在X射线荧光光谱法分析碳酸盐时,采用了两种样片的制法,即熔融法和超细粉末压片法,并对此两种方法进行了比较研究。结果表明:在所测定的15种组分中,采用超细粉末压片法所制样品的分析结果,其检出限有较大的改善,这是由于样品在制备过程中未被稀释;对测定的精密度而言,虽然在主、次组分方面不如熔融法好,但对于痕量组分,则超细粉末压片法占优。此外,在超细粉末压片制样过程中不存在二氧化碳的逃逸,而且粒度效应也基本消除,因此可定量测定碳酸盐中二氧化碳的含量。

In the XRFS analysis of carbonates, a comparative study was made between the methods of preparation of sample discs by the fusion method and by the method of pressure-disking of super-fines (PDSF) in 3 aspects. As shown by the results: ① in the determination of 15 components in carbonate samples, values of detection limits were significantly improved with sample disc prepared by PDSF since no dilution of sample by additives was encountered; ② although higher precision of analytical results of major and minor components were obtained for sample disc prepared by the fusion method, but better precision of results was obtained for trace constituents with sample disc prepared by the PDSF method; and ③ as no escaping of CO2 was observed and the particls size effect was eliminated in the process of PDSF, quantitative determination of CO2 in carbonates was realized by using sample disc thus prepared.