The algorithm of determining the directional coefficients thermal conductivity and specific heat for a homogeneous orthotropic solid materials by means of sensitivity analysis and dynamic sequential estimation method has been presented. Two-dimensional mathematical model of the transient heat conduction within the investigated sample was formulated using control volume method. The sensitivity analysis was carried out to the optimal selection of the places of temperature sensors (thermocouples) in consideration of accuracy of the determined quantities. The inverse heat conduction problem has been solved by means of the dynamic sequential estimation method. The exemplary results of the study are presented.