This article deals with the study of graft copolymerization of methylmethacrylate (MMA) onto Saccharum ciliare fiber in air in the presence of ferrous ammonium sulfate-potassium persulfate (FAS-KPS) as redox initiator. After optimizing the various reaction parameters such as solvent, time, temperature, concentration of monomer, and initiator to obtain maximum graft yield (58%), the grafted fiber has been characterized by various techniques such as scanning electron microscopy (SEM), Fourier transform-infrared spectrophotometry (FT-IR), X-ray diffraction, and thermogravimetric=differential thermal analysis along with DTG studies. The raw fiber and graft copolymerized fibers were also subjected to evaluation of different physical and chemical properties.