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Composite Graphite–Epoxy Electrodes for In Situ Electrochemistry Coupling with High Resolution NMR

[Image: see text] The in situ coupling between electrochemistry and spectrometric techniques can help in the identification and quantification of the compounds produced and consumed during electrochemical reactions. The combination of electrochemistry with nuclear magnetic resonance is quite attract...

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Autores principales: Ferreira da Silva, Pollyana, Ferreira Gomes, Bruna, Silva Lobo, Carlos Manuel, Carmo, Marcelo, Roth, Christina, Colnago, Luiz Alberto
Formato: Online Artículo Texto
Lenguaje:English
Publicado: American Chemical Society 2022
Acceso en línea:https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8851621/
https://www.ncbi.nlm.nih.gov/pubmed/35187316
http://dx.doi.org/10.1021/acsomega.1c05823
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author Ferreira da Silva, Pollyana
Ferreira Gomes, Bruna
Silva Lobo, Carlos Manuel
Carmo, Marcelo
Roth, Christina
Colnago, Luiz Alberto
author_facet Ferreira da Silva, Pollyana
Ferreira Gomes, Bruna
Silva Lobo, Carlos Manuel
Carmo, Marcelo
Roth, Christina
Colnago, Luiz Alberto
author_sort Ferreira da Silva, Pollyana
collection PubMed
description [Image: see text] The in situ coupling between electrochemistry and spectrometric techniques can help in the identification and quantification of the compounds produced and consumed during electrochemical reactions. The combination of electrochemistry with nuclear magnetic resonance is quite attractive in this respect, but it has some challenges to be addressed, namely, the reduction in the quality of the NMR signal when the metallic electrodes are placed close to or in the detection region. Since NMR is not a passive technique, the convective effect of the magnetic force (magnetoelectrolysis), which acts by mixing the solution and increasing the mass transport, has to be considered. In seeking to solve the aforementioned problems, we developed a system of miniaturized electrodes inside a 5 mm NMR tube (outer diameter); the working and counter electrodes were prepared with a mixture of graphite powder and epoxy resin. To investigate the performance of the electrodes, the benzoquinone reduction to hydroquinone and the isopropanol oxidation to acetone were monitored. To monitor the alcohol oxidation reaction, the composite graphite–epoxy electrode (CGEE) surface was modified through platinization. The electrode was efficient for in situ monitoring of the aforementioned reactions, when positioned 1 mm above the detection region of the NMR spectrometer. The magnetoelectrolysis effect acts by stirring the solution and increases the reaction rate of the reduction of benzoquinone, because this reaction is limited by mass transport, while no effect on the reaction rate is observed for the isopropanol oxidation reaction.
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spelling pubmed-88516212022-02-18 Composite Graphite–Epoxy Electrodes for In Situ Electrochemistry Coupling with High Resolution NMR Ferreira da Silva, Pollyana Ferreira Gomes, Bruna Silva Lobo, Carlos Manuel Carmo, Marcelo Roth, Christina Colnago, Luiz Alberto ACS Omega [Image: see text] The in situ coupling between electrochemistry and spectrometric techniques can help in the identification and quantification of the compounds produced and consumed during electrochemical reactions. The combination of electrochemistry with nuclear magnetic resonance is quite attractive in this respect, but it has some challenges to be addressed, namely, the reduction in the quality of the NMR signal when the metallic electrodes are placed close to or in the detection region. Since NMR is not a passive technique, the convective effect of the magnetic force (magnetoelectrolysis), which acts by mixing the solution and increasing the mass transport, has to be considered. In seeking to solve the aforementioned problems, we developed a system of miniaturized electrodes inside a 5 mm NMR tube (outer diameter); the working and counter electrodes were prepared with a mixture of graphite powder and epoxy resin. To investigate the performance of the electrodes, the benzoquinone reduction to hydroquinone and the isopropanol oxidation to acetone were monitored. To monitor the alcohol oxidation reaction, the composite graphite–epoxy electrode (CGEE) surface was modified through platinization. The electrode was efficient for in situ monitoring of the aforementioned reactions, when positioned 1 mm above the detection region of the NMR spectrometer. The magnetoelectrolysis effect acts by stirring the solution and increases the reaction rate of the reduction of benzoquinone, because this reaction is limited by mass transport, while no effect on the reaction rate is observed for the isopropanol oxidation reaction. American Chemical Society 2022-01-31 /pmc/articles/PMC8851621/ /pubmed/35187316 http://dx.doi.org/10.1021/acsomega.1c05823 Text en © 2022 The Authors. Published by American Chemical Society https://creativecommons.org/licenses/by-nc-nd/4.0/Permits non-commercial access and re-use, provided that author attribution and integrity are maintained; but does not permit creation of adaptations or other derivative works (https://creativecommons.org/licenses/by-nc-nd/4.0/).
spellingShingle Ferreira da Silva, Pollyana
Ferreira Gomes, Bruna
Silva Lobo, Carlos Manuel
Carmo, Marcelo
Roth, Christina
Colnago, Luiz Alberto
Composite Graphite–Epoxy Electrodes for In Situ Electrochemistry Coupling with High Resolution NMR
title Composite Graphite–Epoxy Electrodes for In Situ Electrochemistry Coupling with High Resolution NMR
title_full Composite Graphite–Epoxy Electrodes for In Situ Electrochemistry Coupling with High Resolution NMR
title_fullStr Composite Graphite–Epoxy Electrodes for In Situ Electrochemistry Coupling with High Resolution NMR
title_full_unstemmed Composite Graphite–Epoxy Electrodes for In Situ Electrochemistry Coupling with High Resolution NMR
title_short Composite Graphite–Epoxy Electrodes for In Situ Electrochemistry Coupling with High Resolution NMR
title_sort composite graphite–epoxy electrodes for in situ electrochemistry coupling with high resolution nmr
url https://www.ncbi.nlm.nih.gov/pmc/articles/PMC8851621/
https://www.ncbi.nlm.nih.gov/pubmed/35187316
http://dx.doi.org/10.1021/acsomega.1c05823
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