The aim was to investigate the use of oil palm petiole fiber (OPPF) as a source for producing nanocrystalline cellulose. OPPF was treated with alkali (NaOH) first, and bleached before the production of nanocellulose by acid hydrolysis (H2SO4). The materials obtained after each stage of treatments were characterized and their chemical compositions were determined. The produced materials were characterized using scanning electron microscope (SEM) and Fourier transform infrared (FT-IR) spectroscopy. The morphological analysis of nanocellulose displayed clear needle like structure. The extracted cellulose has smaller diameter (8