Poly vinyl alcohol (PVA) and poly ethylene glycol (PEG) blends were prepared and irradiated with different electron beam irradiation doses. The influence of the irradiation dose, and PEG content on the physico-chemical properties was investigated. The data regarding gel content demonstrated that the radiation-induced crosslinking of PVA and PVA/PEG samples increased as a result of increasing irradiation dose and decreasing PEG content. The swelling volume ratio shows an opposite behavior. The XRD parameters (crystllinity percent and d-spacing values) show a decreasing behavior for PVA and PVA/PEG blends as a result of either irradiation or blending PVA matrix with PEG. The DSC data illustrate a decreasing trend in melting point, glass transition temperature, and degree of crystallinity with increasing irradiation dose or PEG content. and unhydrolyzation properties, which makes it more environmentally friendly. In addition, PEG is more common which could reduce the cost of experiments and simplify the experiments process. PVA and PEG blends have been widely explored as water soluble polymers for numerous industrial, biomedical and pharmaceutical applications due to the advantages of nontoxic, non-carcinogenic and bioadhesive properties [8].The miscibility between the constituents of a polymer mixture is an important factor in the development of new materials based on polymeric blends. In miscible polymeric blends, there are often specific interactions between functional groups or polymer segments that lead to decrease of the Gibbs energy of mixing. Miscible polymer blends present only one phase, while immiscible blends present separated domains, and the final properties of polymer blends are directly related to the degree of their miscibilities [9]. In immiscible polymer blends, their physical properties are poor compared with those of parent polymers because of phase separations arising from weak interaction at the boundaries of component polymers. The miscibility and the physical properties of polymer blends can be improved by applying intermolecular interaction such as hydrogen bonding and dipole-dipole interaction between blend components. Intermolecular hydrogen bonding interaction by hydroxyl, halogen, carbonyl, and amide groups leads to the improvement of miscibility based on favorable enthalpic interaction between polymer chains. Addition of compatibilizer into immiscible polymer blends also improves the miscibility and the physical properties [6,[9][10][11][12]. For polymer-polymer miscibility investigations, the most useful techniques are electronic microscopy [13], spectroscopy [14], and thermal analysis [15]. Electron beam irradiation of polymer blends has been employed in improving the properties and miscibility of blends. High energy irradiation produces free radicals that can readily interact with each other forming crosslinking and strengthening the polymer structure. The objective of this study is to determine the effect of electron beam irradiation on the structural, physical and chemical propert...