The presence of volatile organic compounds (VOCs) from traffic and other sources in urban areas is a cause for concern about public health. Canister, chemical derivatisation, particulate sampling and adsorption sampling techniques were used to measure VOC concentrations of a wide range of compounds (C6-C40) during a four day campaign in south London with subsequent laboratory analysis of the samples. Compounds quantified included alkanes, mono- and poly-nuclear aromatic hydrocarbons. Also the first sequential measurements of carbonyl compounds (C1-C8) in a UK urban area are presented. Results from canister and adsorption sampling methods are compared. A comparison of the results with other urban data is presented and the temporal variations in VOC concentrations were interpreted with reference to the prevalent wind speeds and directions. The CALINE4 line source dispersion model was generally successful in reproducing the daytime 12 hour average concentrations of selected VOCs.