Optimal conditions (temperature, porous structure and configuration of mass exchange layer in the chromatomembrane cell, and also the direction of water sample and extractant gas flows through it) for the chromatomembrane gas extraction of volatile organic compounds from aqueous solutions in combination with the gas-adsorption preconcentration of the analytes are selected. An analysis scheme based on a combination of these methods and a two-step thermal desorption of analytes ensures the shortening of the preconcentration time by several times compared to the schemes involving traditional bubbling. Metrological characteristics are given and the accuracy of the developed scheme of analysis is proved.