Determination of major and minor components in phosphate ore by X-ray fluorescence spectrometry with fusion sample preparation
SHI You-chang1,LI Guo-hui*2,LI Zhi-xiong1,ZHAO Gang1,LI Ke-yong1,LIU Shuai1
1.Golden 10 Unit of CAPF,Kunming 650100,China; 2.Institute of Geophysical and Geochemical Exploration,Chinese Academy of Geological Sciences,Langfang 065000,China
Abstract：Phosphate ore is a kind of non-renewable resource, and the associated fluorine also has high value in use. The determination of hardly volatile components in phosphate ore by X-ray fluorescence spectrometry(XRF) after fusion sample preparation has high precision and good accuracy. However, the component fluorine is easily volatilized at high temperature and the detection limit is relatively high. The high temperature volatilization characteristics of fluorine were focused on in the study. The analysis method of 12 components in phosphate ore (including P2O5, F, SiO2, Al2O3, Fe2O3, MgO, CaO, Na2O, K2O, TiO2, MnO and SrO) by X-ray fluorescence spectrometry with fusion sample preparation was established. The analytical conditions were obtained by experiments: the dilution ratio was 1∶15, the pre-oxidation temperature was 700 °C, the sample fusion temperature was 1 050 ℃, and the fusion time was 4 min. F, MgO and K2O belonged to rock-forming light components, and the matrix correction was not necessary; Rhα-c was selected as the internal standard for SrO; the matrix effect on P2O5, SiO2, Al2O3, Fe2O3, CaO, Na2O, TiO2 and MnO was corrected by theoretical coefficient method. The detection limits of method were between 0.000 2% and 0.042%. Particularly, the detection limit of fluorine was 0.042%. The precision of method was investigated using GBW07210 and GBW07212. The relative standard deviations (RSD, n=12) of components were between 0.07% and 5.1%. The national standard sample and synthetic standard samples of phosphate ore were determine according to the experimental method, and the found results were consistent with the certified values of theoretical values.
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