光电直读光谱法测定钛合金中13种元素
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摘要
采用OBLF QSN750型光电直读光谱仪测定钛合金中13种元素(即Al、V、Mo、Sn、Zr、Fe、Si、Cu、Cr、Mn、Ni、W、Nb),文中对仪器工作条件作了介绍。通过曲线的平移或转动对分析线的光谱干扰作出校正,对分析的钛合金样品的大小和形态具体规定如下:(1)铸造样品外径≥40mm,厚度≥310mm;(2)切割加工的样品(棒状)直径≥10mm,长度约40mm;(板状)厚度≥0.5mm,面积≥30mm×30mm;(块状)厚度≥5mm,面积≥30mm×30mm,以上各种形状的样品可采用切削和磨制将其加工出一个合适的分析平面。采用48块钛合金标准样品建立了测定元素的校准曲线,其中Al、V、Mo、Sn、Zr、Cu(324.75nm)及Cr的曲线采用分段拟合,以得到更好的相关系数。另取2块钛合金标准样品,按所提出方法测定以验证其精密度,结果表明:13个元素测定值的相对标准偏差(n=11)在0.34%～5.8%之间。5个不同牌号的钛合金样品的分析结果与电感耦合等离子体原子发射光谱法和化学法的分析结果相符。
OBLF QSN750 Photoelectric direct-reading spectrometer was used in the determination of 13elements(i.e.,Al,V,Mo,Sn,Zr,Fe,Si,Cu,Cr,Mn,Ni,W,Nb)in titanium alloys,and working conditions of the instrument were reported in detail.Correction of spectral interferences with the analytical spectral lines was made by translational or rotational moving of the curves.Size and shape of the solid samples required for the analysis were stipulated as follows:(1)for casting samples:oulter diameter≥40mm,thickness≥ 10mm;(2)for cutting samples:(in stick form)diameter ≥10 mm,length ca.40 mm;(in plate form)thickness ≥0.5 mm,area≥30mm×30mm;(in lump form)thickness≥ 5mm,area≥ 30mm×30mm.All the solid samples in various shapes should be processed by cutting or grinding to give a suitable,plain surface for analysis.Calibration curves of the 13 elements were prepared by using 48 standard samples of titanium alloys and the calibration curves of 7elements(i.e.,Al,V,Mo,Sn,Zr,Cu 324.75 nm and Cr)were prepared by the method of segmented fitting in order to obtain better correlation coefficients.Two standard samples of titanium alloy were analyzed in parallel by the proposed method to test its precision,values of RSDs(n=11)found for the 13 elements were in the range of 0.34% to 5.8%.Five samples of titanium alloys of various models were analyzed by the proposed method,giving determined values in consistency with those found by ICP-AES and chemical method.
OBLF QSN750 Photoelectric direct-reading spectrometer was used in the determination of 13elements(i.e.,Al,V,Mo,Sn,Zr,Fe,Si,Cu,Cr,Mn,Ni,W,Nb)in titanium alloys,and working conditions of the instrument were reported in detail.Correction of spectral interferences with the analytical spectral lines was made by translational or rotational moving of the curves.Size and shape of the solid samples required for the analysis were stipulated as follows:(1)for casting samples:oulter diameter≥40mm,thickness≥ 10mm;(2)for cutting samples:(in stick form)diameter ≥10 mm,length ca.40 mm;(in plate form)thickness ≥0.5 mm,area≥30mm×30mm;(in lump form)thickness≥ 5mm,area≥ 30mm×30mm.All the solid samples in various shapes should be processed by cutting or grinding to give a suitable,plain surface for analysis.Calibration curves of the 13 elements were prepared by using 48 standard samples of titanium alloys and the calibration curves of 7elements(i.e.,Al,V,Mo,Sn,Zr,Cu 324.75 nm and Cr)were prepared by the method of segmented fitting in order to obtain better correlation coefficients.Two standard samples of titanium alloy were analyzed in parallel by the proposed method to test its precision,values of RSDs(n=11)found for the 13 elements were in the range of 0.34% to 5.8%.Five samples of titanium alloys of various models were analyzed by the proposed method,giving determined values in consistency with those found by ICP-AES and chemical method.
引文
[1]张喜燕,赵永庆,白晨光.钛合金及应用[M].北京:化学工业出版社,2005.
[2]邓炬.正在崛起的中国钛工业[J].稀有金属快报,2007,26(6):1-6.
[3]蔡建明,曹春晓.新一代600℃高温钛合金材料的合金设计及应用展望[J].航空材料学报,2014,34(4):27-36.
[4]周廉.美国、日本和中国钛工业发展评述[J].稀有金属材料与工程,2003,32(8):577-584.
[5]GB/T 3620.1-2016钛及钛合金牌号和化学成分[S].
[6]GB/T 4698-1996海绵钛、钛及钛合金化学分析方法[S].
[7]黄永光.我国钛及钛合金牌号的发展和标准化[J].稀有金属快报,2008,27(4):7-10.
[8]黄永光.我国钛及钛合金标准现状思考[J].标准科学,2004(6):32-34.
[9]黄永光,庞洪,李宝霞.中国钛材行业的新标准[J].亚洲钛业咨询,2006(4):17-20.
[10]徐秋心.实用发射光谱分析[M].成都:四川科学技术出版社,1992.
[2]邓炬.正在崛起的中国钛工业[J].稀有金属快报,2007,26(6):1-6.
[3]蔡建明,曹春晓.新一代600℃高温钛合金材料的合金设计及应用展望[J].航空材料学报,2014,34(4):27-36.
[4]周廉.美国、日本和中国钛工业发展评述[J].稀有金属材料与工程,2003,32(8):577-584.
[5]GB/T 3620.1-2016钛及钛合金牌号和化学成分[S].
[6]GB/T 4698-1996海绵钛、钛及钛合金化学分析方法[S].
[7]黄永光.我国钛及钛合金牌号的发展和标准化[J].稀有金属快报,2008,27(4):7-10.
[8]黄永光.我国钛及钛合金标准现状思考[J].标准科学,2004(6):32-34.
[9]黄永光,庞洪,李宝霞.中国钛材行业的新标准[J].亚洲钛业咨询,2006(4):17-20.
[10]徐秋心.实用发射光谱分析[M].成都:四川科学技术出版社,1992.