In a study conducted in late summer 2000, a wide range of volatile organic compounds (VOCs) were measured throughout five target cities in the Pearl River Delta (PRD) region of south China. Twenty-eight nonmethane hydrocarbons (NMHCs; 13 saturated, 9 unsaturated, and 6 aromatic) are discussed. The effect of rapid industrialization was studied for three categories of landuse in the PRD: industrial, industrial-urban, and industrial-suburban. The highest VOC mixing ratios were observed in industrial areas. Despite its relatively short atmospheric lifetime (2–3 days), toluene, which is largely emitted from industrial solvent use and vehicular emissions, was the most abundant NMHC quantified. Ethane, ethene, ethyne, propane, n-butane, i-pentane, benzene, and m-xylene were the next most abundant VOCs. Direct emissions from industrial activities were found to greatly impact the air quality in nearby neighborhoods. These emissions lead to large concentration variations for many VOCs in the five PRD study cities. Good correlations between isoprene and several short-lived combustion products were found in industrial areas, suggesting that in addition to biogenic sources, anthropogenic emissions may contribute to urban isoprene levels. This study provides a snapshot of industrial, industrial-urban, and industrial-suburban NMHCs in the five most industrially developed cities of the PRD. Increased impact of industrial activities on PRD air quality due to the rapid spread of industry from urban to suburban and rural areas, and the decrease of farmland, is expected to continue until effective emission standards are implemented.