X射线荧光光谱法测定高铬型钒渣中主次组分
|
摘要
称取于750~800℃灼烧2h后的试样0.300 0g,置于盛有4.000 0g四硼酸锂、3.000 0g偏硼酸锂、0.500 0g碳酸锂的铂黄坩埚中,搅匀,加入300g·L-1溴化锂溶液0.5mL,在(1 050±20)℃熔融制片,采用X射线荧光光谱法测定高铬型钒渣中主次组分含量。采用钒渣标准样品和由标准样品加基准物质配制成的系列校准样品绘制校准曲线以消除基体效应,选择分析谱线并进行谱线重叠干扰校正。各组分的质量分数在一定范围内与荧光强度呈线性关系。方法用于分析高铬型钒渣样品,所得结果与滴定法、电感耦合等离子体原子发射光谱法的结果一致,测定值的相对标准偏差(n=10)在0.030%~7.3%之间。
After ignition at 750-800 ℃for 2 h,0.300 0 g of the sample was mixed well with 4.000 0 g of lithium tetraborate,3.000 0 g of lithium metaborate,and 0.500 0 g of lithium carbonate in a platinum yellow crucible.Then 0.5 mL of 300 g·L-1 lithium bromide solution was added into the crucible and the mixture was melted at(1 050±20)℃ to prepare sample sheets.The contents of major and minor components in the high chromium type vanadium slag were determined by X-ray fluorescence spectrometry.Vanadium slag standard samples and a series of calibration samples prepared with the standard samples and the reference substance were used to draw calibration curves to eliminate the matrix effect.The analysis lines were selected and spectral line overlap interference correction was performed.Linear relationships were found between values of the fluorescence intensity and the mass fractions of each component within definite ranges.The method was applied to analysis of high chromium type vanadium slag samples,giving results in consistency with those obtained by titration and inductively coupled plasma atomic emission spectrometry,and RSDs(n=10)were between 0.030% and 7.3%.
After ignition at 750-800 ℃for 2 h,0.300 0 g of the sample was mixed well with 4.000 0 g of lithium tetraborate,3.000 0 g of lithium metaborate,and 0.500 0 g of lithium carbonate in a platinum yellow crucible.Then 0.5 mL of 300 g·L-1 lithium bromide solution was added into the crucible and the mixture was melted at(1 050±20)℃ to prepare sample sheets.The contents of major and minor components in the high chromium type vanadium slag were determined by X-ray fluorescence spectrometry.Vanadium slag standard samples and a series of calibration samples prepared with the standard samples and the reference substance were used to draw calibration curves to eliminate the matrix effect.The analysis lines were selected and spectral line overlap interference correction was performed.Linear relationships were found between values of the fluorescence intensity and the mass fractions of each component within definite ranges.The method was applied to analysis of high chromium type vanadium slag samples,giving results in consistency with those obtained by titration and inductively coupled plasma atomic emission spectrometry,and RSDs(n=10)were between 0.030% and 7.3%.
引文
[1]YB/T 547.1-2014钒渣五氧化二钒含量的测定硫酸亚铁铵滴定法[S].
[2]YB/T 547.2-2014钒渣二氧化硅含量的测定高氯酸脱水重量法[S].
[3]YB/T 547.3-2014钒渣氧化钙含量的测定火焰原子吸收光谱法和高锰酸钾容量法测定氧化钙量[S].
[4]YB/T 547.4-2014钒渣磷含量的测定铋磷钼蓝分光光度法[S].
[5]黎香荣,陈永欣,罗明贵,等.波长色散X射线荧光光谱法同时测定钒渣中的主次量成分[J].岩矿测试,2011,30(2):222-225.
[6]任保林.X射线荧光光谱法测定钒渣、钒渣熟料和提钒尾渣中主次组分[J].冶金分析,2015,35(7):79-83.
[7]陈荣庆.粉末压片-X射线荧光光谱法测定钒渣中的化学成分[J].光谱实验室,2008,25(3):416-420.
[8]杨洪春,冯宗平.电感耦合等离子体原子发射光谱法测定钒渣中主次成分[J].冶金分析,2010,30(6):50-53.
[9]杨新能,李小青,杨大军.X射线荧光光谱法测定含金属等还原剂的炼钢辅料中化学成分[J].冶金分析,2014,34(2):40-43.
[10]方海星.高铬型钒渣的物化性质及钒铬选择性提取方法的研究[D].重庆:重庆大学,2014.
[11]克拉斯,布兰切特.硼酸盐熔融的物理与化学:献给X射线荧光光谱学工作者[M].卓尚军,译.上海:华东理工大学出版社,2006.
[12]李国会,李小莉.X射线荧光光谱分析熔融法制样的系统研究[J].冶金分析,2015,35(7):1-9.
[2]YB/T 547.2-2014钒渣二氧化硅含量的测定高氯酸脱水重量法[S].
[3]YB/T 547.3-2014钒渣氧化钙含量的测定火焰原子吸收光谱法和高锰酸钾容量法测定氧化钙量[S].
[4]YB/T 547.4-2014钒渣磷含量的测定铋磷钼蓝分光光度法[S].
[5]黎香荣,陈永欣,罗明贵,等.波长色散X射线荧光光谱法同时测定钒渣中的主次量成分[J].岩矿测试,2011,30(2):222-225.
[6]任保林.X射线荧光光谱法测定钒渣、钒渣熟料和提钒尾渣中主次组分[J].冶金分析,2015,35(7):79-83.
[7]陈荣庆.粉末压片-X射线荧光光谱法测定钒渣中的化学成分[J].光谱实验室,2008,25(3):416-420.
[8]杨洪春,冯宗平.电感耦合等离子体原子发射光谱法测定钒渣中主次成分[J].冶金分析,2010,30(6):50-53.
[9]杨新能,李小青,杨大军.X射线荧光光谱法测定含金属等还原剂的炼钢辅料中化学成分[J].冶金分析,2014,34(2):40-43.
[10]方海星.高铬型钒渣的物化性质及钒铬选择性提取方法的研究[D].重庆:重庆大学,2014.
[11]克拉斯,布兰切特.硼酸盐熔融的物理与化学:献给X射线荧光光谱学工作者[M].卓尚军,译.上海:华东理工大学出版社,2006.
[12]李国会,李小莉.X射线荧光光谱分析熔融法制样的系统研究[J].冶金分析,2015,35(7):1-9.