当前应用X射线荧光光谱熔片制样技术分析测定较低含量、低荧光产额氟组分时,准确度较低,精密度较差、检出限较高。本文运用5:1较低稀释比熔样制片技术,采用波长色散X射线荧光光谱法测定磷矿石中11个主次量组分(F、Na2O、MgO、A12O3、SiO2、P2O5、K2O、CaO、TiO2、MnO、TFe2O3)和1个痕量组分(SrO)。采用磷矿石、岩石国家一级标准物质、磷矿石管理样品和人工配制标准样品校准,经验系数法进行基体校正,结果表明12个组分分析方法的精密度和准确度较好,检出限较低,未知样品的分析结果比较满意;氟的精密度、准确度和检出限均好于文献中10:1熔样稀释比得出的结果。该方法解决了压片制样测定氟组分,熔片制样测定其他主次量组分的技术问题,同时也降低了熔片制样技术测定氟的检出限。
The accuracy and precision are lower, and the detection limit is higher for the determination of F with low content and low fluorescence yield by using X-ray Fluorescence Spectrometry combined with lower dilution ratio fused bead samples preparation. In this paper a method has been reported for the determination of 11 major, minor elements (F, Na20, MgO, A1203, SiO2, P205, K20, CaO, TiO2, MnO, TFe203) and 1 trace element (SrO) in phosphate ores by wavelength dispersive X-ray Fluorescence Spectrometry. A lower-dilution ratio (5 : 1 reagent to sample) fused bead sample preparation mix was used for measurements. Chinese National Standard Materials with similar matrix elemental compositions to the samples were used to calibrate the matrix effect with the experience coefficient method. Results show that precision and accuracy of the method are greatly improved for 12 components, with lower detection limits and satisfactory results for unknown samples. Especially, precision, accuracy and detection limit of F were better than the analytical results in literature and were obtained by using a 10 : 1 fused dilution ratio. Meanwhile, this method solved the technological problem by determining the F component using a pressed pellet sample, and other major and minor components by using fused bead pellet samples. The detection limit of F was also lowered by using this method.