This paper documented the synthesis of cellulose nanocrystals (CNCs) extracted from commercially-sourced microcrystalline cellulose (MCC) via acid hydrolysis and the subsequent characterization analyses of the yield. The hydrolysis process was completed using 64% sulphuric acid at 45°C for 1 hour. The yield of (CNCs) exhibited prominent physicochemical properties. The X-ray diffraction (XRD) analysis suggested that the crystallinity degree of the CNCs was 8.94% higher than MCC sample. Meanwhile, zeta potential (ζ) analysis showed that the CNCs sample possesses highly negative surface charges of -25.6±8.24 mV. Further investigation by transmission electron microscopy (TEM) analysis revealed the rod-like morphology of the CNCs sample with average diameter of 9.36±3.81nm and 83.84% crystallinity index. Whereas, via field emission scanning electron microscopy (SEM) analysis confirmed considerable reduction in particle size and changes in surface morphology post-acid hydrolysis of the CNCs, with diameter of 7.65±2.56 nm. It is envisaged that the acid hydrolysis technique is promising in synthesizing CNCs of high crystallinity with smaller size for various possible applications, potentially as a contrast agent.