This work reports the syntheses of an inexpensive and efficient asphalt-derived mesoporous carbon (AdMC) as an adsorbent. The adsorbent was activated with potassium hydroxide to increase its surface area and then characterized by SEM–EDS, FT-IR, and BET. The adsorption properties of AdMC were evaluated for the adsorptive removal of eleven Poly Aromatic Hydrocarbons (PAHs) and diesel from water samples. The prepared AdMC showed very high surface areas and high micropore volumes equal to 2316 m2/g and 1.2 cm3/g, respectively. Various experimental conditions influencing the adsorption capacity of eleven PAHs and diesel were investigated. At high concentrations, PAHs and diesel solubility in water is very low. Hence, samples were emulsified with a surfactant, and then maximum adsorption capacity was investigated. Adsorption profile of individual PAHs was examined using gas chromatography/mass spectrometry analysis followed by liquid–liquid extraction. Total hydrocarbon removal was studied using a total organic analyzer. Asphalt-derived mesoporous sorbent showed an extreme ability to remove PAHs and diesel (average adsorption capacity of 166 mg/g for individual PAHs and diesel (maximum capacity of 1600 mg/g). The experimental results fitted the Langmuir model with a correlation efficiency of 0.9853. The results obtained for both adsorbents also matched to pseudo-second-order kinetics, suggesting that the adsorption of PAHs and diesel is chemical, monolayer, and homogeneous process.