Monitoring electrochemical reactions in situ using steady-state free precession C-13 NMR spectroscopy

Author(s)

Nunes, Luiza M. S. ^{[1, 2]} ; Moraes, Tiago B. ^{[1, 3]} ; Barbosa, Lucio L. ^[4] ; Mazo, Luiz H. ^[2] ; Colnago, Luiz A. ^[1]

Affiliation

^[1] EMBRAPA Instrumentacao, BR-13560970 Sao Paulo - Brazil

^[2] Univ Sao Paulo, Inst Quim Sao Carlos, BR-13560070 Sao Paulo - Brazil

^[3] Univ Sao Paulo, Inst Fis Sao Carlos, BR-13566590 Sao Paulo - Brazil

^[4] Univ Fed Espirito Santo, Dept Quim, BR-29075910 Vitoria, Espirito Santo - Brazil

• Document type: Journal article
• Source: Analytica Chimica Acta; v. 850, p. 1-5, NOV 19 2014.
• Web of Science Citations: 14

Abstract

All attempts to use in situ C-13 NMR in spectroelectrochemical studies, using static cells and unlabeled substrates, have failed due to the very long average time (several hours). In this paper, we demonstrated that steady-state free precession (SSFP) pulse sequence can enhance signal to noise ratio and reduces the average time of C-13 NMR signals by more than one order of magnitude. The results showed that each C-13 NMR spectrum during the electrochemical reduction of 9-chloroanthracene, in a static cell, can be acquired in eleven minutes. This short averaging time allowed the analysis of the reaction every 30 min during 3 h. The phase and truncation anomalies present in SSFP spectra were minimized using Traff apodization function and Krylov basis diagonalization method (KBDM). (C) 2014 Elsevier B.V. All rights reserved. (AU)

• FAPESP's process: 07/07436-8 - Use of SSFP-NMR to enhance signal to noise ratio in Electrochemical-NMR experiments in situ.
• Grantee: Luiza Maria da Silva Nunes
• Support Opportunities: Scholarships in Brazil - Doctorate
• FAPESP's process: 11/11160-3 - Development of steady state free precession (SSFP) sequences with phase alternation for rapid acquisition of high resolution NMR spectra
• Grantee: Tiago Bueno de Moraes
• Support Opportunities: Scholarships in Brazil - Doctorate