In this study, we demonstrate the usefulness of chemical-based method in combination with atomic force microscopy (AFM) to characterize the degradable regions in a wide range of polymer blends. This approach is based on selective hydrolysis of one of the components in a multiple-phase system, and the ability of AFM to provide nanoscale lateral information about the different phases in the polymer system. Composite films containing different percentage of hydrolyzable polymer were either melt processed or solution casted and then exposed to a hydrolytic acidic environment. Tapping mode AFM was used to analyze the samples before and after hydrolysis. Dramatic topographic changes such as pits were observed on the acid exposed samples, indicating that the degradation was localized and the more susceptible component in the blend was hydrolyzed. Additionally, the progressive hydrolysis of the composites was studied by attenuated total reflection FTIR (ATR-FTIR) analyses to confirm the AFM results. (c) 2006 Wiley Periodicals, lnc.