High-porosity syndiotactic polystyrene aerogels characterized by nanofibrils that give rise to a microporous cryst. d-phase (see Figure) present a high sorption capacity for volatile org. compds. at low concns., typical of the d-phase, as well as high sorption kinetics, typical of aerogels. These sorption properties make these new aerogels very promising for industrial applications in chem. sepns. and water purifn.