An electrophoresis cell of rectangular cross-section has been constructed using cleaved sheets of mica as the side windows. A dilute dispersion of polystyrene latex particles was placed in the cell and the velocity profile of particles at different depths in the cell was observed. Linearisation of these data enabled the electro-osmotic velocity of the fluid close to the mica surface to be determined and hence the zeta potential. The zeta potential of mica as a function of potassium chloride concentration was determined and the results were compared with the surface potential obtained from direct force measurements. Results were also obtained from the zeta potential of mica as a function of the concentration of alkyltrimethylammonium bromides with chain lengths of C-8, C-10, C-12 and C-16.