Determination of aluminum oxide, magnesium oxide and silicon oxide in alumina-magnesia spinel by energy dispersive X-ray fluorescence spectrometry with fusion sample preparation
HU Zheng-yang, LUO Qi-sheng, ZHANG Song-lin, WANG De-jun
R & D Institute of Raitai-Masteel New Material Technology Co., Ltd., Maanshan 243000, China
Abstract：The analysis of alumina-magnesia spinel in standards mainly adopted wet method or wavelength dispersion X-ray fluorescence spectrometry. With the rapid development of energy dispersive X-ray fluorescence spectrometer (EDXRF), it has been widely used for the elemental analysis in many industries. A determination method of Al2O3, MgO and SiO2 in alumina-magnesia spinel by EDXRF with fusion sample preparation was established. Since there were no ready-made certified reference materials (CRMs) of alumina-magnesia spinel, proper CRMs such as special bauxite and high-purity magnesia were selected in experiments. Meanwhile, a series of calibration samples were synthesized with special bauxite CRM and high-purity magnesia CRM, as well as aluminum oxide primary standard and high purity magnesia CRM according to the production process of alumina-magnesia spinel. When the sample mass as was fixed at 0.5000g, the dilution ratio of sample to anhydrous lithium tetraborate (Li2B4O7) flux was 1∶16, and four drops of 0.5g/mL NH4Br solution was used as the releasing reagent, the melting effect of sample was good at 1150℃. The calibration curves were prepared with the selected CRMs and calibration sample. The root-mean-square (RMS) of calibration curves for Al2O3, MgO and SiO2 were 0.916, 0.888 and 0.029, respectively. The precision test was conducted with the CRMs of magnesia-alumina brick. The relative standard deviation (RSD, n=5) of determination results for Al2O3, MgO and SiO2 were 1.4%, 0.42% and 3.1%, respectively. The CRMs of magnesia-alumina brick and alumina-magnesia refractory as well as alumina-magnesia spinel actual sample were analyzed according to the experimental method. The results of Al2O3, MgO and SiO2 were basically consistent with the certified values or those obtained by the wet method. The proposed method could meet the requirements of production inspection.
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HU Zheng-yang, LUO Qi-sheng, ZHANG Song-lin, WANG De-jun. Determination of aluminum oxide, magnesium oxide and silicon oxide in alumina-magnesia spinel by energy dispersive X-ray fluorescence spectrometry with fusion sample preparation. , 2019, 39(3): 33-37.
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