光谱实验室,2012,29(2):992-995.SUN Hong-ying.Determination of Mn in high manganese steel by direct reading spectrometry and its evaluation of uncertainty[J].Chinese Journal Spectroscopy Laboratory,2012,29(2):992-995.
[4]
邓军华,王一凌.X射线荧光光谱法测定高锰钢中锰的方法[J].鞍钢技术,2013(2):34-37.DENG Jun-hua,WANG Yi-ling.Method for determining content of manganese in high manganese steel by X-ray fluorescence spectrometry[J].Angang Technology,2013(2):34-37 .
[5]
吴旭晖,尹娜.电感耦合等离子体发射光谱法同时测定高锰钢中硅、锰、磷、铬[J].福建分析测试,2016,25(1):39-42.WU Xu-hui,YIN Na.Determination of Si,Mn,P,Cr in high manganese steel by ICP-AES[J].Fujian Analysis &Testing,2016,25(1):39-42.
R Kenneth Marcus,José A C Broekaert.Glow discharge plasmas in analytical spectroscopy[M].Chichester:John Wiley ＆Sons Ltd.,2003.
[8]
滕璇,李小佳,王海舟.中低合金钢的辉光放电发射光谱分析研究[J].冶金分析,2003,23(5):1-5.TENG Xuan,LI Xiao-jia,WANG Hai-zhou.Study on the analysis of middle-low alloy steels by dc-glow discharge optical emission spectrometry[J].Metallurgical Analysis,2003,23(5):1-5.
[9]
Nelis T,Payling R.Glow discharge optical emission spectroscopy:a practical guide[M].London: Royal Society of Chemistry,2004.
[10]
张毅,邬君飞,陈英颖.辉光放电原子发射光谱法快速分析生铸铁[J].理化检验:化学分册,2007,43(3):174-178.ZHANG Yi,WU Jun-fei,CHEN Ying-ying.Analysis of cast iron by glow-discharge atomic emission spectrometry[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2007,43(3):174-178.
[11]
余卫华,张穗忠,于录军.钢铁材料表面成分及其深度分布的射频辉光放电光谱研究[J].冶金分析,2008,28(7):11-17.YU Wei-hua,ZHANG Sui-zhong,YU Lu-jun.Study on surface composition and depth analysis of steel by radio frequency glow discharge optical emission spectrometry[J].Metallurgical Analysis,2008,28(7):11-17.
[12]
余兴,李小佳,王海舟.辉光光谱法同时测定高温合金中多种元素含量[J].钢铁研究学报,2006,18(5):55-59.YU Xing,LI Xiao-jia,WANG Hai-zhou.Simultaneous multielement determination for superalloy by glow discharge optical emission spectrometry[J].Journal of Iron and Steel Research,2006,18(5):55-59.
