Determination of eight components in magnesium-aluminum refractory materials by X-ray fluorescence spectrometry with fusion sample preparation
LI Xiangwei1,2, WANG Zhibiao1,2, LI Jie1,2
1. Yangquan Comprehensive Inspection and Testing Center,Yangquan 045000, China; 2. National Quality Supervision and Inspection Center for Silicon-Aluminum Refractories(Shanxi), Yangquan 045000, China
Abstract：Magnesium-aluminum refractory materials are widely used in many industries such as steel, cement and glass. At present, GB/T 5069-2015 is commonly used for the chemical analysis of magnesium-aluminum refractory materials in inspection work. However, this method is time-consuming. Since there were few standard samples of magnesium-aluminum refractory materials, the calibration samples were self-made in laboratory using the certified reference materials of magnesia, magnesium-aluminum brick and magnesium stone with different mixing ratios, which overcame the limitations of shortage of the standard samples. The sample was prepared by fusion method. The determination method of major and minor components in magnesium aluminum refractory materials (MgO, CaO, SiO2, Al2O3, Fe2O3, TiO2, K2O, Na2O) by X-ray fluorescence spectrometry (XRF) was established. The conditions for sample fusion were optimized as follows: 6.000 0 g of Li2B4O7 flux and 0.500 0 g of sample were accurately weighed (the dilution ratio of sample was 1∶12); 0.4 mL of 300 g/L NH4Br solution was added and used as release reagent; the mixture was fused at 1 050 ℃ for 10 min. The matrix correction was conducted by empirical α coefficient method through Super Q software to eliminate the absorption enhancement effect of each element in the sample. The standard samples of magnesium-aluminum brick 423 and Al-Mg-mix-2 were determined according to the experimental method. The results showed that the relative standard deviation (RSD) of determination results of all components were between 0.081% and 2.9%. The trueness test could meet the requirements of the standard method.
李向威, 王志彪, 李杰. 熔融制样-X射线荧光光谱法测定镁铝质耐火材料中8种组分[J]. 冶金分析, 2021, 41(8): 43-47.
LI Xiangwei, WANG Zhibiao, LI Jie. Determination of eight components in magnesium-aluminum refractory materials by X-ray fluorescence spectrometry with fusion sample preparation. , 2021, 41(8): 43-47.
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