A carbon-disk microelectrode was used to investigate the surface concentration profile of etchant Br-2, which was electrogenerated on the Pt working electrode. The steady state reducing currents of Br-2 at different distances away from the Pt electode was measured. The concentration profile was estimated from the current-distance variation curves as a function of different sampling times. Experimentally determined concentration profiles are in good agreement with those estimated from the microetching results. The microelectrode technique has offered a good method to choose suitable etching solution for chemical micromachining