手持式激光诱导击穿光谱仪现场测定钢铁制品中铬镍锰铜硅
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摘要
钢铁中各元素组成及含量对钢种质量和性能都有重要影响,实时、快速对钢铁中各元素进行有效检测分析是目前钢铁行业的关注重点。实验探讨了手持式激光诱导击穿光谱(LIBS)技术在钢铁中多元素同步、快速分析方面的可行性:选取3个钢铁标准样品,以Cr(I)520.84nm、Ni(I)232.003nm、Mn(I)403.075nm、Cu(I)324.753nm、Si(I)288.16nm作为分析谱线,以Fe(I)373.486nm作为内标谱线,考察了手持式LIBS分析仪对钢铁标准样品分析的精密度和正确度。标样验证试验结果表明,手持式LIBS分析仪快速定量分析Cr、Ni、Cu及Si 4种元素的准确性较高,对于Mn的定量分析存在一定的系统偏差,但也基本能反映元素含量。随机选取不同种类的钢铁材料日常实际样品,采用实验方法进行快速定量分析,同时以电感耦合等离子体原子发射光谱(ICP-AES)进行对照,绘制两种方法测定结果的线性趋势图,并与理想趋势线(y=x)进行对比。结果表明,Cr、Ni、Cu及Si 4种元素的LIBS与ICP-AES测试结果表现较一致,Mn的测试结果普遍较ICP-AES偏低,但二者存在较好的相关性。在整个试验过程中,手持式LIBS分析仪测试一组数据的时间平均为5s,该技术用于钢铁行业快速定量分析是可行的。
The composition and content of elements in steel had important influence on the quality and performance of steels.At present,the real-time and rapid determination of elements in steel were focused in steel industry.The feasibility of simultaneous and rapid analysis of multi-elements in steel using handheld laser induced breakdown spectrometer(LIBS)was discussed.Three standard steel samples were tested.Cr(I)520.84 nm,Ni(I)232.003 nm,Mn(I)403.075 nm,Cu(I)324.753 nm and Si(I)288.16 nm were selected as the analytical lines.Fe(I)373.486 nm was used as the internal standard line.The precision and trueness of sample analysis of standard steel samples using hand-held LIBS were investigated.The verification test results showed that the accuracy was relatively high when hand-held LIBS was used for the rapid and quantitative analysis of four elements including Cr,Ni,Cu and Si.Although the quantitative analysis of Mn had certain system deviation,the results could basically reflect the elemental content.Some actual samples of various steel materials in daily life were randomly selected for rapid and quantitative analysis according to the experimental method.Meanwhile,the inductively coupled plasma atomic emission spectrometry(ICP-AES)method was employed for comparison.The linear trend diagrams of determined results by two methods were plotted and compared with the ideal trend line(y=x).The results indicated that the determination results of Cr,Ni,Cu and Si by LIBS were consistent with those obtained by ICPAES.The results of Mn by LIBS were lower than those obtained by ICP-AES,but they showed good correlation relationship.In whole test process,the average analysis time for one set of data by hand-held LIBS was 5 s.The proposed method was feasible for the rapid and quantitative analysis in steel industry.
The composition and content of elements in steel had important influence on the quality and performance of steels.At present,the real-time and rapid determination of elements in steel were focused in steel industry.The feasibility of simultaneous and rapid analysis of multi-elements in steel using handheld laser induced breakdown spectrometer(LIBS)was discussed.Three standard steel samples were tested.Cr(I)520.84 nm,Ni(I)232.003 nm,Mn(I)403.075 nm,Cu(I)324.753 nm and Si(I)288.16 nm were selected as the analytical lines.Fe(I)373.486 nm was used as the internal standard line.The precision and trueness of sample analysis of standard steel samples using hand-held LIBS were investigated.The verification test results showed that the accuracy was relatively high when hand-held LIBS was used for the rapid and quantitative analysis of four elements including Cr,Ni,Cu and Si.Although the quantitative analysis of Mn had certain system deviation,the results could basically reflect the elemental content.Some actual samples of various steel materials in daily life were randomly selected for rapid and quantitative analysis according to the experimental method.Meanwhile,the inductively coupled plasma atomic emission spectrometry(ICP-AES)method was employed for comparison.The linear trend diagrams of determined results by two methods were plotted and compared with the ideal trend line(y=x).The results indicated that the determination results of Cr,Ni,Cu and Si by LIBS were consistent with those obtained by ICPAES.The results of Mn by LIBS were lower than those obtained by ICP-AES,but they showed good correlation relationship.In whole test process,the average analysis time for one set of data by hand-held LIBS was 5 s.The proposed method was feasible for the rapid and quantitative analysis in steel industry.
引文
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[8]沈桂华,李华昌,史烨弘.激光诱导击穿光谱发展现状[J].冶金分析,2016,36(5):16-25.SHEN Gui-hua,LI Hua-chang,SHI Ye-hong.Progress in laser induced breakdown spectroscopy[J].Metallurgical Analysis,2016,36(5):16-25.
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[10]马翠红,王汉炳.LIBS结合自由定标法对钢液中多元素成分定量分析[J].激光杂志,2017,38(11):38-41.MA Cui-hong,WANG Han-bing.Composition quantitative analysis of multiple elements in liquid steel based on LIBS combined with calibration-free method[J].Laser Journal,2017,38(11):38-41.
[2]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 and sulfur in oriented silicon steel by spark source atomic emission spectrometry[J]Metallurgical Analysis,2013,33(10):19-23.
[3]张志刚,李方军,蔡萍,等.X射线荧光光谱法测定不锈钢中15种元素[J].冶金分析,2009,29(7):19-23.ZHANG Zhi-gang,LI Fang-jun,CAI Ping,et al.Determination of fifteen elements in stainless steel by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2009,29(7):19-23.
[4]邓军华,曲月华,王一凌.X射线荧光光谱法快速测定钢基中锰元素[J].中国无机分析化学,2011,1(2):63-65.DENG Jun-hua,QU Yue-hua,WANG Yi-ling.Rapid quantitative determination of manganese element in steel by X-ray fluorescence spectrometry[J].Chinese Journal of Inorganic Analytical Chemistry,2011,1(2):63-65.
[5]杨新能,冯宗平,羊绍松,等.电感耦合等离子体原子发射光谱法测定钒铁合金中杂质元素[J].冶金分析,2014,34(11):37-41.YANG Xin-neng,FENG Zong-ping,YANG Shao-song,et al.Determination of impurity elements in ferrovanadium alloy by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(11):37-41.
[6]杨丽荣,于媛君,亢德华,等.电感耦合等离子体原子发射光谱法测定钢中铌钨锆[J].冶金分析,2014,34(11):51-55.YANG Li-rong,YU Yuan-jun,KANG De-hua,et al.Determination of niobium,tungsten and zirconium in steel by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2014,34(11):51-55.
[7]邵妍,张艳波,高勋,等.激光诱导击穿光谱技术的研究与应用新进展[J].光谱学与光谱分析,2013,33(10):2593-2598.SHAO Yan,ZHANG Yan-bo,GAO Xun,et al.Latest research on and applications progress in laser-induced breakdown spectroscopy[J].Spectroscopy and Spectral Analysis,2013,33(10):2593-2598.
[8]沈桂华,李华昌,史烨弘.激光诱导击穿光谱发展现状[J].冶金分析,2016,36(5):16-25.SHEN Gui-hua,LI Hua-chang,SHI Ye-hong.Progress in laser induced breakdown spectroscopy[J].Metallurgical Analysis,2016,36(5):16-25.
[9]孙兰香,于海斌,丛智博,等.激光诱导击穿光谱技术结合神经网络定量分析钢中的Mn和Si[J].光学学报,2010(9):2757-2765.SUN Lan-xiang,YU Hai-bin,CONG Zhi-bo,et al.Quantitative analysis of Mn and Si of steels by laser-induced breakdown spectroscopy combined with neural networks[J].Acta Optica Sinica,2010(9):2757-2765.
[10]马翠红,王汉炳.LIBS结合自由定标法对钢液中多元素成分定量分析[J].激光杂志,2017,38(11):38-41.MA Cui-hong,WANG Han-bing.Composition quantitative analysis of multiple elements in liquid steel based on LIBS combined with calibration-free method[J].Laser Journal,2017,38(11):38-41.