Synthesis of vinyl benzyl chloride (VBC)/divinylbenzene (DVB) copolymers via surfactant-freeemulsion polymerization yields near monodisperse chloromethylated polystyrene precursor nanospheres ~400nm in diameter. These are analogous to gel-type suspension polymerized particles typically of ~100-500
m indiameter and are essentially nonporous in the dry state having only a very nominal surface area (~10 m
2 g
-1).Cross-linking of appropriate dichloroethane swollen precursors with a high content of VBC residues in the presenceof FeCl
3 (i.e., using a Davankov-type strategy) yields near monodisperse porous hyper-cross-linked nanoparticleswith extremely high surface areas up to ~1200 m
2 g
-1. The latter display all the characteristics of Davakov-typeresins in terms of their ability to sorb both thermodynamically "poor" and "good" solvents and in particulardespite their superficial hydrophobic makeup are able to sorb significant quantities of water (up to ~2.5 g/g). Byadjusting the content of VBC in the precursor particles, the surface area of the near monodisperse nanoparticlescan be adjusted in the range ~15-1300 m
2 g
-1.