全自动制样-X射线荧光光谱法测定硅铁中硅
|
摘要
采用全自动制样,建立了X射线荧光光谱法(XRF)快速测定硅铁中硅的方法。通过对比X-ray专用助磨剂、进口助磨剂、微晶纤维素、硬脂酸等几种助磨剂在制作硅铁压片时的使用效果,确定使用X-ray专用助磨剂作为硅铁压片添加剂,样品与助磨剂的添加比例为9∶1(质量比);全自动制样机制备硅铁压片时,样品初始粒度要求过160目筛网(孔径96μm)、研磨时间为130s、压力为35t、保压时间为20s。用上述方法可以得到结构均匀致密、外表平整光滑的硅铁压片。采用不同时期的多个生产样合并为一个管理样,与购买的硅铁标样配制校准曲线标样,校准曲线硅含量范围能够满足测定要求,并有效消除矿物效应对测定的影响。采用实验方法测定硅铁中硅,分析结果同SN/T 1014.1—2001的氟硅酸钾滴定法相吻合,相对标准偏差(RSD,n=11)小于0.2%。
The rapid determination method of silicon in ferrosilicon by X-ray fluorescence spectrometry(XRF)after fully-automatic sample preparation was established.The effect of several grinding aids(including specific grinding aid for XRF analysis,imported grinding aid,microcrystalline cellulose and stearic acid)on pressed ferrosilicon sample was compared.The specific grinding aid for XRF analysis was selected as additive for sample preparation of ferrosilicon.The addition ratio of sample and grinding aid was 9∶1(mass ratio).During the preparation of ferrosilicon sample by fully-automatic machine,the initial particle size of sample should pass through 160-mesh screen(particle size of 96μm).The grinding time was 130 s,the pressure was 35 tand the pressure keeping time was 20 s.The ferrosilicon sample with uniform and dense structure and smooth surface could be obtained.Several production samples from different stages were combined as one control sample,which was used to prepare calibration curve with purchased ferrosilicon standard sample.The content range of silicon in calibration curve could meet determination requirements.The influence of mineral effect on determination could be effectively eliminated.The proposed method was applied to the determination of silicon in ferrosilicon.The found results were consistent with those obtained by SN/T 1014.1—2001potassium fluosilicate titration method.The relative standard deviation(RSD,n=11)was less than 0.2%.
The rapid determination method of silicon in ferrosilicon by X-ray fluorescence spectrometry(XRF)after fully-automatic sample preparation was established.The effect of several grinding aids(including specific grinding aid for XRF analysis,imported grinding aid,microcrystalline cellulose and stearic acid)on pressed ferrosilicon sample was compared.The specific grinding aid for XRF analysis was selected as additive for sample preparation of ferrosilicon.The addition ratio of sample and grinding aid was 9∶1(mass ratio).During the preparation of ferrosilicon sample by fully-automatic machine,the initial particle size of sample should pass through 160-mesh screen(particle size of 96μm).The grinding time was 130 s,the pressure was 35 tand the pressure keeping time was 20 s.The ferrosilicon sample with uniform and dense structure and smooth surface could be obtained.Several production samples from different stages were combined as one control sample,which was used to prepare calibration curve with purchased ferrosilicon standard sample.The content range of silicon in calibration curve could meet determination requirements.The influence of mineral effect on determination could be effectively eliminated.The proposed method was applied to the determination of silicon in ferrosilicon.The found results were consistent with those obtained by SN/T 1014.1—2001potassium fluosilicate titration method.The relative standard deviation(RSD,n=11)was less than 0.2%.
引文
[1]尹显武,刘灿.碱熔-氟硅酸钾容量法测定硅铁中硅含量应用实践[J].天津冶金,2012(6):51-54.YIN Xian-wu,LIU Can.Applications of alkaline dissolving-potassium fluorosilicate volumetric analysis in determination of silicon in ferrosilicon[J].Tianjin Metallurgy,2012(6):51-54.
[2]陆晓明,金德龙,胡莹.X射线荧光光谱法测定镍铬合金中15种元素[J].冶金分析,2013,33(10):49-55.LU Xiao-ming,JIN De-long,HU Ying.Determination of fifteen elements in nickel-chromium alloy by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2013,33(10):49-55.
[3]罗学辉,张勇,艾晓军,等.熔融玻璃片-波长色散X射线荧光光谱法测定铁矿石中全铁及其它多种元素的分析进展[J].中国无机分析化学,2009,29(3):16-19.LUO Xue-hui,ZHANG Yong,AI Xiao-jun,et al.Analytical progress of determining TFe and other elements in iron ore by liquated sheet glass-WDXRF[J].Chinese Journal of Inorganic Analytical Chemistry,2011,1(3):23-26.
[4]郑荣华,刘建坤.粉末压片-X射线荧光光谱法测定矿石中钨、锡[J].理化检验:化学分册,2013,49(1):66-68.ZHENG Rong-hua,LIU Jian-kun.Determination of tungsten and stannum in ore by pressed powder-XRF[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2013,49(1):66-68.
[5]王利杰,张健,杨志强,等.应用粉末压片-X射线荧光光谱法检验铁矿石样品的均匀性[J].冶金分析,2012,32(5):40-44.WANG Li-jie,ZHANG Jian,YANG Zhi-qiang,et al.Xray fluorescence spectrometric examination of uniformity of iron ore sample with pressed powder pellet[J].Metallurgical Analysis,2012,32(5):40-44.
[6]韩蔚,丁建军,梅一飞,等.X射线荧光光谱法测定石膏中11种元素的含量[J].理化检验:化学分册,2015,51(2):188-191.HAN Wei,DING Jian-jun,MEI Yi-fei,et al.XRFS determination of 11elements in gypsum[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2015,51(2):188-191.
[7]高树峰,张海岩,张玉平,等.X射线荧光光谱法测定氮化钒铁中铁、钒、硅的含量[J].理化检验:化学分册,2014,50(6):681-684.GAO Shu-feng,ZHANG Hai-yan,ZHANG Yu-ping,et al.XRFS determination of iron,vanadium and silicon in ferrovanadium nitride[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2014,50(6):681-684.
[8]高捷,盛成,卓尚军.X射线荧光光谱分析用的含铁尘泥标准样品的研制[J].冶金分析,2015,35(2):74-78.GAO Jie,SHENG Cheng,ZHUO Shang-jun.Development of ferric-containing dust and sludge standard samples used for X-ray fluorescence spectrometric analysis[J].Metallurgical Analysis,2015,35(2):74-78.
[9]高建民,曲志勇,张愈洁,等.X射线荧光光谱法测定生铁中10种元素[J].冶金分析,2011,31(4):39-43.GAO Jian-min,QU Zhi-yong,ZHANG Yu-jie,et al.Determination of ten elements in cast iron by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2011,31(4):39-43.
[10]徐永宏.X荧光光谱法测定硅铁中主次量元素[J].梅山科技,2004(2):18-20.XU Yong-hong.Determination of the major and minor elements in ferrosilicon by XRFS[J].Meishan Science and Technology,2004(2):18-20.
[11]姚燕群,魏海青.离心浇铸制样-X射线荧光光谱法测定硅铁中的硅[J].浙江冶金,2011,5(2):20-21.YAO Yan-qun,WEI Hai-qing.Determination of silicon in ferrosilicon by centrifugal casting sample preparation-XRF[J].Journal of Zhejiang Metallurgy,2011,5(2):20-21.
[12]任玉伟,胡晓静,盛向军,等.X-射线荧光光谱法测定稀土硅铁合金中锰硅铝钙钛[J].冶金分析,2009,29(1):59-62.REN Yu-wei,HU Xiao-jing,SHENG Xiang-jun,et al.Determination of Mn,Si,Al,Ca,Ti in rare earth ferrosilicon alloy by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2009,29(1):59-62.
[2]陆晓明,金德龙,胡莹.X射线荧光光谱法测定镍铬合金中15种元素[J].冶金分析,2013,33(10):49-55.LU Xiao-ming,JIN De-long,HU Ying.Determination of fifteen elements in nickel-chromium alloy by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2013,33(10):49-55.
[3]罗学辉,张勇,艾晓军,等.熔融玻璃片-波长色散X射线荧光光谱法测定铁矿石中全铁及其它多种元素的分析进展[J].中国无机分析化学,2009,29(3):16-19.LUO Xue-hui,ZHANG Yong,AI Xiao-jun,et al.Analytical progress of determining TFe and other elements in iron ore by liquated sheet glass-WDXRF[J].Chinese Journal of Inorganic Analytical Chemistry,2011,1(3):23-26.
[4]郑荣华,刘建坤.粉末压片-X射线荧光光谱法测定矿石中钨、锡[J].理化检验:化学分册,2013,49(1):66-68.ZHENG Rong-hua,LIU Jian-kun.Determination of tungsten and stannum in ore by pressed powder-XRF[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2013,49(1):66-68.
[5]王利杰,张健,杨志强,等.应用粉末压片-X射线荧光光谱法检验铁矿石样品的均匀性[J].冶金分析,2012,32(5):40-44.WANG Li-jie,ZHANG Jian,YANG Zhi-qiang,et al.Xray fluorescence spectrometric examination of uniformity of iron ore sample with pressed powder pellet[J].Metallurgical Analysis,2012,32(5):40-44.
[6]韩蔚,丁建军,梅一飞,等.X射线荧光光谱法测定石膏中11种元素的含量[J].理化检验:化学分册,2015,51(2):188-191.HAN Wei,DING Jian-jun,MEI Yi-fei,et al.XRFS determination of 11elements in gypsum[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2015,51(2):188-191.
[7]高树峰,张海岩,张玉平,等.X射线荧光光谱法测定氮化钒铁中铁、钒、硅的含量[J].理化检验:化学分册,2014,50(6):681-684.GAO Shu-feng,ZHANG Hai-yan,ZHANG Yu-ping,et al.XRFS determination of iron,vanadium and silicon in ferrovanadium nitride[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2014,50(6):681-684.
[8]高捷,盛成,卓尚军.X射线荧光光谱分析用的含铁尘泥标准样品的研制[J].冶金分析,2015,35(2):74-78.GAO Jie,SHENG Cheng,ZHUO Shang-jun.Development of ferric-containing dust and sludge standard samples used for X-ray fluorescence spectrometric analysis[J].Metallurgical Analysis,2015,35(2):74-78.
[9]高建民,曲志勇,张愈洁,等.X射线荧光光谱法测定生铁中10种元素[J].冶金分析,2011,31(4):39-43.GAO Jian-min,QU Zhi-yong,ZHANG Yu-jie,et al.Determination of ten elements in cast iron by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2011,31(4):39-43.
[10]徐永宏.X荧光光谱法测定硅铁中主次量元素[J].梅山科技,2004(2):18-20.XU Yong-hong.Determination of the major and minor elements in ferrosilicon by XRFS[J].Meishan Science and Technology,2004(2):18-20.
[11]姚燕群,魏海青.离心浇铸制样-X射线荧光光谱法测定硅铁中的硅[J].浙江冶金,2011,5(2):20-21.YAO Yan-qun,WEI Hai-qing.Determination of silicon in ferrosilicon by centrifugal casting sample preparation-XRF[J].Journal of Zhejiang Metallurgy,2011,5(2):20-21.
[12]任玉伟,胡晓静,盛向军,等.X-射线荧光光谱法测定稀土硅铁合金中锰硅铝钙钛[J].冶金分析,2009,29(1):59-62.REN Yu-wei,HU Xiao-jing,SHENG Xiang-jun,et al.Determination of Mn,Si,Al,Ca,Ti in rare earth ferrosilicon alloy by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2009,29(1):59-62.