Fired pressed pellet as a sample preparation technique of choice for an energy dispersive X-ray fluorescence analysis of raw clays

• Published in: Talanta (Oxford) 2023-01, Vol.252, p.123844-123844, Article 123844
• Main Authors: Mijatović, Nevenka, Vasić, Milica, Miličić, Ljiljana, Radomirović, Milena, Radojević, Zagorka
• Format: Article
• Language: English
• Subjects: calibration; Chemical analysis; clay; detection limit; EDXRF; energy-dispersive X-ray analysis; Raw clays; Sample preparation; X-ray fluorescence spectroscopy
• ISSN: 0039-9140; 1873-3573
• DOI: 10.1016/j.talanta.2022.123844

In this paper, the main subject concerns comparing different techniques to prepare raw clay samples for energy-dispersive X-ray fluorescence spectrometry (EDXRF). Three kinds of sample preparation procedures are examined, such as loose powder, pressed pellet, and fired pressed pellet. The fired pressed pellet approach was observed as a part of universal sample preparation for physic, mechanical, and instrumental analysis, which has not been previously tested as a solution in chemical analysis by the EDXRF method. The observed sample preparation techniques were compared by calculating the parameters of validation (recoveries, limit of detection - LOD, limit of quantification - LOQ, precision, and expanded uncertainties of measurements) of 11 elements (Si, Al, Fe, Ca, Mg, K, Na, Ti, P, Mn, and S) using 15 certified reference materials (CRMs). Calibration curves were created and evaluated using 30 reference materials (RM) for all three approaches. Results proved that the fired pressed pellet is the most practical and precise approach for sample preparation of raw clays. [Display omitted] •Validation of sample preparation methods for an energy dispersive X-ray fluorescence analysis of raw clays.•Fired pressed pellet developed here appeared to be of the most precise recoveries compared to the other two approaches loose powder and pressed pellet with wax.•Fired pressed pellet is also suitable for testing other important properties of the samples after the firing process.