Determination of fifteen components in siliceous, aluminum, magnesia and chrome refractory materials by X-ray fluorescence spectrometry with fusion sample preparation
CUI Hong-li
Tangshan Jianlong Special Steel Co., Ltd., Tangshan 064200, China
Abstract：The analysis of MgO, Na2O, Fe2O3, MnO, Cr2O3, TiO2, P2O5, SiO2, CaO, K2O, Al2O3 in siliceous, aluminum, magnesia and chrome refractory materials usually adopts EDTA titration method, spectrophotometry and flame atomic absorption spectrometry. However, these methods are cumbersome and time-consuming. On the other hand, if X-ray fluorescence spectrometry is employed, different fusion methods and calibration curves are required for four kinds of refractory materials. In order to unify the sample preparation method of four kinds of refractory materials and simultaneously determine the major and minor components (i.e., MgO, ZrO2, Na2O, ZnO, NiO, Fe2O3, MnO, Cr2O3, V2O5, TiO2, P2O5, SiO2, CaO, K2O, Al2O3) using the same set of calibration curves, three sets of foreign standard sample of refractory material were selected to optimize the fusion sample preparation conditions such as melting temperature, time and dilution ratio. The voltage, current, collimator and other conditions of each element were obtained by peak position and intensity scanning to achieve the best sensitivity and resolution. The pulse width was determined by scanning PHA to improve the accuracy. The theoretical α coefficient was used to correct the absorption enhancement effect among elements. The proportional method was adopted to calculate and calibrate the overlapping of spectral lines, thus optimizing the calibration curve and improving the accuracy of analysis method. The linear correlation coefficients (R2) of calibration curves of components were between 0.9940 and 0.9999. Three standard samples (JRRM507, JRRM803 and JRRM129) were fused and determined according to the experimental method. The precision tests of method and melt bead were conducted. The results showed that the repeatability could meet the requirements of GB/T 21114-2007. The correctness verification was performed using three kinds of standard substances (i.e., magnesia-chrome ore, kaolin and bauxite) according to the experimental method. The determination results of major and minor components (including MgO, ZrO2, Na2O, ZnO, NiO, Fe2O3, MnO, Cr2O3, V2O5, TiO2, P2O5, SiO2, CaO, K2O, Al2O3) in standard substances (VS P14/3, UNS KK and ZBK394) were consistent with the certified values.
宋祖峰,阚斌,陈健.镁铝铬质耐火材料的X射线荧光光谱分析[J].理化检验:化学分册,2005,41(9):648-650.SONG Zu-feng,KAN Bin,CHEN Jian.X-ray fluorescence spectrum analysis of magnesium aluminum chromium refractories[J].Physical Testing and Chemical Analysis Part B:Chemical Analysis,2005,41(9):648-650.
[8]
唐红霞,付宝荣.X射线荧光光谱法测定镁质耐火材料中多元素[J].甘肃冶金,2011,33(6):91-93.TANG Hong-xia,FU Bao-rong.Determination of multi-elements in magnesia refractories by X-ray fluorescence spectrometry[J].Gansu Metallurg,2011,33(6):91-93.
[9]
宋霞,张少文,张军.X荧光光谱分析法测定含铬不定形耐火材料[J].光谱学与光谱分析,2011,31(10):2851-2855.SONG Xia,ZHANG Shao-wen,ZHANG Jun.X-ray fluorescence spectrometric determination of chromium-containing amorphous refractories[J].Spectroscopy and Spectral Analysis,2011,31(10):2851-2855.
[10]
罗立强,詹秀春,李国会.X射线荧光光谱仪[M].北京:化学工业出版社,2007:157-159.
[11]
Birks L S.X射线光谱分析[M].高新华,译.北京:冶金工业出版社,1973:159-161.
