Determination of calcium fluoride and silicon dioxide in fluorite by X-ray fluorescence spectrometry with fusion sample preparation
LI Yong1, GU Qiang*2, LIU Hongyan1
1. The Testing Center of Environmental Science and Technology Co., Ltd. No. 1 Bureau of CMGB.,Langfang 065201, China; 2. Technical Center of Handan Iron and Steel Plant,HBIS Group Co.,Ltd.,Handan 056015, China
Abstract：Fluorite is widely used in iron and steel industry as an auxiliary for iron and steel making. The main index to evaluate the quality of fluorite is the content of CaF2 and SiO2. The determination of calcium fluoride in fluorite by X-ray fluorescence spectrometry (XRF) with fusion sample preparation usually adopts two methods, i.e., fluorine spectrum method and calcium spectrum method. If the fluorine spectrum method is used, the determination results are usually higher due to the interference of magnesium fluoride which possibly existed in fluorite. If the calcium spectrum method was used, the determination result is the total amount of calcium, and the component of calcium carbonate should be subtracted, so the method is relatively complicated. Since calcium carbonate in fluorite can be dissolved by dilute acetic acid, while calcium fluoride and silicon dioxide cannot be dissolved, the sample was treated with 10% acetic acid in experiments. The residue was reserved after filtration, realizing the separation of calcium carbonate from the sample. The residue and filter paper were ashed and then fused with lithium tetraborate-lithium metaborate-lithium fluoride (m∶m∶m=65∶25∶10) mixed flux and potassium bromide for sample preparation. The determination of calcium fluoride and silicon dioxide in fluorite by XRF was realized. The experiment results showed that the linear correlation coefficients of calibration curves for calcium fluoride and silicon dioxide were above 0.997. The limit of detection of silicon dioxide of method was 0.089%. The precision of fluorite samples was investigated, and the relative standard deviations (RSD, n=12) of the determination results of calcium fluoride and silicon dioxide were not more than 0.12% and 0.92% respectively. The standard samples and actual samples of fluorite were determined according to the experimental method. The measured results of calcium fluoride and silicon dioxide in standard sample were consistent with the standard values. The measured results of calcium fluoride in actual sample were in good agreement with that obtained by EDTA titration in standard method GB/T 5195.1-2017, and the measured results of silicon dioxide were in good agreement with that obtained by silicon molybdenum blue spectrophotometry in standard method GB/T 5195.8-2017.
李勇, 顾强, 刘洪艳. 熔融制样-X射线荧光光谱法测定萤石中氟化钙和二氧化硅[J]. 冶金分析, 2022, 42(8): 29-34.
LI Yong, GU Qiang, LIU Hongyan. Determination of calcium fluoride and silicon dioxide in fluorite by X-ray fluorescence spectrometry with fusion sample preparation. , 2022, 42(8): 29-34.
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