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

作者：Nunes Luiza M S; Moraes Tiago B; Barbosa Lucio L; Mazo Luiz H; Colnago Luiz A^*

来源：Analytica Chimica Acta, 2014, 850: 1-5.

DOI：10.1016/j.aca.2014.05.022

• NMR
• Carbon-13
• SSFP
• Steady-state free precession
• Spectroelectrochemistry

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).

• 出版日期2014-11-19