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The removal of benzene and toluene from aqueous solutions by single and multi walled carbon nano tubes (SWCNT and MWCNT) and hybrid carbon nano tube (HCNT) were evaluated. In this study nanomaterials in a dose of 1 g/l and contact time 10 min with benzene and toluene concentrations of 10 mg/l and pH 7 were chosen. Synthetic samples were analyzed by GC/MS. In order to analysis data Design of Experiment (DOE) softwere was used. The equilibrium amount (qe) (mg/g) for SWCNT (B: 9.98 mg/g, T: 9.96 mg/g) was found higher than MWCNT and HCNT. The amount of uptake for SWCNT was T > B, that was due to increasing of water solubility and decreasing of its molecular weight. It could be concluded that recycling by heating at 105±2ºC provide better adsorption performance for recycled CNTs than their initial state. So that benzene and toluene removal efficiency improved to 99.8 percent. This study showed the SWCNTs are efficient as benzene and toluene adsorbents in environmental pollution control technology.