熔融制样-X射线荧光光谱法测定黑刚玉中6种组分

黑刚玉是一种以Al₂O₃、SiO₂和TiO₂为主要成分的新型环保材料,其化学成分的分析一般采用滴定法、分光光度法或原子吸收光谱法等,这些方法操作相对繁琐、流程长。实验采用H₃BO₃-Li₂CO₃ 混合熔剂(m∶m＝7∶3)按质量比为1∶10的稀释比进行熔融制样,加入0.15 g NH₄I脱模剂,有效地消除了矿物效应、粒度效应。实验选择矾土、黏土、焦宝石等与黑刚玉组分相似的标准物质和人工合成校准样品建立校准曲线,各组分校准曲线的相关系数均大于0.998,实现了熔融制样-X射线荧光光谱法对黑刚玉中Al₂O₃、SiO₂、Fe₂O₃、TiO₂、CaO和MgO含量的同时测定。对黑刚玉样品进行准确度考察,实验方法的测定值与其他方法的测定值吻合较好,各组分测定结果的相对标准偏差(RSD)均小于2.0%。

Determination of six components in black corundum by X-ray fluorescence spectrometry with fusion sample preparation

The black corundum is a kind of new environmental protection material with aluminum oxide, silicon oxide and titanium oxide as the main components. The chemical composition of black corundum is generally analyzed by titration method, spectrophotometry or atomic absorption spectrometry. These methods are relatively cumbersome with long process. In the experiments, H₃BO₃-Li₂CO₃ mixed flux (m∶m=7∶3) was used to melt the sample according to the mass ratio of 1∶10. In sample preparation, 0.15 g of NH₄I was added as the release agent. The mineral effect and granularity effect were effectively eliminated. The calibration curve was drawn using the artificially synthesized calibration samples and standard materials of bauxite, clay and scorched gemstone, which had similar components to the black corundum. The correlation coefficients of calibration curves were all higher than 0.998. The simultaneous determination of Al₂O₃, SiO₂, Fe₂O₃, TiO₂, Cao and MgO in black corundum by X-ray fluorescence spectrometry (XRF) with fusion sample preparation was realized. The accuracy tests of black corundum sample were conducted. The found results of proposed method were in good agreement with those obtained by other methods. The relative standard deviations (RSD) of determination results were all less than 2.0%.