火花放电原子发射光谱法分析硅钢中硅和铝元素的影响因素探讨
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摘要
在硅钢冶炼中,硅和铝元素成分的精准控制是提高硅钢冶炼质量的重要保证。实验就火花放电原子发射光谱法分析硅钢中硅和铝元素的影响因素进行了探讨,研究了铣床制样参数、电极清洁次数、光谱分析程序、液氩使用管路、仪器使用状态、样品分析过程和光谱仪使用透镜等影响因素。结果发现:铣床制样参数、光谱仪两种分析程序和使用透镜情况对硅和铝元素的影响不显著,但电极清洁次数、液氩使用管路、仪器使用状态、样品分析过程对硅和铝元素的精密度和正确度都有显著影响。因此,在进行硅钢样品分析时,要保证电极清洁彻底、液氩管路两级净化、样品室温,仪器在长时间不分析样品时,开始使用前要预分析样品约30min后再进行使用。通过控制硅钢样品分析过程中的影响因素,可以提高样品分析的精密度和正确度,从而提高生产效率,控制产品质量。
In silicon steel smelting process,the accurate control of silicon and aluminum contents in silicon steel is important to guarantee the smelting quality.The influence factors in spark discharge atomic emission spectrometric determination of silicon and aluminum in silicon steel were discussed,including the sample preparation parameters of milling machine,the cleaning times of electrode,the spectral analysis procedures,the using pipeline of liquid argon,the using state of instrument,the sample analysis process and the lens used in spectrometer.The results showed that the sample preparation parameters of milling machine,two analysis procedures of spectrometer and the lens used had little influence on the determination of silicon and aluminum.However,the determination precision and trueness of silicon and aluminum were greatly affected by the cleaning times of electrode,the using pipeline of liquid argon,the using state of instrument and the sample analysis process.Therefore,during the analysis of silicon steel sample,the cleaning of electrode should be thorough,the pipeline of liquid argon should have two-stage purification,and the sample was determined at room temperature.If the instrument was not used for long time,the pre-analysis for about 30 min should be conducted before use.By controlling the influencing factors in analysis of silicon steel sample,the determination precision and trueness could be improved,thus enhancing the production efficiency and controlling the product quality.
In silicon steel smelting process,the accurate control of silicon and aluminum contents in silicon steel is important to guarantee the smelting quality.The influence factors in spark discharge atomic emission spectrometric determination of silicon and aluminum in silicon steel were discussed,including the sample preparation parameters of milling machine,the cleaning times of electrode,the spectral analysis procedures,the using pipeline of liquid argon,the using state of instrument,the sample analysis process and the lens used in spectrometer.The results showed that the sample preparation parameters of milling machine,two analysis procedures of spectrometer and the lens used had little influence on the determination of silicon and aluminum.However,the determination precision and trueness of silicon and aluminum were greatly affected by the cleaning times of electrode,the using pipeline of liquid argon,the using state of instrument and the sample analysis process.Therefore,during the analysis of silicon steel sample,the cleaning of electrode should be thorough,the pipeline of liquid argon should have two-stage purification,and the sample was determined at room temperature.If the instrument was not used for long time,the pre-analysis for about 30 min should be conducted before use.By controlling the influencing factors in analysis of silicon steel sample,the determination precision and trueness could be improved,thus enhancing the production efficiency and controlling the product quality.
引文
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[3]朱诚意,陈先红,李光强.高品质取向硅钢成分控制的新进展及其对钢磁性能的影响[J].材料导报,2015,29(1):6-14.ZHU Cheng-yi,CHEN Xian-hong,LI Guang-qiang.New progress in composition control of high quality oriented silicon steel and its influence on magnetic properties of steel[J].Materials Review,2015,29(1):6-14.
[4]孙晓天,王玲,张振禹,等.ICP-AES法测定高硅钢中的硅[J].当代化工,2007,36(6):663-664,668.SUN Xiao-tian,WANG Ling,ZHANG Zhen-yu,et al.Determination of silicon in highly silicon steel by ICPAES[J].Contemporary Chemical Industry,2007,36(6):663-664,668.
[5]邓军华,曹新全,李化.直流辉光放电发射光谱法测定电工钢中多元素含量[J].化学分析计量,2010,19(6):39-41.DENG Jun-hua,CAO Xin-quan,LI Hua.Dtermination of multiple elements in electrical steel by direct current glow discharge emission spectrometry[J].Chemical Analysis and Meterage,2010,19(6):39-41.
[6]邓军华.辉光放电发射光谱法测定电工钢中8种元素[J].鞍钢技术,2011(1):39-41.DENG Jun-hua.Determination of eight elements in electrical steel by glow discharge emission spectrometry[J].AnGang Techniques,2011(1):39-41.
[7]邓军华,邴一宏.直流辉光放电发射光谱法同时测定硅钢中11种元素[J].冶金分析,2010,30(1):24-28.DENG Jun-hua,BING Yi-hong.Simultaneous determination of eleven elements in silicone steel by direct-reading glow discharge emission spectrometry[J].Metallurgical Analysis,2010,30(1):24-28.
[8]徐永林,梁潇,张东生.火花源原子发射光谱法测定取向硅钢中碳硅锰磷硫[J].冶金分析,2013,33(10):19-23.XU Yong-lin,LIANG Xiao,ZHANG Dong-sheng.Determination of carbon,silicon manganese,phosphorus,sulfur in oriented silicon steel by spark source atomic emission spectrometry[J].Metallurgical Analysis,2013,33(10):19-23.
[9]曹新全,李化,邓军华.火花源原子发射光谱法测定硅钢中硅锰磷硫铝[J].黑龙江冶金,2014,34(6):1-3,6.CAO Xin-quan,LI Hua,DENG Jun-hua.Determination of silicon,manganese,phosphorus,sulphur,aluminum in silicon steel by atomic emission spectrometry[J].Heilongjiang Metallurgy,2014,34(6):1-3,6.
[10]张嵬巍,郭少毅,张娅红,等.光电直读光谱仪测定硅钢中的氮[J].云南冶金,2012,41(1):56-58.ZHANG Wei-wei,GUO Shao-yi,ZHANG Ya-hong,et al.Determination of nitrogen in silicon steel by photoelectric direct reading spectrometer[J].Yunnan Metallurgy,2012,41(1):56-58.
[11]李杰,李洁,张穗忠,等.电感耦合等离子体质谱法测定硅钢中的痕量铝钼钒钛铌[J].冶金分析,2013,33(1):22-26.LI Jie,LI Jie,ZHANG Sui-zhong,et al.Determination of trace aluminum,molybdenum,vanadium,titanium and niobium in silicon steel by inductively coupled plasma mass spectrometry[J].Metallurgical Analysis,2013,33(1):22-26.