Abstract：Impurity content is an important basis to evaluate the quality grade of white fused alumina. Therefore, it is of great significance for the accurate and fast determination of impurity content in the white fused alumina. At present, the wet analysis methods are commonly used to determine the content of impurities in white fused alumina. However, these methods are tedious and time-consuming with long analysis cycle, which is not suitable for the bulk inspection. Ethanol was used as adhesive for pressed powder pellet sample preparation by package with polyester (PET) thin film. The calibration samples of white fused alumina with various content gradients of testing components were synthesized using the standard samples of brown fused alumina, white fused alumina, and alumina according to the different proportions. The calibration curves were obtained by fitting. The analysis method for the simultaneous determination of SiO2, CaO, Fe2O3, K2O, Na2O, TiO2 and P2O5 in white fused alumina by X-ray fluorescence spectrometry (XRF) was established. The technical problem of the lack of white fused alumina standard samples was solved by manually configuring standard samples to make the detection range was closer to the impurity content range of white fused alumina. The introduction of PET thin film into the pressed powder pellet for XRF analysis could not only reduce the dust contamination and reduce the probability of instrumental damage to a minimum, but also prevent the sample from being exposed to the air and increase the preservation time of the sample. The sample preparation conditions were determined experimentally as follows: the sample was ground through 400-mesh (38 μm) screen; the pressure of pellet press was 3.0 t; the pressure holding time was 30 s. The build-in TL equations in OXSAS software were adopted for the correction of matrix effect. The linear correlation coefficients of calibration curves were all greater than 0.99. The limits of detection were between 3.7 μg/g and 27 μg/g. The precision was measured with white fused alumina sample. The relative standard deviations (RSD, n=10) of determination results were between 1.7% and 4.5%. The proposed method was applied to the determination of certified reference materials and samples of white fused alumina, and the results were in good agreement with the certified values or those obtained by standard methods in GB/T 3044-2020.
[1] 中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.GB/T 3044—2020 白刚玉、铬刚玉化学分析方法[S].北京:中国标准出版社,2020. [2] 罗湘宁,李友元,吴志华.X射线荧光光谱法测定氧化铝中杂质含量[J].冶金分析,2003,23(5):43-46. LUO Xiangning,LI Youyuan,WU Zhihua.Determina-tion of impurity content in alumina by XRF[J].Metallurgical Analysis,2003,23(5):43-46. [3] 马慧侠,张爱芬.X射线荧光光谱法测定氧化铝中杂质元素[J].理化检验(化学分册),2006,42(12):980-983. MA Huixia,ZHANG Aifen.XRFS determination of impurities in aluminum oxide[J].Physical Testing and Chemical Analysis (Part B:Chemical Analysis),2006,42(12):980-983. [4] Peschel B U,Fittschen U E A,Pepponi G,et al.Direct analysis of Al2O3 powders by total reflection X-ray fluorescence spectrometry[J].Analytical and Bioanalytical Chemistry,2005(382):1958-1964. [5] 白雪,李慧,杨本勇.X射线荧光光谱法测定氧化铝中PdO和La2O3的含量[J].中原工学院学报,2007,18(1):59-60. BAI Xue,LI Hui,YANG Benyong.X-ray fluorescence spectrometry of determining PdO and La2O3 in Al2O3[J].Journal of Zhongyuan University of Technology,2007,18(1):59-60. [6] 张晓平.X-射线荧光光谱直接压片法测定氧化铝中杂质Ga2O3含量[J].轻金属,2011(3):25-26. ZHANG Xiaoping.Direct compression method with X-ray fluorescence spectrometry for measuring Ga2O3 in alumina[J].Light Metals,2011(3):25-26. [7] 张爱芬,刘帅,马慧侠,等.粉末压片X射线荧光光谱法测定氧化铝中杂质元素[J].冶金分析,2012,32(12):51-56. ZHNAG Aifen,LIU Shuai,MA Huixia,et al.Determination of impurity elements in alumina by pressed powder pellet X-ray fluorescence spectrometry[J].Metallurgical Analysis,2012,32(12):51-56. [8] 王永辉,刘珂,曹晓晔.X射线荧光光谱压片法测定白刚玉中微量元素含量[J].广东化工,2017,44(17):173-174. WANG Yonghui,LIU Ke,CAO Xiaoye.Determination of minor elements in white fused alumina by the pressed powder slice X-ray fluorescence spectrometry[J].Guangdong Chemical Industry,2017,44(17):173-174.
