Raman spectra, capacitance (C{degree}), phenanthrenequinone (PQ) adsorption, and heterogeneous electron-transfer rates for ferri/ferrocyanide, dopamine, and ascorbic acid were monitored after fracturing, polishing, and laser activating glassy carbon electrodes (GC-30). Alterations in the Raman spectrum indicate changes in carbon microstructure, while PQ adsorption and C{degree} provide measures of microscopic surface area. It was observed that polishing caused minor changes in carbon disorder and microscopic surface area, but the polished surface had poor electron-transfer kinetics. A k{degree} of above 0.5 cm s{sup {minus}1} was observed for Fe(CN){sub 6} for the first time. A clean, fractured GC surface exhibited a k{degree} of 0.5 cm s{sup {minus}1} and was very active toward ascorbic acid and dopamine oxidation. The results are consistent with a surface-cleaning mechanism for laser activation, accompanied by little or no observable surface restructuring or roughening.