Activated carbon can be produced from carboneous materials. The aims of this study are 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) gave the activated carbon more porous structure. 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 Fluorescent (XRF) and surface chemical was characterized using Fourier Transformation Infrared (FTIR). It was concluded that production of activation activated carbon from coconut shell and sugarcane bagasse can be used in a lot of applications like dye absorbent and waste water treatment