This paper presents study on methane/steam reforming process and method to develop effective experimental-calculation procedure to deliver the reliable kinetic reaction rate expression with the decreased number of necessary experimental measurements for the calculations of the empirical parameters. The experimental studies were conducted on the NiO/YSZ (60/40vol%) catalyst, one of the most typical materials, for Solid Oxide Fuel Cell anodes. By the analysis with the Orthogonal Least Squares method and an analysis of a-posteriori covariance matrix, the experimentation process has been optimized. The proposed systematic approach was applied to evaluate the minimal number of measurements required to achieve the assumed accuracy of final solution and to reveal the influence of distribution of experimental condition for the quality of final reaction kinetic equation. It was proved that the number of experimental measurements can be reduced without significant deterioration in the quality of solution, if the dismissed measurements are properly chosen.