Synchrotron‐induced EDXRF determination of uranium and thorium in mixed uranium–thorium oxide pellets

Abstract

Uranium and thorium in their mixed oxides were determined by synchrotron-induced energy dispersive X-ray fluorescence (EDXRF) spectrometry. Mixed oxide calibration mixtures containing uranium and thorium in different relative amounts and approximately fixed amount of yttrium were prepared in the form of pellets. The EDXRF spectra of the pellets were measured at the microfocus XRF (BL-16) beam line of Indus-2 synchrotron radiation facility (Raja Ramanna Centre of Advanced Technology, Indore, India). Characteristic X-ray lines U La, Th La, and Y Ka were used as analyte lines. Calibration plot for the determination of uranium was prepared by plotting amount ratios of U and Y against the intensity ratios of U La and Y Ka. Similarly, a calibration plot for thorium analysis was also made. The amounts of uranium and thorium in the sample mixtures prepared in similar way as the calibration mixtures were determined using the aforementioned calibration plots. The precision values obtained for uranium and thorium determinations were found to be 0.3 and 0.2% (relative standard deviation, 1s), respectively. The EDXRF results deviated from the expected values by 1% for uranium and 0.9% for thorium determinations. These analytical features are much superior compared with laboratory-based analysis results.

A green analytical approach for the direct non-destructive compositional analysis of (Th, U)O2 fuel pellets by the X-Ray Fluorescence technique using single universal calibration

“…This is the major advantage over the previously reported EDXRF-based technique for the direct compositional analysis of MOX fuel pellets, where different matrix-matched standards are required for different types of samples. 13,32…”

“…10,11 There are some reports in the literature where these EDXRF and WDXRF techniques have been utilized for the compositional analysis of MOX fuel pellets. 9,12–14 However, these techniques require matrix-matched calibration standards due to the presence of severe matrix effects in XRF geometry. The calibration process itself is time-consuming.…”

Exploring Actinide Materials Through Synchrotron Radiation Techniques

“…Though focused beam decreases intensity of incident light, the high flux and brilliance of synchrotron radiation can still ensure enough photo­ns are incident on samples and subsequently results in high sensitivity as well as high spatial resolution. The research on determinating amounts of uranium and thorium in their mixed oxides by Misra et al at SR‐μ‐XRF beam line of Indus‐2 synchrotron radiation facility in India, gave precision values of 0.3% and 0.2% and deviation of 1% and 0.9% from the expected values respectively for uranium and thorium, which is much better than conventional XRF results. Sensitivity of SR‐μ‐XRF is also superior to nuclear spectroscopy.…”

A microfocus X-ray fluorescence beamline at Indus-2 synchrotron radiation facility

“…The BL-16 beamline has been used for microfluorescence measurements of a variety of heterogeneous multi-element samples (Misra et al, 2013). In a case study, the microfluorescence mapping capabilities of the beamline have been examined by analyzing a Cu grid structure.…”