A relatively simple continuous dilution method with on-line spectrophotometric measurement has been used to determine the phase transition boundaries of aqueous two-phase polymer systems. The observed range of compositions over which the phase transition occurs is dominated by the polydispersity of the polymers, but also is a function of the dilution path followed. The binodal curve obtained by the continuous dilution method agrees well with the results obtained by the traditional method of phase equilibration, separation and analysis of liquid chromatography, which is slower and requires more expensive equipment.