By employing the method of inverse gas chromatography and using the retention diagrams of methanol and heptane in the temperature range between −55 and + 180°C, the glass transition temperatures, T g, were determined for glycidyl methacrylate—ethylene dimethacrylate ( T g = 40°C) and styrene—divinylbenzene ( T g = 100°C) macroporous copolymers. The standard method (differential thermal analysis) failed in these instances. For macroporous copolymers, a disturbance is observed in the dependence on reciprocal of temperature, not only for the retention volume, but also for the peak asymmetry, width and area, which is proportional to the response. Using the dependence log V MeOH/ V C 7 H 16 , not only T g, but also a change in the polarity of the individual types of copolymers can be determined. At low temperatures (−55°C), the polarities of macroporous copolymers approach each other owing to the “freezing” of polymer chains. Constant properties are assumed by the polymer surface only above T g where the polarity decreases in the order macroporous glycidyl methacrylate—ethylene dimethacrylate copolymer, the above methacrylate copolymer with chemically bonded PEG and styrene—divinylbenzene copolymer (Synachrom E5). A similar picture of the polarity of these polymers is also provided by the enthalpy of solution (Δ H s) and enthalpy of adsorption (Δ H a) of methanol and heptane determined for the copolymers investigated.