The paper is a review of the procedures for the determination of volatile and semivolatile oxygenated organic compounds (O-VOCs) in effluent samples by gas chromatography. Current trends and outlook for individual steps of the procedure for the determination of O-VOCs in effluents are discussed. The available sample preparation techniques and their limitations are described along with GC capillary columns used for O-VOCs separation and selective and universal detectors used for their determination. The results of determination of O-VOC content in various types of real effluents are presented. The lack of legal regulations regarding the presence of the majority of O-VOCs is pointed out as well as the availability of just a few procedures allowing a comprehensive evaluation of the O-VOC content in effluents.