The blending of polymers is of great interest, since the modification gives rise to diverse physical properties with the functionality of a polymer, without synthesis. Water-soluble antitumor-active poly(maleic anhydride-alt-acrylic acid) poly(MA-alt-AA) and poly(ethylene glycol) (PEG) blends were prepared by casting, and compatible properties were investigated by dilute solution viscometry. Viscosity measurements were made on ternary systems of polymer (1)/polymer (2)/solvent (H2O) and p-dioxane, at different concentrations of PEG and poly(MA-alt-AA). The interaction parameters Δβ, μ, Δk, Δb, β and α, which have been proposed, have been obtained using the viscosity data, to probe the miscibility of the polymer blends. The solid blends prepared were characterized with ATR-FTIR, (1)H-NMR, DTA and TGA.