Study of the coupling between electrochemistry and low-field, mid-resolution NMR for the in situ and on line analysis of redox reactions of organic compounds and the evaluation of the magnetic field effect on the velocity of the in situ reactions

• Grant number: 16/01537-6
• Support Opportunities: Scholarships abroad - Research Internship - Doctorate (Direct)
• Start date: October 10, 2016
• End date: October 09, 2017
• Field of knowledge: Physical Sciences and Mathematics - Chemistry - Analytical Chemistry
• Principal Investigator: Luiz Alberto Colnago
• Grantee: Bruna Ferreira Gomes Lobo
• Supervisor: Bernhard Bluemich
• Host Institution: Embrapa Instrumentação Agropecuária. Empresa Brasileira de Pesquisa Agropecuária (EMBRAPA). Ministério da Agricultura, Pecuária e Abastecimento (Brasil). São Carlos , SP, Brazil
• Institution abroad: RWTH Aachen University, Germany
• Associated to the scholarship: 12/22281-9 - NMR study of the magneto-convective phenomenon on paramagnetic ions during electrodeposition, BP.DD

Abstract

The coupling between electrochemistry and NMR spectroscopy (EC-NMR) is a powerful technique to elucidate reaction mechanisms specially in oxidative degradation reactions. It can be a good option to evaluate unstable species. Despite the advantages, there are some problems resulting from the coupling, such as the noise generated by the electrochemical signal and the reducing of NMR peak resolution due to loss of magnetic field homogeneity caused by the introduction of the electrochemical cell. To solve this problem, some papers suggest the use of carbon fiber as working and counter electrodes and the use of a Pd or Ag wire as reference electrode. Despite the advantages of NMR spectroscopy to evaluate the structures of the organic compounds, it is known that the magnetic field can both change the reaction rate as well as the morphology of the electrochemical deposit. This effect is known as magnetoelectrolysis, although it has been known for a few decades, no EC-NMR work using high resolution took into account this phenomenon. This effect is proportional to the intensity of the magnetic field and recently we published an article which demonstrated the effect of the magnetic field in the copper deposition rate during the EC-NMR coupling using a low-field equipment (0.33 T). Therefore, it is expected the reaction rate increases for reactions conducted in situ in the presence of a high intensity magnetic field. Therefore, we intend to evaluate both the magnetic field effect on these reactions performed in situ and on line, as well as the efficiency of the EC-NMR coupling with low magnetic field and medium resolution for elucidation of the compounds involved in redox reactions. (AU)

Scientific publications

(5)

(References retrieved automatically from Web of Science and SciELO through information on FAPESP grants and their corresponding numbers as mentioned in the publications by the authors)

GOMES, BRUNA FERREIRA; SILVA LOBO, CARLOS MANUEL; COLNAGO, LUIZ ALBERTO. Monitoring Electrochemical Reactions in Situ with Low Field NMR: A Mini-Review. APPLIED SCIENCES-BASEL, v. 9, n. 3, FEB 1 2019. (16/01537-6, 17/12864-0, 12/22281-9)

DA SILVA, POLLYANA FERREIRA; GOMES, BRUNA FERREIRA; SILVA LOBO, CARLOS MANUEL; KENG QUEIROZ JUNIOR, LUIZ HENRIQUE; DANIELI, ERNESTO; CARMO, MARCELO; BLUEMICH, BERNHARD; COLNAGO, LUIZ ALBERTO. Electrochemical NMR spectroscopy: Electrode construction and magnetic sample stirring. Microchemical Journal, v. 146, p. 658-663, MAY 2019. (17/12864-0, 12/22281-9, 16/01537-6)

LOBO, CARLOS M. S.; GOMES, BRUNA F.; BOUZOUMA, HAJAR; DANIELI, ERNESTO; BLUEMICH, BERNHARD; COLNAGO, LUIZ A.. Improving in operando low field NMR copper electrodeposition analyses using inductively coupled coils. Electrochimica Acta, v. 298, p. 844-851, MAR 1 2019. (17/12864-0, 12/22281-9, 16/01537-6)

BENDERS, STEFAN; GOMES, BRUNA FERREIRA; CARMO, MARCELO; COLNAGO, LUIZ ALBERTO; BLUEMICH, BERNHARD. In-situ MRI velocimetry of the magnetohydrodynamic effect in electrochemical cells. JOURNAL OF MAGNETIC RESONANCE, v. 312, MAR 2020. (12/22281-9, 17/12864-0, 16/01537-6)

GOMES, BRUNA FERREIRA; HOLZHAEUSER, FABIAN JOSCHKA; SILVA LOBO, CARLOS MANUEL; DA SILVA, POLLYANA FERREIRA; DANIELI, ERNESTO; CARMO, MARCELO; COLNAGO, LUIZ ALBERTO; PALKOVITS, STEFAN; PALKOVITS, REGINA; BLUEMICH, BERNHARD. Sustainable Electrocoupling of the Biogenic Valeric Acid under in Situ Low-Field Nuclear Magnetic Resonance Conditions. ACS SUSTAINABLE CHEMISTRY & ENGINEERING, v. 7, n. 22, p. 18288-18296, NOV 18 2019. (12/22281-9, 16/01537-6)