A desirable feature of any parameter estimation method is to obtain as much information as possible with one experiment. However, achieving multiple objectives with one experiment is often not possible. In the field of thermal parameter estimation, a determination of thermal conductivity, volumetric heat capacity, heat addition rate, surface emissivity, and convection coefficient may be desired from a set of temperature measurements in an experiment where a radiant heat source is used. It would not be possible to determine all of these parameters from such an experiment; more information would be needed. The work presented in the present research shows how thermal parameters can be determined from temperature measurements using complementary experiments where the same material is tested more than once using a different geometry or heating configuration in each experiment. The method of ordinary least squares is used in order to fit a mathematical model to a temperature history in each case. Several examples are provided using one-dimensional conduction experiments, with some having a planar geometry and some having a cylindrical geometry. The parameters of interest in these examples are thermal conductivity and volumetric heat capacity. Sometimes, both of these parameters cannot be determined simultaneously from one experiment but utilizing two complementary experiments may allow each of the parameters to be determined. An examination of confidence regions is an important topic in parameter estimation and this aspect of the procedure is addressed in the present work. A method is presented as part of the current research by which confidence regions can be found for results from a single analysis of multiple experiments.