The method of nonlinear parameter estimation(NPE), which is a statistical and an inverse method, is used to estimate the thermal diffusivity of the porous insulation material. In order to apply the NPE method for measuring the thermal diffusivity, and algorithm for programing suitable to IBM personal computer is established, and is studied the statistical treatment of experimental data and theory of estimation. The experimental data obtained by discrete measurement using a constant heat flux technique are used to find the boundary conditions, initial conditions, and the thermal diffusivity, and then the final values are compared with the values obtained by some different methods. The results are presented as follows:(1) NPE method is used to establish the estimation of the thermal diffusivity and compared results with experimental output shows, that this method can be applicable to define the thermal diffusivity without considering hear flux types. (2) Because of all of the temperatures obtained by the discrete measurement on each steps of time are used to estimate the thermal diffusivity. Although some error in the temperature measurements of temperature are included in estimating process, its influences on the final value are minimzed in NPE method. (3) NPE method can reduce the experimental time including the time of data collecting in a few minutes and can take smaller specimen compared with steady state method. If the tube-type furnace is used, also the adjusting time of surrounding temperature can be reduced.