The aim of this study is to synthesis and characterize activated carbon from Cocos nucifera L. (coconut) shell and sugarcane bagasse by carbonization and activation process. The samples were carbonized and activated at 300°C in a furnace. As the concentration of activating agent increased, the percentage of weight loss also increased due to more volatiles in samples that were released. Addition of phosphoric acid (H3PO4) and potassium hydroxide (KOH) resulting more porous structure in the activated carbon. The result indicated that the activated carbon derived from coconut shell has higher carbon content compared to sugarcane bagasse. Besides, the elements that contained in the samples were analysed using X-ray Diffraction (XRD) and surface chemical was characterized using Fourier Transformation Infrared-Attenuated Total Reflection (FTIR-ATR). It was concluded that production of activated carbon from coconut shell and sugarcane bagasse can be used in a lot of applications like dye absorbent for waste water treatment.