The surface area and pore size distribution of Eucalyptus samples that were pretreated by different methods were determined by the Brunauer–Emmett–Teller (BET) technique. Three methods were applied to prepare cellulosic biomass samples for the BET measurements, air, freeze, and critical point drying (CPD). The air and freeze drying caused a severe collapse of the biomass pore structures, but the CPD effectively preserved the biomass morphology. The surface area of the CPD prepared Eucalyptus samples were determined to be 58–161 m²/g, whereas the air and freeze dried samples were 0.5–1.3 and 1.0–2.4 m²/g, respectively. The average pore diameter of the CPD prepared Eucalyptus samples were 61–70 Å. The CPD preserved the Eucalyptus sample morphology by replacing water with a non-polar solvent, CO₂ fluid, which prevented hydrogen bond reformation in the cellulose.