Determination of major and minor components in rutile by X-ray fluorescence spectrometry with fusion sample preparation
HUANG Kang1, LI Zhong-xia2, ZHU Wen-jing2, LIU Er-qing2
1. Testing Center of Tianshui Institute of Mineral Exploration of Gansu Nonferrous Metals Geological Survey Bureau, Tianshui 741025, China; 2. Testing Center of Hebei Institute of Regional Geological Survey, Langfang 065000, China
Abstract:During the evaluation of rutile grade, the contents of major and minor components in rutile should be determined. The content of titanium dioxide in rutile sample was usually very high. Moreover, it belonged to refractory compound. Thus, the fused bead was easily broken and burst during the determination of rutile by X-ray fluorescence spectrometry (XRF) with fusion sample preparation. The dilution ratio and fusion temperature were optimized in experiments. The rutile fused bead was successfully prepared by adding suitable amount of glass molding agent SiO2. Then, the determination of major and minor components (including Fe2O3, TiO2, MnO, SiO2, Al2O3, CaO, MgO, K2O) in rutile by XRF was realized. The standard sample of ilmenite, the certified reference material of gabbro and titanium dioxide of high purity reagent were ground and uniformly mixed in a certain proportion to prepare 10 rutile synthetic samples with certain content gradients. Then the calibration curves were drown. The correction of matrix effect and spectral overlapping were carried out with mathematical correction formula. The correlation coefficients of calibration curves of major and minor components were all greater than 0.9979. The contents of major and minor components in rutile synthetic sample (which was prepared by proportional mixing of ilmenite standard sample and titanium dioxide of high purity reagent) were determined according to the experimental method. The relative standard deviations (RSD) of determination results were between 0.22% and 1.6%. Two rutile synthetic samples (which were prepared by proportional mixing of ilmenite standard sample and titanium dioxide of high purity reagent) were determined according to the experimental method. The determination results for the major and minor components were in good agreement with the theoretical values (calculated based on the certified values of standard samples).
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HUANG Kang, LI Zhong-xia, ZHU Wen-jing, LIU Er-qing. Determination of major and minor components in rutile by X-ray fluorescence spectrometry with fusion sample preparation. , 2020, 40(3): 68-72.
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