Determination of major and minor components in refractories containing aluminum,chromium and zirconium by X-ray fluorescence spectrometry with fusion sample preparation
REN Guotao, DENG Junjie, LI Tingting, HAN Jingjing, LI Qingqing, ZHANG Lixin
Sinosteel Luonai Materials Technology Corporation, Luoyang 471039, China
Abstract：For the analysis of chemical composition of new refractory materials containing aluminum, chromium and zirconium, there is currently no matching certified reference materials(CRMs) and suitable X-ray fluorescence spectrometry (XRF) analysis methods in the industry. The traditional wet method is still used, which is cumbersome to operate with poor sensitivity for minor components with low content. In experiments, nine calibration samples series with different concentration gradients were prepared based on existing CRMs of aluminum-zirconium-silicon (JRRM708, JRRM710) and vanadine (JRRM310) by adding primary reagents of chromium oxide and zirconium oxide. 0.2 g of each calibration sample was mixed with flux [m(Li2B4O7)∶m(LiBO2)∶m(LiF)=65∶25∶10]. The dilution ratio was 1∶30. The melting temperature was 1 100℃. 200 g/L ammonium bromide solution was used as release agent. The analysis method of major and minor components in refractories containing aluminum, chromium and zirconium by XRF was established with 45 kV-75 mA as the excitation conditions. The correlation coefficients of major components were not less than 0.999. The limits of detection of minor components were not more than 0.014%. The precision test indicated that the relative standard deviations (RSD,n=6) of all components were less than 1% besides 1.4% for silica with low content. The conventional samples of refractories containing aluminum, chromium and zirconium were analyzed according to the experimental method, and the found results were consistent with those obtained by the chemical wet method. The proposed method could meet the XRF analysis requirements of new refractory materials containing aluminum, chromium and zirconium.
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REN Guotao, DENG Junjie, LI Tingting, HAN Jingjing, LI Qingqing, ZHANG Lixin. Determination of major and minor components in refractories containing aluminum,chromium and zirconium by X-ray fluorescence spectrometry with fusion sample preparation. , 2021, 41(4): 68-72.
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