Phenol and isomeric cresols are common highly toxic atmospheric air pollutants, the determination of which requires highly effective pre-concentration methods. The aim of this work is to select the conditions for express sorption pre-concentration of phenols from an air flow on surface-layer carbon-fluoroplastic sorbents for their subsequent HPLC determination at the level of maximum permissible concentrations. This aim is achieved by using surface-layer carbon-fluoroplastic sorbents. As the optimal carbon sorbent, FAD activated carbon was selected, which provides the maximum volumes of phenol retention from the flow of analysed air. To evaluate the effectiveness of the studied sorbents, model gas mixtures with a constant phenol concentration of 50 mg/m³ were used. These mixtures were obtained by passing the air flow through aqueous solutions with a known concentration of phenols. It was found that in the selected range of volumetric air flow rates (100-500) sm³/min, the equilibrium distribution of phenols between the phases and the constancy of their concentration in the gas phase during the experiment were ensured. It was established that, ceteris paribus, the developed surface-layer sorbents can increase the concentration of phenols by a factor of 2-3 and reduce the duration of the sorption concentration stage by a factor of 1.5-2 compared to traditional volume-porous activated carbons. When implementing the analysis procedure, 15 litres of analysed air were passed through a sorption column at a flow rate of 0.5 dm³/min for 30 minutes. Phenols were desorbed directly from the sorption column using 1.5 sm³ of acetonitrile, which was analysed in a reverse phase HPLC with a fluorimetric detector. The lower limit of the range of determined concentrations of phenol and isomeric cresols was 2 μg/m³, and their MPC in atmospheric air was 10 and 5 μg/m³, respectively.