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Issue 36, 2015
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Electrochemical electron paramagnetic resonance utilizing loop gap resonators and micro-electrochemical cells

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Abstract

A miniaturised electrochemical cell design for Electron Paramagnetic Resonance (EPR) studies is reported. The cell incorporates a Loop Gap Resonator (LGR) for EPR investigation of electrochemically generated radicals in aqueous (and other large dielectric loss) samples and achieves accurate potential control for electrochemistry by using micro-wires as working electrodes. The electrochemical behaviour of the cell is analysed with COMSOL finite element models and the EPR sensitivity compared to a commercial TE011 cavity resonator using 4-hydroxy-2,2,6,6-tetramethylpiperidin-1-oxyl (TEMPOL) as a reference. The electrochemical EPR performance is demonstrated using the reduction of methyl viologen as a redox probe in both water and acetonitrile. The data reported herein suggest that sub-micromolar concentrations of radical species can be detected in aqueous samples with accurate potential control, and that subtle solution processes coupled to electron transfer, such as comproportionation reactions, can be studied quantitatively using EPR.

Graphical abstract: Electrochemical electron paramagnetic resonance utilizing loop gap resonators and micro-electrochemical cells

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Publication details

The article was received on 21 Jul 2015, accepted on 12 Aug 2015 and first published on 13 Aug 2015


Article type: Paper
DOI: 10.1039/C5CP04259C
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Phys. Chem. Chem. Phys., 2015,17, 23438-23447
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    Electrochemical electron paramagnetic resonance utilizing loop gap resonators and micro-electrochemical cells

    M. A. Tamski, J. V. Macpherson, P. R. Unwin and M. E. Newton, Phys. Chem. Chem. Phys., 2015, 17, 23438
    DOI: 10.1039/C5CP04259C

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