In situ FT-IR and ex situ EPR analysis for the study of the electroreduction of carbon dioxide in N, N-dimethylformamide on a gold interface

• Published in: Journal of electroanalytical chemistry (Lausanne, Switzerland) Switzerland), 2005-04, Vol.578 (1), p.87-94
• Main Authors: Pérez, Eduardo R., Garcia, Jarem R., Cardoso, Daniel R., McGarvey, Bruce R., Batista, Elisete A., Rodrigues-Filho, Ubirajara P., Vielstich, Wolf, Franco, Douglas W.
• Format: Article
• Language: English
• Subjects: Carbamates; Chemistry; DMF + TBAF electrolyte; Electrochemistry; Electroreduction of CO 2; EPR spectroscopy; Exact sciences and technology; FT-IR spectroscopy; General and physical chemistry; Gold interface
• ISSN: 1572-6657; 1873-2569
• DOI: 10.1016/j.jelechem.2004.11.044

Carbon monoxide, formate and carbonate were found as products from the CO 2 reduction at a gold interface in DMF + TBAF solution. Carbonate could be formed also by reaction of CO 2 with hydroxyl anions generated by reduction of the residual water in solution. The carbonate reacts with amines to form carbamates in good yields (72–96%). In situ FT-IR and ex situ EPR analysis have demonstrated the formation of free radicals in the absence of CO 2 and at potentials more negative than −1.8 V (SCE). FT-IR measurements using s-polarized light have proved that these radicals are in solution. An electrochemical reaction of the electrolyte solution on the gold surface yielded a solid product involving particles from the gold surface.