Miniaturized Carbon Fiber Paper Electrodes for In Situ High Resolution NMR Analyses
- Pollyana Ferreira da SilvaPollyana Ferreira da SilvaInstituto de Química de São Carlos, Universidade de São Paulo, Av. Trabalhador São-carlense, 400, 13566-590São Carlos, SP, BrazilForschungszentrum Jülich GmbH, Wilhelm-Johnen-Straße, 52428Jülich, GermanyMore by Pollyana Ferreira da Silva
- Tatiana Santana RibeiroTatiana Santana RibeiroForschungszentrum Jülich GmbH, Wilhelm-Johnen-Straße, 52428Jülich, GermanyDepartment of Natural Science, Mathematics and Education, Federal University of São Carlos, Rodovia Anhanguera, Km 174, SP-330, 13600-970Araras, SP, BrazilMore by Tatiana Santana Ribeiro
- Bruna Ferreira Gomes*
- Gelson Tiago dos Santos Tavares da SilvaGelson Tiago dos Santos Tavares da SilvaEmbrapa Instrumentação, Rua XV de Novembro, 1452, 13561-206São Carlos, SP, Brazil
- Carlos Manuel Silva Lobo
- Marcelo Carmo
- Cauê Ribeiro
- Rubens Bernardes FilhoRubens Bernardes FilhoEmbrapa Instrumentação, Rua XV de Novembro, 1452, 13561-206São Carlos, SP, BrazilMore by Rubens Bernardes Filho
- Christina Roth
- , and
- Luiz Alberto Colnago
Combining spectroscopic techniques with electrochemistry is a promising strategy, as it allows the detailed investigation of the species that are consumed and produced by the reaction in real time. However, as with any in situ coupling technique, the junction between NMR and electrochemistry presents some challenges, notably the distortion of NMR signals due to the placement of electrodes close to or within the detection region. In this work, miniaturized electrodes made of carbon fiber paper were developed and later modified with platinum. Platinum decoration by cathodic deposition was chosen, as platinum is a prominent element in electrocatalysis, able to catalyze a large variety of reactions. To evaluate the efficiency of this electrochemical system, the oxidation of ascorbic acid was used as a model reaction. It was observed that the electrodes caused substantial signal distortion when placed within the detection region (full width at half-maximum equal to 1.46 Hz), whereas no distortion was observed when the electrodes were placed 1 mm above the detection region (full width at half-maximum equal to 0.95 Hz). With this system, it was also possible to monitor the magnetoelectrolysis effect, caused by the interaction of the magnetic field with the flowing ions, leading to a doubling of the ascorbic acid oxidation rate, compared to the reaction performed without a magnetic field. In addition to its low cost and simplicity in preparation, the developed electrode system allows the electrode surface to be easily modified with other suitable catalysts.
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