This work describes an experimental technique for obtaining, simultaneously, the thermal diffusivity and thermal conductivity of polymer materials. This technique uses experimental data from only one of the sample surfaces. It means functions using experimental and calculated temperature are defined. An objective function representing the eigenvalue phase angle is used to determine thermal diffusivity, while a least square error function is used for the thermal conductivity estimation. The sequential unconstrained optimization technique BFGS is used to calculate the search direction. In each case the golden section method is used in a one-dimensional search, followed by a polynomial approximation. A comparison with the flash method and the guarded hot plate method gives a deviation of 2.97 % and 0.63 % for thermal diffusivity and thermal conductivity, respectively, for a Polychloroethylene (PVC) sample. An uncertainty analysis is also presented.