Usefulness of a Dual Macro- and Micro-Energy-Dispersive X-Ray Fluorescence Spectrometer to Develop Quantitative Methodologies for Historic Mortar and Related Materials Characterization

Abstract

Wavelength dispersive X-ray fluorescence (WD-XRF) spectrometry has been widely used for elemental quantification of mortars and cements. In this kind of instrument, samples are usually prepared as pellets or fused beads and the whole volume of sample is measured at once. In this work, the usefulness of a dual energy dispersive X-ray fluorescence spectrometer (ED-XRF), working at two lateral resolutions (1 mm and 25 μm) for macro and microanalysis respectively, to develop quantitative methods for the elemental characterization of mortars and concretes is demonstrated. A crucial step before developing any quantitative method with this kind of spectrometers is to verify the homogeneity of the standards at these two lateral resolutions. This new ED-XRF quantitative method also demonstrated the importance of matrix effects in the accuracy of the results being necessary to use Certified Reference Materials as standards. The results obtained with the ED-XRF quantitative method were compared with the ones obtained with two WD-XRF quantitative methods employing two different sample preparation strategies (pellets and fused beads). The selected ED-XRF and both WD-XRF quantitative methods were applied to the analysis of real mortars. The accuracy of the ED-XRF results turn out to be similar to the one achieved by WD-XRF, except for the lightest elements (Na and Mg). The results described in this work proved that μ-ED-XRF spectrometers can be used not only for acquiring high resolution elemental map distributions, but also to perform accurate quantitative studies avoiding the use of more sophisticated WD-XRF systems or the acid extraction/alkaline fusion required as destructive pretreatment in Inductively coupled plasma mass spectrometry based procedures.

Risk assessment of radioactive hazards associated with black sand upgrading processes

“…X-ray fluorescence (XRF) Spectrometer (S-8 Tiger Bruker, Germany) was used to define the chemical composition of the studied samples (García-Florentino et al 2018).…”

The Colors of the Circus Mosaic from Barcino (Roman Barcelona): Characterization, Provenance, and Technology Issues

“…Small chips of the three glass tesserae were subjected to macro-and micro-EDXRF analyses to obtain compositional data including trace elements. The dual macro-and micro-EDXRF approach has been proven to be useful for archaeometric characterization [27]. The macro-EDXRF measurements were done by using a touch control S2 Ranger EDXRF system (Bruker AXS GmbH, Karlsruhe, Germany) with a Pd X-ray tube and XFlash ® Silicon Drift Detector (SDD, Peltier cooling at −50 • C, with 128 eV of resolution) (Bruker AXS GmbH, Karlruhe, Germany).…”

Evaluation of compositional micro-homogeneity in MOX fuels using lab based μ-XRF spectrometry

“…m-XRF has been widely used for analysis of geological, biological, environmental, archaeological, and forensic samples. [20][21][22][23][24] But this technique is still under-utilized for analysis and imaging of nuclear materials. Only a few literature reports on the application of m-XRF for nuclear materials are available.…”