X射线荧光光谱法分析铁矿石中19种组分
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摘要
选用铁矿石试样与混合熔剂(四硼酸锂-偏硼酸锂-溴化锂)、稀释比为1∶12、1 000℃熔融25min制备熔片,应用X射线荧光光谱法(XRF)测试铁矿石中全铁、二氧化硅、三氧化二铝、氧化钙、氧化镁、氧化锰、二氧化钛、磷、硫、氧化钾、氧化钠、五氧化二钒、铬、镍、铜、锌、砷、铅、氧化钡等19种组分。通过标准物质、光谱纯物质、人工合成样品及化学定值样品制作校准曲线并进行分段回归。添加氧化钴作内标校正元素铁,应用康普顿散射线校正铜、锌、砷、铅,采用经验系数法校正其他14种组分,可有效克服测定各类铁矿石中各组分时基体效应的影响。对铁矿石样品进行精密度试验考察,各组分测定结果的相对标准偏差(RSD,n=11)在0.13%~7.7%之间;对标准样品及未知样品进行准确度考察,测定值与认定值或湿法值一致。
The iron ore sample is prepared by fusion method under the following conditions:the mixed flux(lithium tetraborate-lithium metaborate-lithium bromide),the dilution ratio of 1∶12,and fusion at 1 000℃for 25 min.The content of 19 components in iron ore were determined by X-ray fluorescence spectrometry(XRF),including total iron,silicon dioxide,aluminum oxide,calcium oxide,magnesium oxide,manganese oxide,titanium dioxide,phosphorus,sulfur,potassium oxide,sodium oxide,vanadium pentoxide,chromium,nickel,copper,zinc,arsenic,lead and barium oxide.The calibration curves were prepared and piecewise regressed using the certified reference materials,spectral purity materials,artificially synthesized samples and samples which were certified by chemical method.The cobalt oxide was added as the internal standard to correct the determination of total iron.The elements of copper,zinc,arsenic and lead were corrected by the Compton scattering line.Other 14 components were corrected by the empirical coefficient method.The matrix effect could be effectively eliminated.The precision test of iron ore sample was conducted.The relative standard deviations(RSD,n=11)were between 0.13% and7.7%.The accuracy tests of standard sample and unknown sample were also conducted.The found results were consistent with the certified values or those obtained by the wet method.
The iron ore sample is prepared by fusion method under the following conditions:the mixed flux(lithium tetraborate-lithium metaborate-lithium bromide),the dilution ratio of 1∶12,and fusion at 1 000℃for 25 min.The content of 19 components in iron ore were determined by X-ray fluorescence spectrometry(XRF),including total iron,silicon dioxide,aluminum oxide,calcium oxide,magnesium oxide,manganese oxide,titanium dioxide,phosphorus,sulfur,potassium oxide,sodium oxide,vanadium pentoxide,chromium,nickel,copper,zinc,arsenic,lead and barium oxide.The calibration curves were prepared and piecewise regressed using the certified reference materials,spectral purity materials,artificially synthesized samples and samples which were certified by chemical method.The cobalt oxide was added as the internal standard to correct the determination of total iron.The elements of copper,zinc,arsenic and lead were corrected by the Compton scattering line.Other 14 components were corrected by the empirical coefficient method.The matrix effect could be effectively eliminated.The precision test of iron ore sample was conducted.The relative standard deviations(RSD,n=11)were between 0.13% and7.7%.The accuracy tests of standard sample and unknown sample were also conducted.The found results were consistent with the certified values or those obtained by the wet method.
引文
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[9]蒋薇.X射线荧光光谱法测定钒钛磁铁矿成分[J].光谱实验室,2005,22(5):940-942.JIANG Wei.Determination of components of vanadium titanium magnetite by X-ray fluorescence spectrometry[J].Chinese Journal of Spectroscopy Laboratory,2005,22(5):940-942.
[10]袁家义,吕振生,姜云.X射线荧光光谱熔融制样法测定钛铁矿中主次量组分[J].岩矿测试,2007,26(2):158-162.YUAN Jia-yi,LZhen-sheng,JIANG Yun.Determination of major and minor elements in ilmenite samples by X-ray fluorescence spectrometry with fusion sample preparation technique[J].Rock and Mineral Analysis,2007,26(2):158-162.
[11]陈忠厚,薛殿鹏.熔融玻璃片法X射线荧光光谱测定铁矿石中的主次量组分[J].有色矿冶,2014,30(2):101-104.CHEN Zhong-hou,XUE Dian-peng.The determination of major and minor components in iron ore by fused glass X-ray fluorescence spectrometry[J].Non-ferrous Mining and Metallurgy,2014,30(2):101-104.
[12]张莉娟,徐铁民,李小莉,等.X射线荧光光谱法测定富含硫砷钒铁矿石中的主次量元素[J].岩矿测试,2011,30(6):772-776.ZHANG Li-juan,XU Tie-min,LI Xiao-li,et al.Quantification of major and minor components in iron ores with sulfur,arsenic and vanadium by X-ray fluorescence spectrometry[J].Rock and Mineral Analysis,2011,30(6):772-776.
[13]吴静,王富仲,许增平.熔融制样—X射线荧光光谱法测定铁矿石中主次成分[J].冶金分析,2009,29(9):40-43.WU Jing,WANG Fu-zhong,XU Zeng-ping.Determination of main and minor components in iron ores by X-ray fluorescence spectrometry with fusion sampling[J].Metallurgical Analysis,2009,29(9):40-43.
[14]李国.扫描道代替固定道作内标通道分析铁矿石—X射线荧光光谱分析[J].理化检验:化学分册,2014,50(4):503-504.LI Guo.XRFS analysis of iron ore with scanning channel instead of fixed channel as internal standard channel[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2014,50(4):503-504.
[15]李国会,卜维,樊守忠.X射线荧光光谱法测定硅酸盐中硫等20个主、次、痕量元素[J].光谱学与光谱分析,1994,14(1):105-110.LI Guo-hui,BU Wei,FAN Shou-zhong.Determination of twenty major,minor and trace elements in silicate by XRF spectrometry[J].Spectroscopy and Spectral Analysis,1994,14(1):105-110.
[2]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(Metallurgical Analysis),2006,26(3):96-97.
[3]欧阳伦熬.X射线荧光光谱法测定多种铁矿和硅酸盐中主次量组分[J].岩矿测试,2005,24(4):303-306.OU YANG Lun-ao.Determination of major and minor elements in iron ores and silicates by XRF spectrometry with fusion sample preparation technique[J].Rock and Mineral Analysis,2005,24(4):303-306.
[4]崔黎黎.X射线荧光光谱法测定铁矿石中主次成分[J].冶金分析,2009,29(12):21-24.CUI Li-li.Determination of major and minor elements in iron ore by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2009,29(12):21-24.
[5]李超.XRF法测定铁矿石中TFe、SiO2和P[J].光谱实验室,2005,22(2):360-361.LI Chao.Determination of TFe,SiO2and P in the iron ore by XRF spectrometry[J].Chinese Journal of Spectroscopy Laboratory,2005,22(2):360-361.
[6]廖海平,付冉冉,任春生,等.X射线荧光光谱法测定铁矿石中全铁及18个次量成分[J].冶金分析,2011,31(5):36-40.LIAO Hai-ping,FU Ran-ran,REN Chun-sheng,et al.Determination of total iron and eighteen minor components in iron ore by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2011,31(5):36-40.
[7]许鸿英,张继丽,张艳萍,等.X射线荧光光谱分析多矿源铁矿石中9种成分[J].冶金分析,2009,29(10):24-27.XU Hong-ying,ZHANG Ji-li,ZHANG Yan-ping,et al.Determination of nine components in various source iron ores by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2009,29(10):24-27.
[8]边立槐,田桂英,杨觎.元素钡对X射线荧光光谱法测定铁矿中全铁的修正作用[J].光谱实验室,2007,24(5):784-786.BIAN Li-huai,TIAN Gui-ying,YANG Yu.The improvement in the determination of total iron in iron ore by X-ray fluorescence spectrometry with addition of bar-um[J].Chinese Journal of Spectroscopy Laboratory,2007,24(5):784-786.
[9]蒋薇.X射线荧光光谱法测定钒钛磁铁矿成分[J].光谱实验室,2005,22(5):940-942.JIANG Wei.Determination of components of vanadium titanium magnetite by X-ray fluorescence spectrometry[J].Chinese Journal of Spectroscopy Laboratory,2005,22(5):940-942.
[10]袁家义,吕振生,姜云.X射线荧光光谱熔融制样法测定钛铁矿中主次量组分[J].岩矿测试,2007,26(2):158-162.YUAN Jia-yi,LZhen-sheng,JIANG Yun.Determination of major and minor elements in ilmenite samples by X-ray fluorescence spectrometry with fusion sample preparation technique[J].Rock and Mineral Analysis,2007,26(2):158-162.
[11]陈忠厚,薛殿鹏.熔融玻璃片法X射线荧光光谱测定铁矿石中的主次量组分[J].有色矿冶,2014,30(2):101-104.CHEN Zhong-hou,XUE Dian-peng.The determination of major and minor components in iron ore by fused glass X-ray fluorescence spectrometry[J].Non-ferrous Mining and Metallurgy,2014,30(2):101-104.
[12]张莉娟,徐铁民,李小莉,等.X射线荧光光谱法测定富含硫砷钒铁矿石中的主次量元素[J].岩矿测试,2011,30(6):772-776.ZHANG Li-juan,XU Tie-min,LI Xiao-li,et al.Quantification of major and minor components in iron ores with sulfur,arsenic and vanadium by X-ray fluorescence spectrometry[J].Rock and Mineral Analysis,2011,30(6):772-776.
[13]吴静,王富仲,许增平.熔融制样—X射线荧光光谱法测定铁矿石中主次成分[J].冶金分析,2009,29(9):40-43.WU Jing,WANG Fu-zhong,XU Zeng-ping.Determination of main and minor components in iron ores by X-ray fluorescence spectrometry with fusion sampling[J].Metallurgical Analysis,2009,29(9):40-43.
[14]李国.扫描道代替固定道作内标通道分析铁矿石—X射线荧光光谱分析[J].理化检验:化学分册,2014,50(4):503-504.LI Guo.XRFS analysis of iron ore with scanning channel instead of fixed channel as internal standard channel[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2014,50(4):503-504.
[15]李国会,卜维,樊守忠.X射线荧光光谱法测定硅酸盐中硫等20个主、次、痕量元素[J].光谱学与光谱分析,1994,14(1):105-110.LI Guo-hui,BU Wei,FAN Shou-zhong.Determination of twenty major,minor and trace elements in silicate by XRF spectrometry[J].Spectroscopy and Spectral Analysis,1994,14(1):105-110.