We measured levels of ambient volatile organic compounds (VOCs) at seven sites in the Pearl River Delta (PRD) region of China during the Air Quality Monitoring Campaign spanning 4 October to 3 November 2004. Two of the sites, Guangzhou (GZ) and Xinken (XK), were intensive sites at which we collected multiple daily canister samples. The observations reported here provide a look at the VOC distribution, speciation, and photochemical implications in the PRD region. Alkanes constituted the largest percentage (>40%) in mixing ratios of the quantified VOCs at six sites; the exception was one major industrial site that was dominated by aromatics (about 52%). Highly elevated VOC levels occurred at GZ during two pollution episodes; however, the chemical composition of VOCs did not exhibit noticeable changes during these episodes. We calculated the OH loss rate to estimate the chemical reactivity of all VOCs. Of the anthropogenic VOCs, alkenes played a predominant role in VOC reactivity at GZ, whereas the contributions of reactive aromatics were more important at XK. Our preliminary analysis of the VOC correlations suggests that the ambient VOCs at GZ came directly from local sources (i.e., automobiles); those at XK were influenced by both local emissions and transportation of air mass from upwind areas.