The occurrence and spatial-temporal variability of 25 volatile organic compounds (VOCs) was studied from May 1998 to November 2000 in the Scheldt estuary. Target VOCs were selected from lists of priority pollutants to the North Sea, and included chlorinated short-chain hydrocarbons (CHCs), monocyclic aromatic hydrocarbons (MAHs) and chlorinated monocyclic aromatic hydrocarbons (CMAHs). Samples were taken between Vlissingen and Temse over a 95 km trajectory, and analysed by purge-and-trap and high resolution gas chromatography-mass spectrometry. Data were attended by analyses deemed ‘in control’ by a rigorous quality assurance/quality control program, as proposed by Quality Assurance of Information for Marine Environmental Monitoring in Europe (QUASIMEME). CHCs were among the most commonly found VOCs in the estuary, ranging from a few ng l-1 to several µg l-1. Most analytes were traceable to a single input source in the upper part of the estuary, which is densely populated and highly industrialized. By contrast, the occurrence of MAHs resulted from contributions of a wide spectrum of sources. The CMAHs were less abundant in the water column, and were mainly detected as chlorobenzene and 1,4-dichlorobenzene. Concentrations of several priority VOCs have markedly decreased since 1995 owing to emission reduction efforts within international frameworks for the protection of the North Sea.