A new Rule of Thumb to evaluate alpha sources prepared by electro precipitation using X-ray Fluorescence

https://doi.org/10.1016/j.apradiso.2020.109555Get rights and content

Highlights

  • XRF is a suitable technique for the characterization of alpha sources in a short time.

  • A Rule of Thumb allows rapid evaluation of alpha-particle sources.

  • Small laboratories will benefit from this method, as the analysis can be performed even with portable devices.

Abstract

This report studies the feasibility of using X-ray Fluorescence for the characterization of alpha sources in a short time and proposes a new Rule of Thumb for the sake of simplicity. An uranium deposit of 0.012 ± 0.001 mg cm−2 which XRF spectrum shows a low intensity U-Lα peak at 13.61 keV, provides good resolution in alpha spectrometry. By this method, long data acquisition times in alpha spectrometry of poorly prepared sources are avoided without the need for expensive equipment.

Introduction

X-ray Fluorescence (XRF) is a non-destructive multi-elemental technique widely used in the study of the composition of feedstock, rocks, soils, clays, cement, cultural heritage objects and in the analysis of biological materials. Thanks to the speed with which an analysis can be performed, quality control of some goods can be carried out in many applications, where immediate results are required.

This study aims to introduce XRF for the evaluation of alpha sources prepared by electro precipitation. In order to obtain good resolution in alpha spectrometry, it is required that just a thin and homogeneous layer of uranium is deposited onto the plate, ideally a thickness of a few atoms, in this way avoiding the interaction between the alpha particles and other materials that leads to energy losses. Many variables are involved in the electro precipitation process, such as the pH of the electrolyte, the salt concentration, the anode shape, the cathode material, the anode rotation, the current density and the deposition time. The discussion about the influence of each variable on the electroplating process is out of the scope of this work, but it can be easily found in literature (Dimitru et al., 2013). Although these parameters can be optimized, the electro precipitation process of uranium from slightly acidic solutions (pH > 2.5) on discs is considered erratic (Saliba-Silva et al., 2014) due to the generation of hydrogen bubbles on the cathode surface that need to be removed in order to form the hydroxyl layer that makes uranium hydroxide and uranium oxide precipitate (Crespo, 2012) . Many investigations are being carried out for improving electro precipitation, including the replacement of metallic substrates by boron-doped diamond, which aims at better peak resolution (Tran et al., 2019). Characterization of alpha sources is extremely helpful for sample preparation, as it allows to accept or reject sources before they go to alpha counting, which usually may take a long time. Several techniques are currently used in the sources characterization, like autoradiography (Jobbagy et al., 2013), Scanning Electron Microscopy/ Energy Dispersive X-ray Spectrometry (SEM/EDS), X-ray Diffraction (XRD), and Raman Spectroscopy (Wilbraham et al., 2015). In this work, we determined that XRF is suitable for the characterization of alpha sources. Over other techniques, it is more accessible, faster and users do not need much training. Furthermore, we have established a smart Rule of Thumb, that allows to make the evaluation of the alpha sources by just taking a glance at the XRF spectrum.

Section snippets

Alpha-particle spectrometer.

A homemade low-cost prototype with PIN Silicon diode detector SS3590-19 (Hamamatsu Photonics K.K., Iwata, Japan) with sensitive area of 10 mm x 10 mm and maximum depletion thickness of 0.3 mm with reversed biased voltage of +12 V was used (Baltuano et al., 2010). Detector is inside a vacuum chamber at 20 mmHg of absolute pressure. Data acquisition was done with basic spectroscopy software Genie TM 2000 (Mirion Technologies (Canberra) Inc., Meriden, Connecticut).

Modular XRF spectrometer.

A modular system consisting of a

Results and discussion

Fig. 1 shows alpha spectra obtained for each sample. It is seen that resolution improves from U-1 to U-4, this latter being the one with the optimal resolution. FWHM values of the  238U peak of samples U-3 and U-4 are shown in Table 1. Since a non-enriched uranium salt was used, it is expected that  235U (4398 keV) peak has very low intensity, which is only possible to see if  238U (4198 keV) and  234U (4776 keV) peaks are very sharp. The tails in the first half of the peaks in samples U-1, U-2

Conclusions

XRF is a promising technique for the rapid characterization of alpha sources, so poorly prepared sources can be discarded without delay, avoiding long acquisition times in alpha spectrometry. Since XRF is a very extensively used technique, this approach provides a fast, cheap, safe and easy characterization of alpha sources, the samples are not destructed, neither they do not require further conditioning, and hand-held and low-maintenance devices can be used instead of more expensive and

CRediT authorship contribution statement

Cynthia Cáceres-Rivero: Conceptualization, Writing - original draft, Visualization, Resources, Formal analysis. Jorge Martínez-Gastelú: Resources, Methodology.

Declaration of Competing Interest

The authors declare that they have no known competing financial interests or personal relationships that could have appeared to influence the work reported in this paper.

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