PtAFT homopolymerization of 2-(diisopropylamino)ethyl methacrylate (DPA) and 2-(diethylamino)ethyl methacrylate (DEA) and their random copolymerization were investigated. The random copolymers of DPA-ran-DEA were synthesized and used as macro-CTA to prepare poly(DPA-ran-DEA)-b-poly(N-(2-hydroxypropyl) methacrylamide) amphiphilic block copolymers. The H-1 NMR and GPC measurements confirmed the successful synthesis of these copolymers. The potentiometric titration results showed that the pK(b) values of these copolymers were in the range of 6.7 similar to 7.7 and linearly varied with the DPA/DEA composition, regardless of the block length of HPMA. The pH-induced micellization in PBS solution was verified by fluorescence spectroscopy. The dynamic light scattering evaluation showed that the hydrodynamic diameters of these micelles are between 37 similar to 43 mn (C) 2008 Wiley Periodicals, Inc.