This study examines the influence of analytical particle size on the surface area and mesopore and micropore volume data obtained from low-pressure N2 and CO2 adsorption analyses in response to the crushing of coal and shale. Pennsylvanian high-volatile bituminous coal (Ro~0.57%) and Devonian to Lower Mississippian low-maturity (Ro~0.57%) and high-maturity (Ro~1.30%) shales from the Illinois Basin were progressively crushed from chunks (~7mm) to 4mesh (<4.78mm), 7mesh (<2.83mm), 18mesh (<1mm), 30mesh (0.595mm), 60mesh (<0.250mm), 200mesh (<0.074mm), and 230mesh (<0.063mm), and, subsequently, low-pressure N2 and CO2 adsorption analyses were performed on all the grain size fractions. Our results demonstrate that the values of both surface area and specific mesopore and micropore change with progressive crushing. For example, BET surface area of coal shows a steady increase from 2m2/g in the 4mesh fraction to 4.7m2/g in the 200mesh fraction. For comparable size ranges, BET surface area changes from 0.15 to 7.82m2/g in the low-maturity shale, and from 0.02 to 6.26m2/g in the high-maturity shale. Changes in mesoporosity and microporosity parameters indicate that the coarsest fractions (4mesh and larger) are not suitable for low-pressure adsorption analysis; the values are very low and not reproducible dominantly because of equilibration problems. Our results demonstrate that the 60mesh fraction for coal and the 200mesh fraction for shales seem to be optimal and the most practical sizes for performing low-pressure N2 and CO2 adsorption analysis; these analytical particle sizes yield results closest to the “real” values, unbiased by disequilibrium.