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采用偏硼酸锂熔融制样的方法,建立了白炭黑中二氧化硅、三氧化二铝、氧化钠、氧化钾、三氧化二铁、氧化钙、氧化镁、二氧化钛、氧化锰的X射线荧光光谱分析方法。熔融实验结果表明,以碘化铵作为脱模剂,熔剂和样品质量比为5∶1,在1 100℃下熔融10 min可得到较好的熔样效果。选用与白炭黑基体类似的硅质砂岩标准物质,同时将其与光谱纯二氧化硅按不同比例混合配制成组分含量有一定梯度的校准样品,有效地解决了白炭黑XRF测定的校准样品缺失的问题,并采用变化的理论α影响系数法对基体效应进行了考察。精密度实验结果表明,各组分的相对标准偏差(RSD,n=11)在0.33%~7.71%。用本方法对实际样品中上述成分进行测定,与湿法化学分析法结果一致。
Using lithium metaborate melting sample preparation method, the silica has been established silica, aluminum oxide, sodium oxide, potassium oxide, ferric oxide, calcium oxide, magnesium oxide, titanium dioxide, manganese oxide X-ray fluorescence Spectral analysis method. The results of melting experiments show that the better melting result is obtained when the mass ratio of flux to sample is 5: 1 with ammonium iodide as mold release agent and melted at 1 100 ℃ for 10 min. The silica sandstone standard material which is similar to the silica body is selected and mixed with the spectrum pure silica in different proportions to prepare a calibration sample with a certain gradient of the component content so as to effectively solve the calibration of the XRF measurement of the silica Sample missing problems, and the use of changes in theoretical α influence coefficient method to examine the matrix effect. The results of precision experiments showed that the relative standard deviations (RSD, n = 11) of the components ranged from 0.33% to 7.71%. The method used in the actual sample of the above ingredients were measured, consistent with the results of wet chemical analysis.