A new type of high-performance capillary columns for gas chromatography, monolithic capillary columns, have been studied, which are characterized by a high loading capacity, a high efficiency, and good deactivation of the capillary wall as early as the step of preparing a monolithic stationary phase. The feasibility of separation of both gaseous and liquid samples at a high carrier-gas pressure has been shown. The influence of temperature programming on the separation properties of the monolithic columns has been examined, and it has been shown that temperature programming on monolithic columns is a convenient and effective means of accelerating gas chromatographic determination of compounds of many classes. DOI: 10.1134/S0965544112060084