Abstract：During the analysis of chemical components in ferrosilicon by X-ray fluorescence spectrometry (XRF) with fusion sample preparation, the key technology is the pre-oxidization of sample to prevent Pt-Au crucible from corroding. According to the sintering principle, the ferrosilicon sample reacted with oxidizing agent to form polycrystal. Then the temperature was increased to completely oxidize the ferrosilicon sample. Finally, the sample was fused to prepare bead, which thoroughly solve the corrosion problem of Pt-Au crucible by iron alloy. The influence of experimental conditions including oxidizing agent, sintering temperature and time, and release agent on the sample preparation was discussed. The results showed that the prepared beads were smooth and uniform, which could meet the determination requirements of XRF, under the following conditions: the lithium carbonate was selected as the oxidizing agent; the sintering temperature was 700℃ and the sintering time was 60min; the complete oxidizing temperature was 800℃ and the oxidizing time was 30min; the sample was fusion at 1050℃ for 15min. One certified reference material (CRM) of ferrosilicon was used for precision test. The relative standard deviations (RSD, n=11) of determination results for silicon, manganese, phosphorus, aluminum and calcium were between 0.31% and 2.0%. Four certified reference materials of ferrosilicon were analyzed according to the experimental method, and the found results were consistent with the certified values, which could meet the detection requirements of components in ferrosilicon.
常利民, 祁巍, 王雪红. 烧结熔融制样-X射线荧光光谱法测定硅铁中主次组分[J]. 冶金分析, 2020, 40(1): 51-55.
CHANG Li-min, QI Wei, WANG Xue-hong. Determination of major and minor components in ferrosilicon by X-ray fluorescence spectrometry with sintering and fusion sample preparation. , 2020, 40(1): 51-55.
鲍希波,赵亮,李才红,等.熔融制样-X射线荧光光谱法测定硅锰合金和锰铁合金中硅锰磷铁[J].冶金分析,2019,39(2):51-55.BAO Xi-bo,ZHAO Liang,LI Cai-hong,et al.Determination of silicon,manganese,phosphorus and iron in silicomanganese and ferromanganese alloys by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2019,39(2):51-55.
常利民,祁巍,刘艳辉,等.X-射线荧光光谱法分析铁合金成份的最新进展[J].冶金设备,2019(s1):124-127.CHANG Li-min,QI Wei,LIU Yan-hui,et al.The latest progress in the analysis of ferro-alloy composition by X-ray fluorescence spectrometry[J].Metallurgical Equipment,2019(s1):124-127.
[8]
张祥,陆晓明,张毅,等.熔融制样-X射线荧光光谱法测定中低碳锰铁合金中锰硅磷铁[J].冶金分析,2019,39(10):55-60.ZHANG Xiang,LU Xiao-ming,ZHANG Yi,et al.Determination of manganese,silicon,phosphorus and iron in medium-low carbon ferromanganese alloy by X-ray fluorescence spectrometry with fusion sample preparation[J].Metallurgical Analysis,2019,39(10):55-60.
[9]
果世驹.粉末烧结理论[M].北京:冶金工业出版社,1998.
[10]
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.
[11]
李小莉.熔融制片-X 射线荧光光谱法测定锰矿样品中主次量元素[J].岩矿测试,2007,26(3):238-240.LI Xiao-li.Determination of major and minor elements in manganese ores by X-ray fluorescence spectrometry with fusion sample preparation[J].Rock and Mineral Analysis,2007,26(3):238-240.
