Mechanistic Study of the Validity of Using Hydroxyl Radical Probes To Characterize Electrochemical Advanced Oxidation Processes

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Department of Chemical Engineering, University of Illinois at Chicago, 810 South Clinton Street, Chicago, Illinois 60607, United States
*Phone: 312-996-0288; fax: 312-996-0808; email: [email protected]
Cite this: Environ. Sci. Technol. 2017, 51, 4, 2355–2365
Publication Date (Web):January 10, 2017
Copyright © 2017 American Chemical Society
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The detection of hydroxyl radicals (OH) is typically accomplished by using reactive probe molecules, but prior studies have not thoroughly investigated the suitability of these probes for use in electrochemical advanced oxidation processes (EAOPs), due to the neglect of alternative reaction mechanisms. In this study, we investigated the suitability of four OH probes (coumarin, p-chlorobenzoic acid, terephthalic acid, and p-benzoquinone) for use in EAOPs. Experimental results indicated that both coumarin and p-chlorobenzoic acid are oxidized via direct electron transfer reactions, while p-benzoquinone and terephthalic acid are not. Coumarin oxidation to form the OH adduct product 7-hydroxycoumarin was found at anodic potentials lower than that necessary for OH formation. Density functional theory (DFT) simulations found a thermodynamically favorable and non-OH mediated pathway for 7-hydroxycoumarin formation, which is activationless at anodic potentials > 2.10 V/SHE. DFT simulations also provided estimates of E° values for a series of OH probe compounds, which agreed with voltammetry results. Results from this study indicated that terephthalic acid is the most appropriate OH probe compound for the characterization of electrochemical and catalytic systems.

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The Supporting Information is available free of charge on the ACS Publications website at DOI: 10.1021/acs.est.6b05513.

  • Literature reviews of OH probes used in various systems, anodic peak potentials of selective compounds, details of LSV simulation, schematics of system setup, LSV of COU, p-CBA and TA on Pt electrode, diffusion coefficients and mass transfer rate constants for COU, TA, and p-BQ, LSV of TA and p-BQ, CV of COU, reaction rate constants for bulk oxidation of COU, TA, and p-BQ, COU oxidation under various temperatures at 1.7 V vs SHE, TA and p-BQ oxidation under various temperatures at 3.0 V vs SHE, theoretical E0 and λf values determined by DFT methods and used to determine Ea vs potential profiles, and transition state structure (PDF)

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