Abstract：A determination method of six elements including niobium, tantalum, copper, titanium, aluminum and phosphorus in ferro-niobium by X-ray fluorescence spectrometry (XRF) was established after sample was prepared with fusion method. The sample was pretreated with hydrofluoric acid and nitric acid. The dissolution reaction was mild, which effectively avoid the corrosion problem of crucible in sample fusion process. The series of ferro-niobium calibration sample composed by ferro-niobium certified reference materials, and the ferro-niobium synthetic samples which were mixed with these certified reference materials, the standard solution of single element and high-purity niobium pentoxide. The content range of calibration curve was broadened. Lithium tetraborate and lithium bromide was used as flux and releasing agent, respectively. The dilution ratio was 1∶30. After fusion at 1 050 ℃ for 15 min, the glass sheet was uniform and smooth without air holes on surface, which could meet the requirement for determination. The matrix effect caused by the change of composition and content of sample was corrected by theoretical α coefficient method combined with empirical coefficient method. The precision and accuracy results indicated that the relative standard deviations (RSD, n=10) of determination results of elements were between 0.26% and 1.0%. The results were consistent with the certified values of ferro-niobium certified reference material. The proposed method could meet the requirement for determination in routine production.
成勇.电感耦合等离子体原子发射光谱法测定铌铁合金中铌[J].冶金分析,2015,35(9):32-35.CHENG Yong.Determination of niobium in niobium-iron alloy by inductively coupled plasma atomic emission spectrometry[J].Metullargical Analysis,2015,35(9):32-35.
[2]
邵海舟,刘成花.电感耦合等离子体原子发射光谱法测定铌铁中铌钛钽硅铝磷[J].冶金分析,2011,31(12):54-57.SHAO Hai-zhou,LIU Cheng-hua.Determination of niobium,titanium,tantalum,silicon,aluminium and phosphorus in ferroniobium by inductively coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2011,31(12):54-57.
[3]
陶俊.电感耦合等离子体原子发射光谱法测定铌铁中多元素[J].冶金分析,2009,29(2):69-72.TAO Jun.Determination of multi-elements in ferroniobium by inductivel coupled plasma atomic emission spectrometry[J].Metallurgical Analysis,2009,29(2):69-72.
[4]
陆晓明,金德龙.离心浇铸制样-X-射线荧光光谱法测定铌铁合金中铌硅磷[J].冶金分析,2009,29(3):16-19.LU Xiao-ming,JIN De-long.Determination of niobium,silicon and phosphorus in ferrocolumbium by X-ray fluorescence spectrometry using sample preparation technique of centrifugal casting[J].Metallurgical Analysis,2009,29(3):16-19.
[5]
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.REN Bao-lin.Determination of major and minor components in vanadium slag,vanadium slag clinker and vanadium tailings by X-ray fluorescence spectrometry[J].Metallurgical Analysis,2015,35(7):79-83.
[6]
李京.熔融制样-X射线荧光光谱法测定锰铁中锰硅磷[J].冶金分析,2011,31(6):51-53.LI Jing.Determination of manganese,silicon and phosphorus in ferromanganese by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2011,31(6):51-53.
[7]
吴银军,李士宏.熔融-X射线荧光光谱法测定镁质类耐火材料主次成分含量[J].冶金标准化与质量,2014,52(4):11-13.WU Yin-jun,LI Shi-hong.Determination of major components in MgO refractories molten-X ray fluorescence spectrometry[J].Metallurgical Standardization & Quality,2014,52(4):11-13.
[8]
林忠,李卫刚,褚宁,等.熔融制样-波长色散X射线荧光光谱法测定红土镍矿中铁、镍、硅、铝、镁、钙、钛、锰、铜和磷[J].分析仪器,2012(4):53-57.LI Zhong,LI Wei-gang,CHU Ning,et al.Determination of iron,nickel,silicon,aluminum,magnesium,calcium,titanium,manganese,copper and phosphorus in laterite nickel ores by wavelength dispersive X-ray fluorescence spectrometry with fusion sample preparation[J].Analytical Instrumentation,2012(4):53-57.
[9]
薛秋红,李静,丁玉龙,等.玻璃熔片制样-X射线荧光光谱法测定矾土中主次量组分[J].岩矿测试,2010,29(2):182-184.XUE Qiu-hong,LI Jing,DING Yu-long,et al.Determination of major and minor components in bauxite by X-ray fluorescence spectrometry with fusion sample preparation[J].Rock and Mineral Analysis,2010,29(2):182-184.
[10]
王一凌,曲月华,邓军华.X 射线荧光光谱分析法熔融制样技术的探讨与应用[J].冶金分析,2010,30(12):10-13.WANG Yi-ling,QU Yue-hua,DENG Jun-hua.Discussion and application of sample preparation by fusion in X-ray fluorescence spectrometry[J].Metallurgical Analysis,2010,30(12):10-13.
