Abstract：According to the standard method of GB/T 4984-2007, the determination of major and minor components in zircon-containing refractory requires the combination of several methods. The operation was relatively complex and time-consuming. Two synthetic samples were prepared by certified reference materials of zirconize refractory special for X-ray fluorescence spectrometry (XRF) analysis by Technical Association of Refractories of Japan (TARJ) as well as primary reagent of ZrO2. Twelve glass sheets of CRMs/calibration samples were prepared with the series of CRMs and synthetic samples. Thus, an analysis method was established for determination of eleven major and minor components in zirconize refractory (ZrO2, HfO2, Cr2O3, MgO, CaO, SiO2, Al2O3, Fe2O3, TiO2, K2O, and Na2O) by XRF. The results showed that the prepared sheets were uniform and smooth to meet the requirements for test under the following experimental conditions: the sample mass was 0.400 0 g; the mix flux of Li2B4O7-LiBO2 (m∶m=12∶22) was used; the dilution ratio was 1∶15; 0.2 mL of 300 g/L NH4I solution was used as release agent; the sample was melted at 1 050 ℃ for 15 min. ZrLɑ and HfLβ1 lines were selected as the analytical lines to overcome the influence of excessive fluorescence intensity of ZrKɑ line. The spectral interference was eliminated by spectral line correction. The matrix effect was corrected by empirical α coefficient method to eliminate the absorption enhancement effect of each element in the sample. The precision quality factor of calibration curve was less than 0.07. The limits of detection of test components were between 0.007% and 0.024%. The zirconize refractory samples were determined according to the experimental method. The relative standard deviations (RSD) of determination results were between 0.24% and 4.9%. The synthetic samples, which were prepared with series of CRMs special for X-ray fluorescence spectrometry (XRF) analysis and primary reagent of ZrO2, were determined by the proposed method and standard method of GB/T 4984-2007 or GB/T 6900-2016. The determination results were consistent with those obtained by standard methods. The errors between the determination results and reference values were within the allowable ranges in standard methods.
王志彪, 关海兰. 熔融制样-X射线荧光光谱法测定锆质耐火材料中11种主次组分[J]. 冶金分析, 2022, 42(3): 78-83.
WANG Zhibiao, GUAN Hailan. Determination of eleven major and minor components in zirconize refractory by X-ray fluorescence spectrometry with fusion sample preparation. , 2022, 42(3): 78-83.
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