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利用高温熔融制备硅石、硅砖样品,应用X射线荧光光谱法测定硅石、硅砖中SiO2、A12O3、CaO、MgO、Fe2O3等主次成分的百分含量。通过国家标准物质和合成校准样品制作校准曲线,研究了熔剂的选择及其与样品的稀释比例,脱膜剂加入量对制样重现性的影响,探讨了采用差量法计算所得的结果的准确性。试验结果表明:该方法的测定值与标准认定值一致,相对标准偏差小于5%,满足了硅石中常见组分快速分析的要求。
Silica and silica brick samples were prepared by high temperature melting, and the percentages of the major and minor components such as SiO2, A12O3, CaO, MgO and Fe2O3 in silica and silica brick were determined by X-ray fluorescence spectrometry. Through the calibration curve of national standard material and synthetic calibration sample, the choice of flux, the ratio of dilution to the sample and the influence of the amount of release agent on the reproducibility of the sample preparation were studied. The results obtained by the difference method accuracy. The test results show that the method has the same determination value as the standard, the relative standard deviation is less than 5%, which meets the requirements of rapid analysis of common components in silica.