Purification of single-walled carbon nanotubes by capillary electrophoresis (CE) is demonstrated. Real-time Raman spectroscopy of the separation process and single-wavelength UV/vis detection show the ability of CE to provide high-resolution separations of nanotube fractions with baseline separation. AFM images of collected fractions demonstrate that separations are based on tube length. The separation method is suggested to be based on alignment of the nanotubes along the separation field.