Abstract: In-situ FTIR reflective spectrometry was used to study the formation and the changes of oxygen-containing functional groups on the GCelectrode surface during its electrochemical activation. The surface functional groups were formed during the high-potential oxidation of GCelectrode, some of which were further oxidized to CO₂Parts of the quinone-like groups were reduced during the cyclic voltammetric process thereafter, and stable surface redox couples were formed at the end. In the differential FTIR reflective spectra in these cycling processes appeared positive peaks at 1669 cm^-1and 1690 cm^-1, corresponding to quinone-like groups and a wide negative peak at 1590 cm^-1, corresponding to the stretching vibration of carboxylic anion and aromatic ring. The potential difference spectra showed a pair of bipolar peaks at 1705 cm^-1and 1750 cm^-1and peaks at 1605 cm^-1and 1580 cm^-1. These results are explained by supposing hydrogen-bonding between quinone-like groups and carboxylic groups and the chemical and electrochemical processes of the surface functional groups.

Key words: Glassy carbon electrode, Electrochemical activation. Electrode surface processes, In-situ FTIR reflective spectroscopy