Determination of 11 major and minor elements in rare earth ferrosilicon by X-ray fluorescence spectrometry with fusion sample preparation
WAN Mang1, LIU Wei2, ZENG Xiaoping1
1. Analytical & Testing Center,South China University of Technology,Guangzhou 510641, China; 2. Technology Center of Shanxi Taigang Stainless Steel Co.,Ltd.,Taiyuan 030003, China
Abstract：During the determination of silicon, manganese, aluminum, iron, titanium and lanthanide-series elements in rare earth ferrosilicon by X-ray fluorescence spectrometry (XRF), the oxidation conditions in the process of fusion sample preparation are not easily controlled. It is easy to cause the phenomenon of premature melting of the wall hanging crucible or poor wall hanging of the crucible, which will seriously erode the platinum-gold crucible. In the experiment, lithium tetraborate was used as the flux on the bottom of platinum-gold crucible for protection. The rare earth ferrosilicon samples were sintered and oxidized with lithium carbonate. Then sodium peroxide was used for deep oxidation, which solved the corrosion problem of platinum-gold crucible by rare earth ferrosilicon sample. The mass ratio of sample to lithium tetraborate flux was 1∶30. After fusion at 1 100 ℃ for 12 min, the prepared glass sheets had good surface quality, which effectively eliminated the influence of grain-size effect and mineral effect. 11 major and minor elements (including silicon,manganese,aluminum,calcium,iron,titanium,lanthanum,cerium,praseodymium, neodymium and samarium) in rare earth ferrosilicon were determined according to the experimental method. The relative standard deviations (RSD, n=10) of the determination results were between 0.39% and 5.0%, and the results were in good agreement with those obtained by standard method and titration method. The proposed method could meet the detection requirements of the major and minor elements in rare earth ferrosilicon.
万芒, 刘伟, 曾小平. 熔融制样-X射线荧光光谱法测定稀土硅铁中11种主次元素[J]. 冶金分析, 2023, 43(1): 54-61.
WAN Mang, LIU Wei, ZENG Xiaoping. Determination of 11 major and minor elements in rare earth ferrosilicon by X-ray fluorescence spectrometry with fusion sample preparation. , 2023, 43(1): 54-61.
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