熔融制样X射线荧光光谱法测定碳酸盐岩样品中的主次成分
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摘要
采用复合熔剂玻璃熔片法制备样片,X射线荧光光谱法测定碳酸盐岩样品中SiO_2、Fe_2O_3、Al_2O_3、TiO_2、CaO、MgO、K_2O、Na_2O、MnO和P_2O_5等主次成分.使用理论α系数校正基体效应,国家一级标准物质验证,方法简单快速.测量结果各元素相对标准偏差(RSD,n=12)低于10%(除含量在检出限附近的元素外),检出限低,能够符合地矿行业的要求.
A method for the determination of major and minor elements including SiO_2,Fe_2O_3,Al_2O_3,TiO_2,CaO,MgO,K_2O,Na_2O,MnO and P_2O_5 in carbonate rock samples by Axios X-ray fluorescence spectrometry with mixed flux fusion pellets was proposed. The matrix effect was corrected using the theoretical alpha coefficient. The method was verified by the first-class national standard material. The method is simple and rapid. The relative standard deviation( RSD,n = 12) of each element in the measurement results was less than 10%( except for the contents of elements near the detection limit),and the detection limit was low,which can meet the requirements of the geological and mining industry.
A method for the determination of major and minor elements including SiO_2,Fe_2O_3,Al_2O_3,TiO_2,CaO,MgO,K_2O,Na_2O,MnO and P_2O_5 in carbonate rock samples by Axios X-ray fluorescence spectrometry with mixed flux fusion pellets was proposed. The matrix effect was corrected using the theoretical alpha coefficient. The method was verified by the first-class national standard material. The method is simple and rapid. The relative standard deviation( RSD,n = 12) of each element in the measurement results was less than 10%( except for the contents of elements near the detection limit),and the detection limit was low,which can meet the requirements of the geological and mining industry.
引文
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[9]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.[LI Guohui,LI Xiao-li.Systematic study on X-ray fluorescence spectroscopy analysis of molten samples[J].Metallurgical Analysis,2015,35(7):1-9.]
[10]Claisse F,Blanchette J S.Physics and Chemisthry of Borate Fusion[M].卓尚军译.上海:华东理工大学出版社,2006.
[2]普旭力,王鸿辉,叶淑爱,等.波长色散X射线荧光光谱法同时测定钨精矿中主次量组分[J].岩矿测试,2010,29(2):143-147.[PU Xu-li,WANG Hong-hui,YE Shu-ai,et al.Simultaneous determination of major and minor components in tungsten concentrate by wavelength dispersive X-ray fluorescence spectrometry[J].Rock and Mineral Testing,2010,29(2):143-147.]
[3]曾江萍,吴磊,李小莉,等.较低稀释比熔融制样X射线荧光光谱法分析铬铁矿[J].岩矿测试,2013,32(6):915-919.[ZENG Jiang-ping,WU Lei,LIXiao-li,et al.X-ray fluorescence spectrometry for analysis of chromite[J].Rock and Mineral Testing,2013,32(6):915-919.]
[4]袁秀茹,余宇,赵峰,等.X射线荧光光谱法同时测定白云岩中氧化钙和氧化镁等主次量组分[J].岩矿测试,2009,28(4):376-378.[YUAN Xiu-ru,YUYu,ZHAO Feng,et al.Simultaneous determination of major and minor components such as calcium oxide and magnesium oxide in dolomite by X-ray fluorescence spectrometry[J].Rock and Mineral Testing,2009,28(4):376-378.]
[5]刘江斌,赵峰,余宇,等.X射线荧光光谱法同时测定地质样品中铌钽锆铪铈镓钪铀等稀有元素[J].岩矿测试,2010,29(1):74-76.[LIU Jiang-bin,ZHAO Feng,YU Yu,et al.Simultaneous determination of Nb,Ta,Zr,Hf,Ce,Ga,Sc,U and other rare elements in Geological Samples by X-ray fluorescence spectrometry[J].Rock and Mineral Testing,2010,29(1):74-76.]
[6]丁仕兵,曲晓霞,岳春雷.X-射线荧光光谱法测定铁矿石中全铁[J].冶金分析,2006,26(3):96-97.[DING Shi-bing,QU Xiao-xia,YUE Chun-lei.X-ray fluorescence spectrometry for the determination of total iron in iron ore[J].Metallurgical Analysis,2006,26(3):96-97.]
[7]朱忠平,李国会.熔融制样-X射线荧光光谱法测定钛铁矿中主次组分[J].冶金分析,2013,33(6):32-36.[ZHU Zhong-ping,LI Guo-hui.Determination of major and minor components in Ilmenite by melt sampling-X-ray fluorescence spectrometry[J].Metallurgical Analysis,2013,33(6):32-36.]
[8]张爱芬,马慧侠,李国会.X射线荧光光谱法测定铝矿石中主次恒量组分[J].岩矿测试,2005,24(4):307-310.[ZHANG Ai-fen,MA Hui-xia,LI Guo-hui.X-ray fluorescence spectrometry for the determination of primary and secondary constant components in aluminium ores[J].Rock and Mineral Testing,2005,24(4):307-310.]
[9]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.[LI Guohui,LI Xiao-li.Systematic study on X-ray fluorescence spectroscopy analysis of molten samples[J].Metallurgical Analysis,2015,35(7):1-9.]
[10]Claisse F,Blanchette J S.Physics and Chemisthry of Borate Fusion[M].卓尚军译.上海:华东理工大学出版社,2006.