Recent research interest has been focused on the successful synthesis of Nanocrystalline Cellulose (NCC). NCC which can be isolated from natural fibre possesses exclusive properties such as large surface area, high aspect ratio, biocompatibility and exceptional mechanical properties for various industry applications. In this study, NCC was isolated from palm oil biomass waste, i.e. empty fruit bunch (EFB) through various stages of chemical treatments. This multistep process embrace a bleaching and alkali treatment to efficiently remove impurities, waxy substances, hemicellulose and lignin from EFB fibre, and the remaining cellulose product was acid hydrolysed into nanocellulose material. Hence, as an evidence the products obtained from each stage were characterized by using Fourier Transform Infrared Spectroscopy (FTIR) to identify the presence of functional groups in cellulose. Additionally, Dynamic Light Scattering (DLS) technique showed NCC with an average particle size of 499.2 nm was obtained.