Abstract：During the determination of major and minor components in fluorite by X-ray fluorescence spectrometry (XRF), the accurate determination of fluorine content is a problem that should be solved. The sample was prepared by fusion sample preparation method with sodium nitrate as oxidizing agent and anhydrous lithium tetraborate-lithium carbonate as mixed flux. The accurate determination of each component in fluorite was realized by XRF. The influence of fusion temperature, dilution ratio and fusion time on the determination of fluorine content was investigated to obtain the optimal experimental conditions. The results showed that the loss of fluorine and sulfur was lowest and the fluorescence intensity of fluorine was highest under the following conditions: the mass ratio of anhydrous lithium tetraborate and sample was 4:1; the mass of sodium carbonate and sodium nitrate was 0.500 0 g, respectively; the fusion temperature was 980 ℃; the fusion time was 8 min. Under the optimal experimental conditions, the linear correlation coefficients of calibration curves for calcium fluoride, silicon dioxide, sulfur and phosphorus were all higher than 0.995. The precision test was conducted with certified reference material of fluorite. The relative standard deviation (RSD, n=11) of calcium fluoride, phosphorus, silicon dioxide and sulfur was 0.31%, 3.6%, 0.72% and 0.92%, respectively. The experimental method was applied to the determination of certified reference material and actual sample of fluorite. The results were consistent with the certified values or those obtained by wet method. The proposed method could meet the requirements of routine testing.
吴超超, 马秀艳, 邢文青, 林丽芳, 李世晶. 熔融制样-X射线荧光光谱法测定萤石中主次成分[J]. 冶金分析, 2017, 37(4): 42-47.
WU Chao-chao, MA Xiu-yan, XING Wen-qing, LIN Li-fang, LI Shi-jing. Determination of major and minor components in fluoriteby X-ray fluorescence spectrometry with fusion sample preparation. , 2017, 37(4): 42-47.
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