Abstract: Poly(methyl methacrylate) (PMMA) hollow nanospheres composed of Fe 2 O nanoparticles have been synthesized using a new microemulsion method. In this stepwise method a core/shell nanocomposite was prepared in an oil-in-water microemulsion system. The polymerized core of the system removed by a solvent to obtain a hollow sphere particle. The synthesized nanocomposite sample was identified using TEM and FT-IR techniques. The fabricated PMMA/Fe 2 O 3 3 hollow nanosphere sample was used as an excellent magnetic adsorbent for removal of sulphur compounds from gasoline. Removal experiment over PMMA/Fe 2 O showed that the desulfurization yield is around 94 % for initial sulfur concentration of 100 ppm for maximum removal time of 60 min.