Porous materials are implemented in several industrial applications such as water desalination, gas separation and pharmaceutical care which they are mainly governed by the pore size and the PSD. Analyzing shale reservoirs are not excluded from these applications and numerous advantages can be gained by evaluating the PSD of a given shale reservoir. Because of the limitations of the conventional characterization techniques, novel methods for characterizing the PSD have to be proposed in order to obtain better characterization results for the porous materials, in general, and shale rocks in particular. Thus, permporosimetry and evapoporometry (EP) technologies were introduced, designed and utilized for evaluating the two key parameters, pore size and pore size distribution. The pore size and PSD profiles of different shale samples from Norway and Argentina were analyzed using these technologies and then confirmed by mercury intrusion porosimeter (MIP). Norway samples showed an average pore diameter of 12.94 nm and 19.22 nm with an average diameter of 13.77 nm and 23.23 nm for Argentina samples using permporosimetry and EP respectively. Both techniques are therefore indicative of the heterogeneity of the shales. The results from permporosimetry are in good agreement with those obtained from MIP technique, but EP for most part over-estimates the average pore size. The divergence of EP results compared to permporosimetry results is referred to the fact that the latter technique measures only the active pores which is not the case with the former technique. Overall, both techniques are complementary to each other which the results from both techniques seem reasonable and reliable and provide two simple techniques to estimate the pore size and pore size distributions for shale rocks.