New beta-cyclodextrin-based side-chain azo amphiphilic polyurethanes were prepared. Aggregation behaviour was studied by employing steady-state fluorescence and UV-Vis spectroscopy techniques and, determination of the hydrodynamic diameter of micellar aggregates in N,N-dimethyl formamide and N,N-dimethyl formamide/ethanol mixture solutions was done. An apparent polarity evidenced by increasing I (1)/I (3) ratio with the increasing concentration of polyurethanes except the polyurethanes with stronger intra- and intermolecular hydrogen bonding of hard segments was obtained. Pyrene resides predominantly in the interfacial region in micellar aggregates that is sensitive to polarity changes due to solvent penetration. Apparent critical micelle concentration due to the presence of beta-cyclodextrin was determined by steady-state fluorescence and UV-Vis spectroscopy techniques which ranged between 10(-2) and 10(-1) g/L. Binding constants from both spectroscopy techniques were determined. The values of hydrodynamic diameter for the amphiphilic poly(ether urethane)s show that their aggregation behaviour is different in function of chemical composition, type and content of hard segment and hydrophobe/hydrophile ratio.