手持式激光诱导击穿光谱仪对铝合金中镁钛元素的定量分析
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摘要
在常温常压下,采用手持式激光诱导击穿光谱仪(LIBS)对铝合金中的镁、钛元素进行定量分析,以验证其稳定性及可靠性。手持式LIBS内置1064nm Nd…YAG脉冲激光器,光路为反射式同轴结构。实验中采用AvaSpec-Mini 2048光谱仪,测量波长范围为240～420nm。选取镁元素在285.17、383.83nm处的特征谱线,钛元素在323.45、334.94nm处的特征谱线,结合偏最小二乘法建立定标曲线模型。同种元素在不同特征谱线下的定标曲线斜率接近,线性相关系数R值均在0.9893及以上。测量结果与标准值具有较好的一致性,测量值相对误差均在8.70%及以下,样品中镁、钛元素检出限可达到10-4量级。说明手持式LIBS能够实现对铝合金中镁、钛元素的定量分析,从而验证了手持式LIBS具有较好的稳定性和可靠性,对LIBS便携化的发展具有十分重要的意义。
Under normal temperature and pressure,the quantitative analysis of magnesium and titanium elements in aluminum alloy is carried out by handheld laser-induced breakdown spectroscopy(LIBS)to verify the instrument′s stability and reliability.The handheld LIBS has a built-in 1064 nm Nd:YAG pulsed laser with a reflective coaxial structure.The AvaSpec-Mini 2048 spectrometer with a measurement wavelength range of 240-420 nm is used in the experiment.The characteristic lines of magnesium element at 285.17 nm and 383.83 nm and those of titanium element at 323.45 nm and 334.94 nm are selected.Then the calibration curve model is established with the partial least square method.The slopes of calibration curves for the same element under different characteristic lines are close to each other,and the values of linear correlation coefficients R are all above 0.9893.Moreover,the measurement results have good consistency with the standard values,and the relative error is no more than 8.70%.The detection limits of magnesium and titanium elements in the samples can reach the level of 10-4.The handheld LIBS can be used to realize the quantitative analysis of magnesium and titanium elements in aluminum alloys and thus that the handheld LIBS has certain stable and reliable performances is verified,which is of great significance to the development of a portable LIBS.
Under normal temperature and pressure,the quantitative analysis of magnesium and titanium elements in aluminum alloy is carried out by handheld laser-induced breakdown spectroscopy(LIBS)to verify the instrument′s stability and reliability.The handheld LIBS has a built-in 1064 nm Nd:YAG pulsed laser with a reflective coaxial structure.The AvaSpec-Mini 2048 spectrometer with a measurement wavelength range of 240-420 nm is used in the experiment.The characteristic lines of magnesium element at 285.17 nm and 383.83 nm and those of titanium element at 323.45 nm and 334.94 nm are selected.Then the calibration curve model is established with the partial least square method.The slopes of calibration curves for the same element under different characteristic lines are close to each other,and the values of linear correlation coefficients R are all above 0.9893.Moreover,the measurement results have good consistency with the standard values,and the relative error is no more than 8.70%.The detection limits of magnesium and titanium elements in the samples can reach the level of 10-4.The handheld LIBS can be used to realize the quantitative analysis of magnesium and titanium elements in aluminum alloys and thus that the handheld LIBS has certain stable and reliable performances is verified,which is of great significance to the development of a portable LIBS.
引文
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[13]Ren H,Sun J X.Analysis of the uncertainty for the determination of zinc in aluminium alloy by AAS[J].Modern Scientific Instruments,2013(1):155-157.任慧,孙建新.原子吸收光谱法测定铝合金中锌含量测量结果的不确定度评定[J].现代科学仪器,2013(1):155-157.
[14]Cai Z L,Yang Q S,Wang Y.Femtosecond laserinduced breakdown spectral analysis of Cu-al alloy sputtered thin films[J].Chinese Journal of Lasers,2015,42(6):0615001.蔡志龙,杨秋松,王阳.铜铝合金溅射薄膜的飞秒激光诱导击穿光谱分析[J].中国激光,2015,42(6):0615001.
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[16]Wallis F J,Chadwick B L,Morrison R J S.Analysis of lignite using laser-induced breakdown spectroscopy[J].Applied Spectroscopy,2000,54(8):1231-1235.
[2]Xu Y,Yao M Y,Liu M H,et al.Laser induced breakdown spectroscopy of chromium in water solution[J].Acta Optica Sinica,2011,31(12):1230002.徐媛,姚明印,刘木华,等.水溶液中铬元素的激光诱导击穿光谱研究[J].光学学报,2011,31(12):1230002.
[3]Wang C H,Huang L,Chen T B,et al.Feasibility of analyzing Cr in rice husk and coarse rice with LIBS[J].Spectroscopy and Spectral Analysis,2017,37(11):3590-3593.王彩虹,黄林,陈添兵,等.水田污染区稻壳与糙米中铬元素的LIBS分析可行性[J].光谱学与光谱分析,2017,37(11):3590-3593.
[4]Xu H G,Guan S C,Fu Y X,et al.Laser induced breakdown spectroscopy of the trace metal element Pb in soil[J].Chinese Journal of Lasers,2007,34(4):577-581.许洪光,管士成,傅院霞,等.土壤中微量重金属元素Pb的激光诱导击穿谱[J].中国激光,2007,34(4):577-581.
[5]Chen L,Deng G L,Feng G Y,et al.Study on the mechanism of laser paint removal based on LIBS and time resolved characteristic signal[J].Spectroscopy and Spectral Analysis,2018,38(2):367-371.陈林,邓国亮,冯国英,等.基于LIBS及时间分辨特征峰的激光除漆机理研究[J].光谱学与光谱分析,2018,38(2):367-371.
[6]Dong L L,Xiu J S,Li J Y,et al.Feasibility analysis of metal elements in drilling fluid based on laser induced breakdown spectroscopy[J].Laser&Optoelectronics Progress,2018,55(3):033001.董丽丽,修俊山,李季远,等.基于LIBS技术分析钻井液中金属元素的可行性[J].激光与光电子学进展,2018,55(3):033001.
[7]Dong M R,Lu J D,Yao S C,et al.Quantitative analysis of carbon content in coal with multivariate calibration by LIBS[J].Journal of Engineering Thermophysics,2012,33(1):175-179.董美蓉,陆继东,姚顺春,等.基于多元定标法的煤粉碳元素LIBS定量分析[J].工程热物理学报,2012,33(1):175-179.
[8]Nan W G,Yoshihiro D,Wang H R,et al.Reduction of CO2effect on unburned carbon measurement in fly ash using LIBS[J].Spectroscopy and Spectral Analysis,2018,38(1):258-262.南维刚,出口祥啓,王焕然,等.减少二氧化碳对LIBS检测飞灰中未燃碳含量影响的研究[J].光谱学与光谱分析,2018,38(1):258-262.
[9]Yamamoto K Y,Cremers D A,Ferris M J,et al.Detection of metals in the environment using a portable laser-induced breakdown spectroscopy instrument[J].Applied Spectroscopy,1996,50(2):222-233.
[10]Duan Y X,Lin Q Y,Wang J,et al.Portable elementary composition analysis device based on laserinduced breakdown spectroscopy technology:CN104007090[P].2014-05-27.段忆翔,林庆宇,王杰,等.基于激光诱导击穿光谱技术的便携式元素成分分析装置:CN104007090[P].2014-05-27.
[11]Luo Y X.Determination of trace Gd,La,Nd,Pr and Sm in aluminum alloy by ICP-OES[J].Chinese Journal of Inorganic Analytical Chemistry,2017,7(2):50-54.罗有雄.电感耦合等离子体发射光谱(ICP-OES)法测定铝合金中微量的钆、镧、钕、镨、钐[J].中国无机分析化学,2017,7(2):50-54.
[12]Tian L F,Zou D S,Dai Y C,et al.Determination of multi-element in aluminum-lithium alloy by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2014,34(10):52-56.田伦富,邹德霜,代以春,等.X射线荧光光谱法测定铝锂合金中多元素含量[J].冶金分析,2014,34(10):52-56.
[13]Ren H,Sun J X.Analysis of the uncertainty for the determination of zinc in aluminium alloy by AAS[J].Modern Scientific Instruments,2013(1):155-157.任慧,孙建新.原子吸收光谱法测定铝合金中锌含量测量结果的不确定度评定[J].现代科学仪器,2013(1):155-157.
[14]Cai Z L,Yang Q S,Wang Y.Femtosecond laserinduced breakdown spectral analysis of Cu-al alloy sputtered thin films[J].Chinese Journal of Lasers,2015,42(6):0615001.蔡志龙,杨秋松,王阳.铜铝合金溅射薄膜的飞秒激光诱导击穿光谱分析[J].中国激光,2015,42(6):0615001.
[15]Chen G F,Chen K,Zeng A J,et al.Reflection type coaxial structure laser-induced breakdown spectroscopy analysis device:CN106596511A[P].2016-12-27.陈国飞,陈宽,曾爱军,等.一种反射式同轴结构激光诱导击穿光谱分析装置:CN106596511A[P].2016-12-27.
[16]Wallis F J,Chadwick B L,Morrison R J S.Analysis of lignite using laser-induced breakdown spectroscopy[J].Applied Spectroscopy,2000,54(8):1231-1235.