Determination of titanium, silicon, manganese, phosphorus andaluminum in ferrotitanium by X-ray fluorescence spectrometry with fusion sample preparation
HOU Gangtie, ZHANG Gaimei, BAO Xibo
HBIS Group Hansteel Company Technology Center,Handan 056015, China
Abstract：During the determination of chemical compositions in ferrotitanium by X-ray fluorescence spectrometry (XRF) with fusion sample preparation, the core technology is the oxidization of alloy sample to effectively avoid the corrosion of platinum-gold crucible by sample in fusion process. The ferrotitanium sample was oxidized to titanium-iron molten globule in graphite backed porcelain crucible with a special oxidant. The sample was prepared to glass bead with mixed flux of lithium tetraborate and lithium carbonate. The determination method of titanium, silicon, manganese, phosphorus and aluminum in ferrotitanium by X-ray fluorescence spectrometry was established. The effects of flux selection, dosage of special oxidant, oxidation conditions, dilution ratio, mold release agent and melting time on the quality of glass bead and testing results were further discussed. The optimal oxidation and melting conditions were obtained. The prepared glass bead had uniform and smooth surface with good strength, which could meet the requirements of XRF determination. The calibration curves were established using the certified reference materials. The correlation coefficients of calibration curves for titanium, silicon, manganese, phosphorus and aluminum were between 0.999 6 and 1.000 0, which could meet the requirements of XRF. The proposed method was applied to the determination of ferrotitanium samples, and the relative standard deviations (RSD) of measurement results of elements were between 0.25% and 6.5%. The accuracy test results showed that the measured values of ferrotitanium standard samples were consistent with the certified values. The experimental method solved the corrosion problem of platinum-gold crucible during the fusion sample preparation of ferrotitanium. It realized the rapid and simultaneous analysis of titanium, silicon, manganese, phosphorus and aluminum contents in ferrotitanium, and could meet the quality control and daily determination requirements of ferrotitanium to guide the steelmaking production.
[1] 张天佑,李国会,仲平.X射线荧光分析[M].北京:科学出版社,1987. [2] 吉昂,陶光仪,卓尚军,等.X射线荧光光谱分析[M].北京:科学出版社,2003. [3] 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,phosphorus in ferromanganese by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2011,31(6):51-53. [4] 刘伟,曹吉祥,郭云涛,等.熔融制样-X-射线荧光光谱法测定硅锰合金中硅锰磷[J].冶金分析,2015,35(8):51-54. LIU Wei,CAO Jixiang,GUO Yuntao,et al.Determination of silicon,manganese,phosphorus in silicomanganese alloy by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2015,35(8):51-54. [5] 吴超超,陈自斌,邢文青,等.熔融制样-X 射线荧光光谱法测定锰铁、硅锰合金中锰硅磷[J].冶金分析,2018,38(3):14-21. WU Chaochao,CHEN Zibin,XING Wenqing,et al.Determination of manganese,silicon,phosphorus in ferromanganese and silicomanganese alloy by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2018,28(3):14-21. [6] 李小青.熔融制样-X射线荧光光谱法测定锰铁和金属锰中锰硅磷[J].冶金分析,2018,38(6):39-42. LI Xiaoqing.Determination of manganese,silicon,phosphorus in ferromanganese and manganese metal by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2018,38(6):39-42. [7] 徐建平.四硼酸锂坩埚内预氧化熔融制样-X-射线荧光光谱法测定锰铁及锰硅合金中的硅、锰、磷[J].理化检验(化学分册)(Physical Testing and Chemical Analysis Part B:Chemical Analysis),2016,52(11):1344-1346. [8] 卓尚军.硼酸盐熔融的物理与化学[M].上海:华东理工大学出版社,2006. [9] ISO 12677—2011 Chemical analysis of refractory products by XRF-fused cast bead methods[S]. [10] 梁钰.X射线荧光光谱分析基础[M].北京:科学出版社,2007.
