In the present work, the polyamide nylon6 was grafted in formic acid with maleic anhydride (MAH) and methyl methacrylate (MMA) using ceric ammonium nitrate as an initiator in aqueous nitric acid medium. Variation of synthetic parameters such as grafting percentage, grafting efficiency, percentage monomer conversion and grafting yield with solvent, reaction time, temperature, monomer and initiator concentrations were investigated for the binary graft copolymer (N6-g-MAH-g-MMA). The observed results indicate that the grafting parameters were increased at first and then decreased with increase in the concentration of initiator, monomer, N6-g-MAH and temperature. Graft copolymers with both high grafting efficiency and high grafting percentage were obtained indicating that ceric ammonium nitrate was an efficient initiator for this graft copolymerization. The synthesized graft copolymers were characterized by Fourier Transform Infrared Spectroscopy (FT-IR), Thermogravimetric analysis (TGA),Differential Scanning Calorimetry (DSC) and X-ray diffraction(XRD)studies. The FT-IR measurements clearly suggest that monomers were effectively grafted onto polyamide Nylon6 and N6-g-MAH.The XRD studies elucidates the change in the crystallinity of the grafted polymeric samples.