Institute for Testing of Materials IMS, Bulevar Vojvode Mišića 43, 11000, Belgrade, Serbia.
Institute for Testing of Materials IMS, Bulevar Vojvode Mišića 43, 11000, Belgrade, Serbia.
Talanta. 2023 Jan 15;252:123844. doi: 10.1016/j.talanta.2022.123844. Epub 2022 Aug 18.
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.
本文主要研究了为能量色散 X 射线荧光光谱法（EDXRF）制备生粘土样品的不同技术。考察了三种样品制备程序，例如松散粉末、压片和烧制压片。烧制压片方法被观察为物理、机械和仪器分析的通用样品制备方法的一部分，以前未曾在 EDXRF 方法的化学分析中作为解决方案进行过测试。通过使用 15 个认证参考材料（CRM）计算 11 种元素（Si、Al、Fe、Ca、Mg、K、Na、Ti、P、Mn 和 S）的验证参数（回收率、检出限-LOD、定量限-LOQ、精密度和测量扩展不确定度），对观察到的样品制备技术进行了比较。为所有三种方法都创建和评估了校准曲线。结果表明，烧制压片是生粘土样品制备最实用和精确的方法。
