Nanoparticles from different cellulosic sources were prepared via hydrolysis using three different acids. Cellulose, Methylcellulose (MC), Cellulose acetate (CA), Propylcellulose (PC) and Ethylcellulose (EC) was hydrolyzed using pulp-to-liquid ratio of 4.57:1 under 1/3/6 h hydrolysis. Different particles ranging from 70 -1580 nm were obtained. The maximum yield (55.3 %) was attained at 3 h hydrolysis with H 3 PO 4 acid, and particle size decreased with increasing reaction time as revealed by SEM and fiber length histograms and BET. Most fibers had pore area around 0.41 µm2. Nanoparticles obtained from all cellulose derivative used had low crystallinity index value attributed to substituent groups. The TGA showed that the prepared nanoparticles have thermal stability at T95 and T90 (5 and 10 wt % mass loss) in the temperature range of 297.51-411.09 o C and 315-508.55 o C with Tmax, 375-525 o C respectively. An extended temperature range was observed for some samples over the whole temperature range with only 50 wt % mass loss of the nanomaterials. FT-IR spectroscopy was employed to study the characteristic functionalities found in crystalline cellulose. BET analysis of samples gave evidences of the nanoparticles possessing large surface area of between 105.698 m2/g and 250.570 m2/g. The Langmuir surface area was 10336.157 m2/g, while the pore size and pore volume, ranged from 1.324 -9.237 nm and 0.01427 -0.07939 cm3/g respectively. The three different acids used gave various yields of nanocrystals with H 3 PO 4 having the highest yield of 55.3 %, followed by HCl, (34.8 %) while H 2 SO 4 has the lowest yield of 30 %. All of these yields were obtained under the same reaction conditions during 3 h hydrolysis. All samples hydrolyzed for 6 h gave low yield, 28.2 % of nanoparticles. The 3 h hydrolysis was the optimum reaction time for the generation of nanoparticles using 4.57 mL/g solid-liquid ratio.