title: Monitoring electrochemical reactions in situ using steady-state free precession (13)C NMR spectroscopy.
abstract: All attempts to use in situ(13)C 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 (13)C NMR signals by more than one order of magnitude. The results showed that each (13)C 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 30min during 3h. The phase and truncation anomalies present in SSFP spectra were minimized using Traff apodization function and Krylov basis diagonalization method (KBDM).
authors.affiliation: Instituto de Química de São Carlos, Universidade de São Paulo, Avenida Trabalhador São-Carlense 400, São Carlos, São Paulo 13560-070, Brazil; Embrapa Instrumentação, Rua XV de Novembro 1452, São Carlos, São Paulo 13560-970, Brazil.
authors.forename: Luiza M S
authors.initials: LM
authors.lastname: Nunes
authors.affiliation: Embrapa Instrumentação, Rua XV de Novembro 1452, São Carlos, São Paulo 13560-970, Brazil; Instituto de Física de São Carlos, Universidade de São Paulo, Avenida Trabalhador São-Carlense 400, São Carlos, São Paulo 13566-590, Brazil.
authors.forename: Tiago B
authors.initials: TB
authors.lastname: Moraes
authors.affiliation: Departamento de Química, Universidade Federal do Espírito Santo, Avenida Fernando Ferrari 514, Vitória, Espírito Santo 29075-910, Brazil.
authors.forename: Lucio L
authors.initials: LL
authors.lastname: Barbosa
authors.affiliation: Instituto de Química de São Carlos, Universidade de São Paulo, Avenida Trabalhador São-Carlense 400, São Carlos, São Paulo 13560-070, Brazil.
authors.forename: Luiz H
authors.initials: LH
authors.lastname: Mazo
authors.affiliation: Embrapa Instrumentação, Rua XV de Novembro 1452, São Carlos, São Paulo 13560-970, Brazil. Electronic address: luiz.colnago@embrapa.br.
authors.forename: Luiz A
authors.initials: LA
authors.lastname: Colnago
keywords: Carbon-13; NMR; SSFP; Spectroelectrochemistry; Steady-state free precession