Betterment in EDXRF analytical results for compositional characterization of mixed uranium thorium oxide samples with bead specimens compared with pressed pellet specimens

Abstract

A comparative study on the energy dispersive X‐ray fluorescence analytical results of uranium determinations, in uranium and uranium–thorium mixed oxides, using specimens in the form of fused beads and pressed pellets, has been made. It was observed that in case of fusion bead specimens, the intensity of the analyte lines was approximately 1.6 times of that observed in pellet specimens under identical instrumental conditions. In case of uranium oxide samples, the analytical results with bead specimens were slightly better compared with the pellet specimens. However, in case of the uranium–thorium oxide mixtures, the average precision obtained with bead specimen was significantly better (1%, 1 s) in comparison with that achieved using pellet specimens (7%, 1 s). This difference may be due to the hardness of thorium oxide compared with uranium oxide, which affects the homogeneity of the pellet specimens prepared. In fusion bead method of sample preparation, even highly refractory material like ThO2 forms uniform glass beads. Addition of internal standard further improves the analytical results, with reduction in the percent deviation of energy dispersive X‐ray fluorescence results from the expected values to 3% from 7% compared with that obtained using without internal standard. The fusion bead method of sample preparation will be very useful for characterization of sintered (U,Th)O2 pellets, which are highly refractory and difficult to dissolve. Copyright © 2016 John Wiley & Sons, Ltd.

X-ray Fluorescence Spectroscopy Features of Micro- and Nanoscale Copper and Nickel Particle Compositions

“…As mentioned by the authors [33], the samples' local density and the local densities of the elements that are not detected by the XRF method play an important role in the scattering and secondary enhancement, thus affecting the quantification of the main elements. A similar impact of oxides on the analytical results was described by the authors [39]. The precision of XRF analysis was improved to 1% by fusing the powder samples compared with that of 7% for initial powders.…”

Universal EDXRF Method for Multi-elemental Determinations Using Fused Bead Specimens

“…15 The resultant is a glass bead which is homogeneous, free from particle size effects and is better specimens compared to pellets in terms of the accuracy and precision. 16 In the bead method of sample preparation, the sample-to flux-ratio depends on the nature of the sample, analyte concentration and their fluorescence yield. A small sample-to flux-ratio may result in line intensities of the analyte proportional to the concentration with a very less matrix effect and with a very low signal-to noise-ratio.…”