Electrochemical precipitation of neptunium with a micro electrochemical quartz crystal microbalance
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Electrochemical precipitation of neptunium with a micro electrochemical quartz crystal microbalance Adan Schafer Medina1 · Gretchen Tibbits1 · Nathalie A. Wall2 · Cornelius F. Ivory1 · Sue B. Clark3,4 · Haluk Beyenal1 Received: 2 December 2019 / Published online: 17 April 2020 © Akadémiai Kiadó, Budapest, Hungary 2020
Abstract Microliter volumes are used in electrochemical detection and preconcentration of radionuclides to reduce the dose received by researchers and equipment. Unfortunately, there is a lack of analysis of radionuclides with coupled electrochemical techniques and microliter volume reactors. The goals of this work are (1) to develop a miniaturized micro-electrochemical quartz crystal microbalance (μeQCM) reactor for use in small volume (50–200 μL) electrogravimetric experiments and (2) to use this reactor to characterize the preconcentration of neptunium on carbon electrodes via electroprecipitation. We successfully deposited neptunium in the new μeQCM reactor and verified its operation. We found that preconcentration of neptunium on carbon coated electrodes was possible by chronoamperometry at − 1.6 VAg/AgCl. The mass shift of the resulting precipitate was indicative of the amount of neptunium on the electrode, although the correlation between the mass increase and activity of the preconcentrated material was not linear. Neptunium precipitate reduced electron transfer to the solution as evidenced by the increase in charge transfer resistance compared to bare electrodes. Keywords Electroprecipitation · Electrochemistry · Radioelectrochemistry · Electrochemical quartz crystal microbalance · Preconcentration · Neptunium
Introduction Arguably, the largest hurdle to expanding nuclear energy is the implementation of a closed nuclear fuel cycle, which requires the reprocessing of used nuclear fuel to reclaim Electronic supplementary material The online version of this article (https://doi.org/10.1007/s10967-020-07138-0) contains supplementary material, which is available to authorized users. Adan Schafer Medina and Gretchen Tibbits are co-first authors and have equal authorship. * Haluk Beyenal [email protected] 1
The Gene and Linda Voiland School of Chemical Engineering and Bioengineering, Washington State University, Pullman, WA, USA
2
Department of Materials Science and Engineering, University of Florida, Gainesville, FL, USA
3
Department of Chemistry, Washington State University, Pullman, WA, USA
4
Pacific Northwest National Laboratory, Energy and Environment Directorate, Richland, WA, USA
unburned uranium and plutonium [1]. The challenges facing reprocessing high level waste start with the source of the radiotoxicity: decay of actinides (specifically plutonium-239 and neptunium-237) and their daughters [2]. Neptunium is of primary interest due to the safety hazards and the potential for use in nuclear weaponry [3]. Therefore, robust neptunium detection, separation, and preconcentration processes are needed. Neptunium, first isolated nearly 70 years ago, is largely unused commercial
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