In this research work, adsorption of VOC (here gasoline vapor) onto synthesized activated carbon (AC) from mesquite grain was investigated. AC was prepared using chemical activation method (with two-step, activation and paralyze) and phosphoric acid as activating agent. Also, the effect of important factors on the surface area and finally the adsorption capacity such as the phosphoric acid ratio to the raw material (RM), time and tem- perature of calcination were studied. Several techniques such as FT-IR, XRD, XPS, TPD, Boehm titration, BET, CHNs, SEM, and TGA/DTA, have been used to determine and confirm physicochemical surface variation during preparing and modifying the adsorbent. It was observed that activation by phosphoric acid at 600 ◦C and a 2 hr (i.e AC5:1.1–2–600) gives a surface area of 1452.4 m2/g. The AC5:1.1–2–600 displayed high adsorption capacity for VOC adsorption (642.86 mg.g