Determination of major components in magnesium-calcium-iron oxide vibrating material by X-ray fluorescence spectrometry with fusion sample preparation
WANG Zhibiao1,2, LI Xiangwei1,2
1. Yangquan Comprehensive Inspection and Testing Center,Yangquan 045000,China; 2. National Quality Supervision and Inspection Center for Silicon-Aluminum RefractoriesShanxi,Yangquan 045000,China
Abstract：In order to ensure good slag resistance, refractoriness and construction strength of magnesium-calcium-iron oxide vibrating material, the chemical composition should be strictly controlled. The sample prepared at 1 050 ℃ for 15 min by fusion sample preparation with Li2B4O7-LiBO2(m∶m=67∶33) as mixed flux and 300 g/L NH4I solution as release agent. The determination of major components (including SiO2, Al2O3, Fe2O3, CaO and MgO) in magnesium-calcium-iron oxide vibrating material was realized by X-ray fluorescence spectrometry(XRF). On the basis of chemical composition of magnesium-calcium-iron oxide vibrating material, the calibration sample series, which had a certain gradient and a certain content span covering the content ranges of elements in the sample, were prepared by mixing the certified reference materials of magnesia refractory, limestone and bauxite to draw calibration curve. Thus, the problem that there were no certified reference materials for magnesium-calcium-iron oxide vibrating material was overcome. Theoretical α coefficient method was employed for matrix correction, eliminating the absorption enhancement effect among elements. The calibration curves were drawn with the component contents as abscissa and their corresponding fluorescence intensity as ordinate. The precision quality factors of calibration curves of components were K＜0.07, and the limits of detection were in range of 0.012%-0.057 9%. The contents of major components in magnesium-calcium-iron oxide vibrating material samples were determined according to the proposed method. The relative standard deviations (RSD, n=12) of determination results were between 0.12% and 2.6%. The contents of SiO2, Al2O3, Fe2O3, CaO and MgO in 2 magnesium-calcium-iron oxide vibrating material samples were determined according to the proposed method. Meanwhile, standard method of GB/T 5069-2015 was used for method comparison. The results showed that the errors between the proposed method and the standard method were within the allowable ranges specified in standard method of GB/T 5069-2015.
王志彪, 李向威. 熔融制样-X射线荧光光谱法测定镁钙铁质振动料中主量成分[J]. 冶金分析, 2024, 44(9): 66-71.
WANG Zhibiao, LI Xiangwei. Determination of major components in magnesium-calcium-iron oxide vibrating material by X-ray fluorescence spectrometry with fusion sample preparation. , 2024, 44(9): 66-71.
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