Acid-catalyzed hydrolysis of 2,5-dimethyl-2,5-hexanediol dimethacrylate (DHDMA)-containing nanoparticles has been carried out to bring about topological reorganization from spherical macromolecular crosslinked particles to linear polymer. The reactive cross-linked poly(methyl methacrylate)-based (x-PMMA) nanoparticles have been prepared via aqueous emulsion techniques where the size of the particles depends upon the type of emulsion polymerization employed, surfactant-free or surfactant-based. Potassium persulfate has been employed as the water-soluble initiator and sodium dodecyl sulfate as the surfactant. Because of the acid-sensitive nature of the tertiary ester groups of the 2,5-dimethyl-2,5-hexanediol dimethacrylate within the cross-linked nanoparticles, they can be easily cleaved into their linear polymer chain composition under acidic conditions. The particles were degraded by heating in dioxane in the presence of p-toluenesulfonic acid at 100 degrees C for 12 h. The cleavage of the cross-linked nanoparticles was observed by the correlation and size distribution plots obtained using dynamic light scattering. The particles and the acid cleaved, linear polymer residue were characterized using scanning electron microscopy (SEM), solubility tests, and gel permeation chromatography.