A rapid and simple analytical method for the determination of organochlorines, such as polychlorinated biphenyls (PCBs) and selected organochlorinated pesticides (OCPs) and organobromines, such as polybrominated diphenyl ethers (PBDEs), in sediment samples was optimised using CRM 536 (PCBs in freshwater sediment). The method involved a hot Soxhlet extraction that reduced the extraction time to 2 h. Elemental sulphur, which is present in sediments and may interfere during the analysis, was removed by means of copper powder added to the sediment during extraction and into the clean-up cartridge. The analysis of PCBs and OCPs was accomplished by gas chromatography with electron capture or mass spectrometric detection. Similar quantitative results for PCB congeners in CRM 536 were obtained using a 50-m capillary column and a 10-m narrow bore column suited for fast analysis. The analysis of PBDEs was done by mass spectrometry in negative chemical ionisation mode. Concentrations of organic pollutants in two sediment cores (approximately 50 cm depth) from the Scheldt river (south of Antwerp, Belgium) showed a relative steady state for PCBs and DDTs, with a slight decrease in the top layers, suggesting a slight decline in their concentrations due to restrictions in their usage. On the contrary, PBDEs were showing an increase in their concentrations in the top layers (up to 270 and 8400 ng/g dry weight for sum of tri- to hexa-BDE congeners and for BDE 209, respectively). This suggests an increasing trend in the concentrations of PBDEs in the Belgian environment.