The stress relaxation of poly(methyl acrylate)-poly(acrylonitrile) copolymer samples was carried out in air, distilled water, pH 3, 7 and 11 solutions at various temperatures using a tensile tester equipped with a solvent chamber. The relaxation spectra of poly(methyl acrylate)-poly(acrylonitrile) copolymers were obtained by applying the experimental stress relaxation curves to the equation of relaxation spectrum derived from the Ree-Eyring and Maxwell model. The determination of relaxation spectra was performed from computer calculation using a Laplace transform method. It was observed that the relaxation spectra of these samples are directly related to the distribution of molecular weights and self-diffusions of flow segments.