Flow Injection Electrochemical Quartz Crystal Microbalance with ICP-OES Detection: Recovery of Silver by Electrodeposition with Redox Replacement in a Flow Cell

Molina, Daniel E.; Wall, Nathalie; Beyenal, Haluk; Ivory, Cornelius F.

doi:10.1149/1945-7111/abfcdd

Flow Injection Electrochemical Quartz Crystal Microbalance with ICP-OES Detection: Recovery of Silver by Electrodeposition with Redox Replacement in a Flow Cell

Journal Article · Mon May 24 00:00:00 EDT 2021 · Journal of the Electrochemical Society

DOI:https://doi.org/10.1149/1945-7111/abfcdd· OSTI ID:1835440

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We developed a new on-line hyphenated flow injection analysis technique (FI-EQCM-ICP-OES) that allows electrochemical deposition and stripping with mass detection and elemental analysis. This technique was used to study a new system for electrochemical recovery of silver from a 0.5 mM Ag ⁺ /5 mM Cu ²⁺ /0.5 M H ₂ SO ₄ solution by pulsed electrodeposition with redox replacement (EDRR) in a small flow cell. The metal ions in a 500 μ l sample are injected into the sulfuric acid carrier stream and deposited onto an electrochemical quartz crystal microbalance (EQCM) electrode housed in a 50 μ l flow cell. The deposits are subsequently stripped off electrochemically in the same cell and analyzed downstream in an ICP-OES. The stripped metal layer was found to be composed of Ag with no detectable Cu for a redox replacement time of 10 s, and 91 wt.% Ag–9 wt.% Cu for a redox replacement time of 5 s. Microscopy measurements demonstrated that the electrode was covered with silver particles, some of which contain Cu in the case of the 5 s replacement time. This technique allowed the study of mass changes on the electrode during electrodeposition and open circuit times in each EDRR cycle in flowing solutions.

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Sponsoring Organization:: USDOE National Nuclear Security Administration (NNSA)

Grant/Contract Number:: NONE; NA0003763

OSTI ID:: 1835440

Alternate ID(s):: OSTI ID: 1828747

Journal Information:: Journal of the Electrochemical Society, Journal Name: Journal of the Electrochemical Society Journal Issue: 5 Vol. 168; ISSN 0013-4651

Publisher:: The Electrochemical SocietyCopyright Statement

Country of Publication:: United States

Language:: English

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