The aim of this investigation was to design iron oxide containing nanocomposites which could display superparamagnetic behavior and thus find application in biomedical and allied fields. To achieve the proposed objectives methyl methacrylate was polymerized by a redox system comprising of metabisulphite and persulphate in the immediate presence of a crosslinker, N,N 0methylene bis acrylamide and a preformed polymer, i.e., polyvinyl alcohol. Into the prepared polymer matrix nanosized magnetite (Fe 3 O 4 ) particles were evenly dispersed by in situ precipitation of Fe 2+ /Fe 3+ ions. The nanocomposite materials were characterized by techniques like FTIR, SEM, TEM, XRD, and DSC. The magnetic behavior of nanocomposites and bulk magnetite particles was studied under varying applied magnetic fields and their superparamagnetic property was examined. The iron-oxide polymer nanocomposites were also studied for microhardness. POLYM. COMPOS., 31:245-255, FIG. 2. SEM image of (a) iron oxide impregnated gel of definite composition: [PVA] ¼ 2.0 g, [MMA] ¼ 9.35 mM, [MBA] ¼ 0.06 mM, and (b) TEM image of iron oxide nanoparticles.