火花放电原子发射光谱仪分析高含量硅时校准曲线的扩展与应用
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摘要
火花放电原子发射光谱仪分析高含量Si(w(Si)≥3.0%)时,其元素含量已超出了校准曲线的线性范围,导致分析值偏低。实验通过增加中低合金钢、硅钢标准样品,完善并扩展了Si校准曲线,完成了共存元素的干扰校正,拓宽了Si元素的分析范围,质量分数上限由3.14%扩展至4.16%,线性相关系数达0.99965。校准曲线扩展后重新选择标准化样品进行漂移校正,校准曲线强度比由9.41扩展至11.01。对扩展含量段的两个样品(w(Si)≥3.0%)进行精密度考察,结果的相对标准偏差(RSD,n=10)为0.43%和0.50%;对比了8个不同Si含量的样品,发现完善、扩展后校准曲线的Si测定值与认定值更相符;同时统计过程控制(SPC)控制图处于受控状态。可见校准曲线经完善、扩展后可满足工艺过程控制和成品分析要求。
During the analysis of high content silicon[w(Si)≥3.0%]by spark discharge atomic emission spectrometer,the elemental content was beyond the linear range of calibration curve,leading to the lower determination results.The standard samples of middle-low alloy steel and silicon steel were added in experiments to improve and expand the calibration curve of silicon.The interference of coexisting elements was corrected.The analysis range of silicon was broadened.The upper limit of mass fraction increased from 3.14%to 4.16%,and the linear correlation coefficient was up to 0.999 65.After extension of calibration curve,the standardization sample was reselected for the drift correction.The intensity ratio of calibration curve was expanded from 9.41 to 11.01.Two samples with expanded silicon content[w(Si)≥3.0%]were used for precision test.The relative standard deviation(RSD,n=10)was 0.43% and 0.50%,respectively.Eight samples with different silicon contents were compared.It was found that the determination results by expanded calibration curves were more consistent with the certified values.Meanwhile,the statistical process control(SPC)chart was within the controlled state.Therefore,the modified and expanded calibration curve could meet the process control and analysis requirements of products.
During the analysis of high content silicon[w(Si)≥3.0%]by spark discharge atomic emission spectrometer,the elemental content was beyond the linear range of calibration curve,leading to the lower determination results.The standard samples of middle-low alloy steel and silicon steel were added in experiments to improve and expand the calibration curve of silicon.The interference of coexisting elements was corrected.The analysis range of silicon was broadened.The upper limit of mass fraction increased from 3.14%to 4.16%,and the linear correlation coefficient was up to 0.999 65.After extension of calibration curve,the standardization sample was reselected for the drift correction.The intensity ratio of calibration curve was expanded from 9.41 to 11.01.Two samples with expanded silicon content[w(Si)≥3.0%]were used for precision test.The relative standard deviation(RSD,n=10)was 0.43% and 0.50%,respectively.Eight samples with different silicon contents were compared.It was found that the determination results by expanded calibration curves were more consistent with the certified values.Meanwhile,the statistical process control(SPC)chart was within the controlled state.Therefore,the modified and expanded calibration curve could meet the process control and analysis requirements of products.
引文
[1]陈卓.中国电工钢生产现状及后期展望[J].中国冶金,2010,20(8):15-23.CHEN Zhuo.Current situation of electrical steel production in China and its prospect[J].China Metallurgy,2010,20(8):15-23.
[2]赵雷,屈华阳,杨敬巍,等.火花源原子发射光谱技术进展与应用[C]∥第十六届冶金及材料分析测试学术报告会论文集.北京:中国金属学会,2012:525-545.
[3]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,phosphorrrrous and sulfur in oriented silicon steel by spark source atomic emission spectrometry[J].Metallurgical Analysis,2012,32(10):19-23.
[4]廖义兵,黄荣青,傅韬,等.硅钢中碳和硅的火花源原子发射光谱分析[C]∥第十二届分析测试学术年会论文集.北京:中国金属学会,2004:45-47.
[5]王辉,刘佳,李剑,等.火花光谱分析中第三元素干扰的校正[C]∥第十六届冶金及材料分析测试学术报告会论文集.北京:中国金属学会,2012:562-565.
[6]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):1-6.CAO Xin-quan,LI Hua,DENG Jun-hua.Determination of silicon,managanese,phosphorus,sulfur and aluminum in silicon steel by spark source atomic emission spectrometer[J].Heilongjiang Metallurgy,2014,34(6):1-6.
[7]陈英,张增坤,王义敏.火花源光谱法的相关性及其应用[J].冶金分析,2002,22(3):61-63.CHEN Ying,ZHANG Zeng-kun,WANG Yi-min.Correlation of spark source spectrometry and its application[J].Metallurgical Analysis,2002,22(3):61-63.
[8]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 4336—2016碳素钢和中低合金钢多元素含量的测定火花放电原子发射光谱法(常规法)[S].北京:中国标准出版社,2016.
[9]孙晓飞,沈克,文孟喜,等.制定碳素钢火花放电原子发射光谱标准的精密度研究[J].冶金分析,2017,37(10):1-9.SUN Xiao-fei,SHEN Ke,WEN Meng-xi,et al.Study on the precision of spark discharge atomic emission spectrometry standard for carbon steel[J].Metallurgical Analysis,2017,37(10):1-9.
[10]畅小军,毕经亮,刘颂,等.控制图在火花源原子发射光谱仪期间核查中的应用[J].冶金分析,2015,35(12):77-81.CHANG Xiao-jun,BI Jing-liang,LIU Song,et al.Application of control chart in intermediate check of spark source atomic emission spectrometer[J].Metallurgical Analysis,2015,35(12):77-81.
[2]赵雷,屈华阳,杨敬巍,等.火花源原子发射光谱技术进展与应用[C]∥第十六届冶金及材料分析测试学术报告会论文集.北京:中国金属学会,2012:525-545.
[3]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,phosphorrrrous and sulfur in oriented silicon steel by spark source atomic emission spectrometry[J].Metallurgical Analysis,2012,32(10):19-23.
[4]廖义兵,黄荣青,傅韬,等.硅钢中碳和硅的火花源原子发射光谱分析[C]∥第十二届分析测试学术年会论文集.北京:中国金属学会,2004:45-47.
[5]王辉,刘佳,李剑,等.火花光谱分析中第三元素干扰的校正[C]∥第十六届冶金及材料分析测试学术报告会论文集.北京:中国金属学会,2012:562-565.
[6]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):1-6.CAO Xin-quan,LI Hua,DENG Jun-hua.Determination of silicon,managanese,phosphorus,sulfur and aluminum in silicon steel by spark source atomic emission spectrometer[J].Heilongjiang Metallurgy,2014,34(6):1-6.
[7]陈英,张增坤,王义敏.火花源光谱法的相关性及其应用[J].冶金分析,2002,22(3):61-63.CHEN Ying,ZHANG Zeng-kun,WANG Yi-min.Correlation of spark source spectrometry and its application[J].Metallurgical Analysis,2002,22(3):61-63.
[8]中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 4336—2016碳素钢和中低合金钢多元素含量的测定火花放电原子发射光谱法(常规法)[S].北京:中国标准出版社,2016.
[9]孙晓飞,沈克,文孟喜,等.制定碳素钢火花放电原子发射光谱标准的精密度研究[J].冶金分析,2017,37(10):1-9.SUN Xiao-fei,SHEN Ke,WEN Meng-xi,et al.Study on the precision of spark discharge atomic emission spectrometry standard for carbon steel[J].Metallurgical Analysis,2017,37(10):1-9.
[10]畅小军,毕经亮,刘颂,等.控制图在火花源原子发射光谱仪期间核查中的应用[J].冶金分析,2015,35(12):77-81.CHANG Xiao-jun,BI Jing-liang,LIU Song,et al.Application of control chart in intermediate check of spark source atomic emission spectrometer[J].Metallurgical Analysis,2015,35(12):77-81.