For the first time, highly porous hypercrosslinked polystyrene layer was synthesized within a gas chromatography capillary column and successfully deposited onto the capillary walls generating porous layer open-tubular capillary column.Elaborated three steps synthetic procedure provides tightly bonded porous polymeric layer and ensues complete elimination of particle shedding and the needs for particle traps. Due to highly developed surface area, porous layer opentubular column provides strong solute retention that is useful for the separation of various volatile solvents and light gas compounds including ethane, ethylene, ethyne. Aqueous injections will not harm the column.