Volatile organic compounds (VOCs) are widespread environmental pollutants that can result in serious environmental and health problems. VOCs consist of aromatic compounds such as toluene or benzene as well as many aliphatic compounds such as n-hexane or 2-methylbutane and are among the most common air pollutants emitted from chemical, petrochemical and related industries. Because of their high vapor pressure, VOCs can easily evaporate into the atmosphere, causing air pollution by the formation of photochemical ozone and secondary organic aerosol (SOA). Recently, emissions of VOCs have become one of the most stringent environmental challenges due to stringent regulations imposed to control the VOCs emissions [1,2]. There are a number of technologies commercially available for VOCs abatement, among which adsorption is a reliable chemical engineering method widely used because of the flexibility of the system, low energy consumption and cheap operation costs. Adsorption on granular activated carbon is one of the well-known used methods for VOCs recovery from gaseous stream. However, activated carbons have some important drawbacks such as the self-firing of the adsorbent and the difficulty in the regeneration of the spent adsorbents [3-6]. Therefore, it is necessary to develop new adsorbent materials to separate and recover VOCs from polluted air streams. In this context, this work discusses the removal of n-hexane vapors by adsorption on two non-functionalized hypercrosslinked polymers type Macronet, MN 202 and MN 250 compared with adsorption of n-hexane vapors on granular activated carbon AC 20, in static conditions. Also, the influence of some parameters like n-hexane concentration vapors, atmospheric humidity and the adsorption equilibrium in static conditions were investigated. All the experiments were performed in headspaces vials and the analysis of VOCs concentration was determined by gas-chromatograph equipped with FID (through Gastight syringe). The results show that the experimental adsorption capacity for n-hexane vapors is greater for polymeric resins that for GAC-AC 20 and the performance of adsorption processes, in all experimental conditions studied, is realized in order MN 250 > AC 20 > MN 202. Also, the experimental adsorption isotherm data were fitted to the Freundlich, Langmuir I and Langmuir II models. The results show that the adsorption equilibrium of n-hexane vapors in static conditions is well defined by Freundlich model indicating a heterogeneous adsorption on all three adsorbents studied, MN 250, MN 202 and AC 20.