Square wave voltammetry for real time analysis of minor metal ion concentrations in molten salt reactor fuel

Zhang, Huan; Choi, Suhee; Zhang, Chao; Faulkner, Emma; Alnajjar, Nora; Okabe, Parker; Horváth, Dávid; Simpson, Michael F.

doi:10.1016/j.jnucmat.2019.151791

Cited by 9 publications

(11 citation statements)

References 21 publications

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“…For example, the redox potential of salt could be monitored and controlled to mitigate the effects of impurities and to measure the efficacy of salt-cleaning procedures, − but the redox potential is affected by all impurities in the mixture. While electrochemical techniques are element specific, , they are relatively low-resolution methods that produce broad element-specific peaks that overlap in multicomponent solutions . By comparison, high-resolution X-ray absorption spectroscopy (XAS) is an extremely sensitive atom-specific method.…”

Section: Introductionmentioning

confidence: 99%

In-Situ Analysis of Corrosion Products in Molten Salt: X-ray Absorption Reveals Both Ionic and Metallic Species

et al. 2023

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Understanding and controlling the chemical processes between molten salts and alloys is vital for the safe operation of molten-salt nuclear reactors. Corrosion processes in molten salts are highly dependent on the redox potential of the solution that changes with the presence of fission and corrosion processes, and as such, reactor designers develop electrochemical methods to monitor the salt. However, electrochemical techniques rely on the deconvolution of broad peaks, a process that may be imprecise in the presence of multiple species that emerge during reactor operation. Here, we describe in situ measurements of the concentration and chemical state of corrosion products in molten FLiNaK (eutectic mixture of LiF–NaK–KF) by high-resolution X-ray absorption spectroscopy. We placed a NiCr foil in molten FLiNaK and found the presence of both Ni2+ ions and metallic Ni in the melt, which we attribute to the foil disintegration due to Cr dealloying.

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Section: Introductionmentioning

confidence: 99%

In-Situ Analysis of Corrosion Products in Molten Salt: X-ray Absorption Reveals Both Ionic and Metallic Species

et al. 2023

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“…24 The influence of uranium concentration on the electrode processes and the characteristics of the cathodic deposits produced in molten salts were also studied. 25,26 The electrochemical behavior of oxygen-free uranium ions in chlorides melts on reactive liquid metal electrodes was studied using various electrochemical techniques. [27][28][29][30][31][32][33][34][35][36][37][38][39][40] In a number of works cadmium was considered as the material of the reactive electrode, mainly because the low boiling point of cadmium enables its easy subsequent separation from the alloy with deposited uranium.…”

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confidence: 99%

Mechanism of Metallic Uranium and Bimetallic U-Ga, U-Cd Alloys Electrodeposition in Molten LiCl–KCl–CsCl Eutectic

Новоселова

Smolenski

Volkovich

et al. 2023

J. Electrochem. Soc.

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Speciation and behavior of uranium (III) chloride in the ternary low melting LiCl–KCl–CsCl eutectic was studied by electrochemistry and spectroscopy techniques. Cathodic reduction of U(III) ions on inert (tungsten) and reactive (gallium, cadmium) electrodes was investigated at 623-923 K using cyclic and square wave voltammetry. The potential scan rate was changed from 0.075 to 0.5 V/s in all experiments. It was established that the electrochemical reduction process on the inert electrode was irreversible, proceeded in one stage, and was controlled by the charge transfer. Formation of uranium alloys with gallium and cadmium was studied using active liquid Ga and Cd electrodes. Reduction of uranium ions of the reactive electrodes proceeded with considerable depolarization. The effect of current density on the composition of the cathodic product was considered. Conditions for the electrochemical production of alloys of a given composition were determined.

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“…A variety of studies have been conducted in systems with multiple electroactive species. 59,60,94,98,[105][106][107][108][109][110][111][112][113][114][115][116][117] These studies typically find that in deposition reactions the accuracy of concentration measurement is diminished when reduction peaks overlap, and even when separated, the second deposition reaction is affected by the first. Standard reduction potentials indicate that corrosion of typical structural metals will impact the accuracy of the vital measurements for U and Pu in electrorefiners.…”

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confidence: 99%

Review—Concentration Measurements In Molten Chloride Salts Using Electrochemical Methods

Williams

Shum

Rappleye

2021

J. Electrochem. Soc.

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The electrochemical measurement of concentration in molten chloride salts is a valuable tool for the control of existing and potential industrial processes, recycling of precious materials and energy production. The electrochemical techniques commonly used to measure concentration and each techniques’ associated theory are discussed. Practices which improve measurement accuracy and precision are set forth. Exceptionally accurate and precise measurements published in the literature are evaluated based on their performance in specified concentration ranges. The strengths and weaknesses of the most accurate measurements are briefly explored. Chronopotentiometry (CP) and square wave voltammetry (SWV) are accurate and precise with low concentration measurements. SWV was accurate at low concentrations, even in multi-analyte mixtures. CP was accurate for only single analyte mixtures. Open-circuit potentiometry (OCP) is accurate and precise in single-analyte mixtures but yields large errors in multianalyte mixtures. Cyclic voltammetry (CV), chronoamperometry (CA) and normal pulse voltammetry (NPV) are accurate and precise across all concentration ranges. NPV is exceptionally well suited for measurements in melts with multiple electroactive species.

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Square wave voltammetry for real time analysis of minor metal ion concentrations in molten salt reactor fuel

Cited by 9 publications

References 21 publications

In-Situ Analysis of Corrosion Products in Molten Salt: X-ray Absorption Reveals Both Ionic and Metallic Species

In-Situ Analysis of Corrosion Products in Molten Salt: X-ray Absorption Reveals Both Ionic and Metallic Species

Mechanism of Metallic Uranium and Bimetallic U-Ga, U-Cd Alloys Electrodeposition in Molten LiCl–KCl–CsCl Eutectic

Review—Concentration Measurements In Molten Chloride Salts Using Electrochemical Methods

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