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

• Analysis of electrochemical reaction in situ by 13C NMR spectroscopy was demonstrated.
• 13C NMR signals are obtained in few minutes, using steady-state free precession (SSFP) pulse sequence.
• The analysis is performed in standard NMR spectrometer.
• KBDM can be an alternative to Fourier Transform to process SSFP signal.

All attempts to use in situ13C 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 13C NMR signals by more than one order of magnitude. The results showed that each 13C 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).

Figure optionsDownload as PowerPoint slide