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The present work analyzes the effect of process variables and the method of characterization of cellulose micro/nanofibers (CMNFs) obtained by different treatments. A chemical pre-treatment was performed using oxalic acid at 25 wt.% and 50 wt.%. Moreover, for mechanical pre-treatments, a rotary homogenizer or a PFI mill refiner were considered. For the mechanical fibrillation to obtain CMNFs, 5 and 15 passes through a pressurized homogenization were considered. The best results of nanofibrillation yield (76.5%), transmittance (72.1%) and surface charges (71.0 µeq/g CMNF) were obtained using the PFI mill refiner, 50 wt.% oxalic acid and 15 passes. Nevertheless, the highest aspect ratio (length/diameter) determined by Transmission Electron Microscopy (TEM) was found using the PFI mill refiner and 25 wt.% oxalic acid treatment. The aspect ratio was related to the gel point and intrinsic viscosity of CMNF suspensions. The values estimated for gel point agree with those determined by TEM. Moreover, a strong relationship between the intrinsic viscosity [η] of the CMNF dispersions and the corresponding aspect ratio (p) was found (ρ[η] = 0.014 p2.3, R2 = 0.99). Finally, the tensile strength of films obtained from CMNF suspensions was more influenced by the nanofibrillation yield than their aspect ratio.