The morphology of a synthesized poly[(tert-butyl acrylate)-b-styrene-b-isobutylene-b-styrene-(tert butyl acrylate)] pentablock terpolymer was determined using transmission electron microscopy, atomic force microscopy and small angle X-ray scattering methods. The outer blocks of this material were converted to the acrylic acid form by a thermal process that caused a beta-scission reaction in a simple thermal process, as verified by FTIR and NMR spectroscopies as well as thermogravimetric analysis. An initial heat-vacuum treatment induced a morphology that was more disordered relative to the precursor material, but when these samples were recast in THF solvent and annealed again, a considerably more refined and ordered morphology consisting of hexagonally packed cylinders resulted. This simple heat treatment allows for the tert-butyl groups to be converted to acrylic acid groups without dissolving the polymer or further sample cleaning. A dynamic mechanical investigation of the PtBuA form revealed three or two relaxation features depending interpretations based on the presence of three-phase morphology or a two-phase morphology in which there are mixed hard block domains. (C) 2008 Elsevier Ltd. All rights reserved.