X射线荧光光谱法测定合金中钨的含量
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摘要
采用X射线荧光光谱法测定了多种含钨合金钢以及含钨较高的镍基和钴基合金中钨的含量。方法中选择钨的Lβ1线为分析线,并选择2θ角在39.50°处作为背景位置。在合金中钽的Lβ2线对钨分析线有重叠干扰,选两套标准样品用基本参数法(FP)测出了干扰系数k,将k值列入仪器的FP工作软件中来消除钽对钨测定的重叠干扰。用所提出的方法分析了钨质量分数在0.054%～11.71%内的5个标准样品,测定值与认定值相符,测定值的相对标准偏差(n=7)在0.55%～9.5%之间。
XRFS was applied to the determination of tungsten in various tungsten containing alloy stees,Nibased and Co-based alloys.The spectral line of Lβ1 of W was chosen as analytical spectral line,and 2θof 39.50°was selected as background site.Spectral line of Lβ2 of Ta was found to interfere with the line of Lβ1 of W.Two sets of standard samples were selected and fundamental parameter(FP)method was used with help of FP software to find out the overlap-interfering coefficient k,which was listed in FP software to eliminate the overlap-interference from Ta to W.5 standard samples with W content ranging from 0.054% to 11.71%,were analyzed by the proposed method,giving results in consistency with the certified values,and RSDs(n=7)ranged from 0.55%to 9.5%.
XRFS was applied to the determination of tungsten in various tungsten containing alloy stees,Nibased and Co-based alloys.The spectral line of Lβ1 of W was chosen as analytical spectral line,and 2θof 39.50°was selected as background site.Spectral line of Lβ2 of Ta was found to interfere with the line of Lβ1 of W.Two sets of standard samples were selected and fundamental parameter(FP)method was used with help of FP software to find out the overlap-interfering coefficient k,which was listed in FP software to eliminate the overlap-interference from Ta to W.5 standard samples with W content ranging from 0.054% to 11.71%,were analyzed by the proposed method,giving results in consistency with the certified values,and RSDs(n=7)ranged from 0.55%to 9.5%.
引文
[1] GB/T 223.43-2008钢铁及合金钨含量的测定重量法和分光光度法[S].
[2] GB/T 223.66-1989钢铁及合金化学分析方法硫氰酸盐-盐酸氯丙嗪-三氯甲烷萃取光度法测定钨量[S].
[3] HB 5220.31-2008高温合金化学分析方法辛可宁-乙萘喹啉重量法测钨含量[S].
[4] HB 5220.32-2008高温合金化学分析方法硫氰酸盐吸光光度法测定钨含量[S].
[5] GB/T 4336-2016碳素钢和中低合金钢火花源原子发射光谱分析方法[S].
[6]梁钰.X射线荧光光谱分析基础[M].北京:科学出版社,2007.
[7]葛颖新,张环月,唐侠.X射线荧光光谱分析中谱线重叠校正系数的测量[J].理化检验-化学分册,2017,53(2):183-189.
[8] ASTM E1621-08 Standard practice for correction of spectral line overlap in wavelength dispersive X-ray spectrometry[S].
[9]唐侠,葛颖新,张庸.X射线荧光光谱法测定铁基中合金组分的通用工作曲线的制作[J].理化检验-化学分册,2015,51(5):680-685.
[10]闫秀芬,唐侠,张环月.X射线荧光光谱法测定镍基高温合金中合金组分的通用工作曲线的制作[J].理化检验-化学分册,2014,50(11):1434-1440.
[11]宋小龙,安继儒.新编中外金属材料手册[M].北京:化学工业出版社,2012.
[12] GB/T 223.79-2007钢铁多元素含量的测定X射线荧光光谱法[S].
[2] GB/T 223.66-1989钢铁及合金化学分析方法硫氰酸盐-盐酸氯丙嗪-三氯甲烷萃取光度法测定钨量[S].
[3] HB 5220.31-2008高温合金化学分析方法辛可宁-乙萘喹啉重量法测钨含量[S].
[4] HB 5220.32-2008高温合金化学分析方法硫氰酸盐吸光光度法测定钨含量[S].
[5] GB/T 4336-2016碳素钢和中低合金钢火花源原子发射光谱分析方法[S].
[6]梁钰.X射线荧光光谱分析基础[M].北京:科学出版社,2007.
[7]葛颖新,张环月,唐侠.X射线荧光光谱分析中谱线重叠校正系数的测量[J].理化检验-化学分册,2017,53(2):183-189.
[8] ASTM E1621-08 Standard practice for correction of spectral line overlap in wavelength dispersive X-ray spectrometry[S].
[9]唐侠,葛颖新,张庸.X射线荧光光谱法测定铁基中合金组分的通用工作曲线的制作[J].理化检验-化学分册,2015,51(5):680-685.
[10]闫秀芬,唐侠,张环月.X射线荧光光谱法测定镍基高温合金中合金组分的通用工作曲线的制作[J].理化检验-化学分册,2014,50(11):1434-1440.
[11]宋小龙,安继儒.新编中外金属材料手册[M].北京:化学工业出版社,2012.
[12] GB/T 223.79-2007钢铁多元素含量的测定X射线荧光光谱法[S].