普铝中Fe,Si元素的激光诱导击穿光谱测试条件及定量分析研究
Investigation on Experimental Conditions and Quantitative Analysis for Fe and Si Elements in General Aluminum by Laser Induced Breakdown Spectroscopy Technique
查看参考文献17篇
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文摘
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为推广LIBS技术在电解铝行业中的应用,充分发挥其快速、免制样、多元素同时检测的优势。利用激光诱导击穿光谱技术首次对铝电解生产得到的普铝中Fe和Si元素进行测试研究,探索了合理的实验参数条件,在合理的实验条件基础上建立定标曲线并对普铝中Fe和Si元素进行定量分析,结合国标GB/T 7999—2015《铝及铝合金光电直读发射光谱分析方法》考察LIBS测试结果的准确性。以Nd∶YAG脉冲激光器基频1 064nm激光作为光源激发等离子体,采用多通道光栅光谱仪和ICCD检测器检测、记录光谱信息。首先探测了LIBS光谱谱线,并对谱线进行了归属;综合分析,选取AlⅠ266.04nm,SiⅠ288.15nm与Fe Ⅰ259.92nm作为分析谱线用于定量分析研究。分别研究了触发延迟时间、1Q延迟时间、激光器设定电压对光谱信号强度及信噪比SNR的影响。实验结果表明,触发延迟时间4μs、1Q延迟时间170~190μs、激光器设定电压560V对于Si与Fe元素定量测试分析而言是较为合理的实验参数。根据谱线强度与元素浓度的关系,采用内标法建立了定标曲线,Si与Fe元素定标曲线中相关系数分别为0.919 72与0.952 11,其相对标准偏差(RSD)分别为7.25%与6.34%,说明谱线强度与元素浓度具有良好的线性关系,并基于此模型对12个样品进行了定量测试分析。将测试结果与光电直读发射光谱测得的结果进行比对,结果表明,Fe含量的相对误差绝对值在0~17.3%之间,Si含量相对误差绝对值在0~14.3%之间。依照国标GB/T 7999— 2015《铝及铝合金光电直读发射光谱分析方法》中规定的实验室之间分析结果相对误差≤17%的规定,12个测试样品中,试样Si含量测试100%符合允许差要求,试样Fe含量测试91.7%符合允许差要求。该实验结果表明,LIBS技术在电解铝普铝Fe和Si元素检测中具有一定的推广利用价值。 |
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其他语种文摘
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In order to promote the application of LIBS technology in electrolytic aluminum industry,give full play to its advantages of rapidness,no preparation and multi-element simultaneous detection.The contents of Fe and Si elements in general aluminium procuced from electrolysis process were detected by means of laser induced breakdown for the first time,and the reasonable experimental conditions were explored,the calibration curves were established and the content of Fe and Si in general aluminium were quantitatively analyzed based on reasonable experimental conditions.The accuracy of LIBS measurement results were examined according to national standard GB/T 7999—2015“optical emission spectrometric analysis method of aluminum and aluminum alloy”.The fundamental frequency 1 064 nm laser produced by Nd∶YAG pulsed laser device as the excitation source producing plasma,the spectral informations were detected and recorded by multi-channel grating spectrometer and ICCD detector. First of all,LIBS spectral line was detected and the spectral line was assigned,the line of AlⅠ266.04 nm,SiⅠ288.15 nm and FeⅠ259.92 nm were selected for quantitative analysis through comprehensive consideration.The influence of trigger delay time,1Qdelay time,laser setting voltage on the spectral signal intensity and SNR were researched respectively in the paper. The experimental results show that the trigger delay time of 4μs,1Qdelay time of 170~190μs,the laser set voltage of 560Vare the reasonable experimental parameters for Si and Fe element quantitative analysis in this paper.According to the relationship between spectral intensity and elemental concentration,the calibration curves were cestablished by the internal standard method.The correlation coefficients were 0.952 11 and 0.919 72,and the relative standard deviation were 6.34%and 7.25% for Fe and Si elements respectively.There was a good linear relationship between concentration and spectral intensity,and the 12 samples were quantitatively analyzed base on the above model.The relative error of Fe content is 0~17.3%and the relative error of Si content is 0~14.3%compared with the results obtained by OES.The measurement results 100%comply with the allowable requirements for Si content in 12samples,and the results 91.7% meet the allowable difference requirements according to national atandard GB/T 7999—2015“optical emission spectrometric analysis method of aluminum and aluminum alloy”.The experimental results show that,LIBS technology has a certain value of promotion and using in the electrolytic aluminum industry for Fe and Si elements detection. |
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来源
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光谱学与光谱分析
,2019,39(4):1267-1273 【核心库】
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DOI
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10.3964/j.issn.1000-0593(2019)04-1267-07
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关键词
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激光诱导击穿光谱
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铝电解
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普铝
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Fe和Si元素
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定量分析
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地址
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1.
北京科技大学, 钢铁冶金新技术国家重点实验室, 北京, 100083
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国家铝镁电解装备工程技术研究中心, 国家铝镁电解装备工程技术研究中心, 贵州, 贵阳, 550081
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中国科学院沈阳自动化研究所, 辽宁, 沈阳, 110016
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语种
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中文 |
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文献类型
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研究性论文 |
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ISSN
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1000-0593 |
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学科
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物理学;化学 |
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基金
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国家863计划
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国家国际合作计划项目
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中铝公司明星计划项目
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国家重点研发计划项目
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文献收藏号
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CSCD:6479276
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