Laboratory-scale analysis of natural rocks provides petrophysical properties such as density, porosity, pore diameter/pore-throat diameter distribution, and fluid accessibility, in addition to the size and shape of framework grains and their contact relationship with the rock matrix. Different types of laboratory approaches for petrophysical characterization involve the use of a range of sample sizes. While the sample sizes selected should aim to be representative of the rock body, there are inherent limitations imposed by the analytical principles and holding capacities of the different experimental apparatuses, with many instruments only able to accept samples at the μm–mm scale. Therefore, a total of nine (three limestones, three shales, two sandstones, and one dolomite) samples were collected from Texas to fill the knowledge gap of the sample size effect on the resultant petrophysical characteristics. The sample sizes ranged from 3 cm cubes to <75 μm particles. Using a combination of petrographic microscopy, helium expansion pycnometry, water immersion porosimetry, mercury intrusion porosimetry, and (ultra-) small-angle X-ray scattering, the impact of sample size on the petrophysical properties of these samples was systematically investigated here. The results suggest that the sample size effect is influenced by both pore structure changes during crushing and sample size-dependent fluid-to-pore connectivity.

By using gas physisorption and multifractal theory, this study analyzes pore structure heterogeneity and influencing factors during thermal maturation of naturally immature but artificially matured shale from the Kongdian Formation after being subjected to hydrous pyrolysis from 250 °C to 425 °C. As thermal maturity increases, the transformation of organic matter, generation, retention, and expulsion of hydrocarbons, and formation of various pore types, lead to changes in pore structure heterogeneity. The entire process is divided into three stages: bitumen generation stage (250–300 °C), oil generation stage (325–375 °C), and oil cracking stage (400–425 °C). During the bitumen generation stage, retained hydrocarbons decrease total-pore and mesopore volumes. Fractal parameters ΔD indicative of pore connectivity shows little change, while Hurst exponent H values for pore structure heterogeneity drop significantly, indicating reduced pore connectivity due to bitumen clogging. During the peak oil generation stage, both ΔD and H values increase, indicating enhanced pore heterogeneity and connectivity due to the expulsion of retained hydrocarbons. In the oil cracking stage, ΔD increases significantly, and H value rises slowly, attributed to the generation of gaseous hydrocarbons further consuming retained hydrocarbons and organic matter, forming more small-diameter pores and increased pore heterogeneity. A strongly negative correlation between ΔD and retained hydrocarbon content, and a strongly positive correlation with gaseous hydrocarbon yield, highlight the dynamic interaction between hydrocarbon phases and pore structure evolution. This study overall provides valuable insights for petroleum generation, storage, and production.