This review focuses on a number of key procedural steps in the analysis of volatile organic compounds (VOCs) in estuarine waters. The most critical step, from an analytical point of view, is sample preparation. So far, only purge-and-trap and, to some extent, membrane inlet mass spectrometry have successfully been applied in estuarine monitoring of VOCs. The advantages and disadvantages of both techniques are discussed and novel developments are reviewed. Other key elements in VOC analysis and assessment include quality assurance (QA), quality control (QC) and statistical data analysis. This paper gives a brief overview of QA/QC measures of interest in the estuarine monitoring exercise, and provides guidelines for adequate statistical treatment of environmental data. Finally, field measurements of VOCs in estuarine waters are reviewed. Concentrations are reported, and distribution patterns, sources and time-trends are discussed. In addition to data, results of a 3-year monitoring survey (May 1998-November 2000) in the Scheldt estuary are presented.