The synthesis and self-assembly properties in aqueous solutions of novel arnphiphilic block copolymers composed of one hydrophilic, pH and temperature responsive pctly(dimethyl amino ethyl methacrylate) (PDMAEMA) block and one weakly hydrophobic, water insoluble, potentially thermoresponsive poly(hydroxy propyl methacrylate) (PHPMA) block, are reported. The block copolymers were prepared by RAFT polymerization and were molecularly characterized by size exclusion chromatography, NMR, and FTIR spectroscopies, The PDMAEMA-b-PHPMA amphiphilic block copolymers self assemble in different nanostructured aggregates when inserted in aqueous media. The effects of different solubilization protocols, as well as the effects of solution temperature and pH on the structure of the aggregates, are studied by light scat tering and fluorescence spectroscopy measurements. Experimental results indicate that there is a number of solution preparation and physicochemical parameters that anew the control and manipulation of the structure and thermoresponsive properties of PDMAEMA-b-PHPMA aggregates in aqueous media. (C) 2018 Wiley Periodicals, Inc.