Volatile organic compounds (VOCs) have been determined to be human risk factors in urban environments, as well as primary contributors to the formation of photochemical oxidants. Ambient air quality measurements of 54 VOCs including hydrocarbons, halogenated hydrocarbons and carbonyls were conducted in or near 13 urban locations in the United States during September 1996 to August 1997. Air samples were collected and analyzed in accordance with US Environmental Protection Agency-approved methods. The target compounds most commonly found were benzene, toluene, xylene and ethylbenzene. These aromatic compounds were highly correlated and proportionally related in a manner suggesting that the primary contributors were mobile sources in all the urban locations studied. Concentrations of total hydrocarbons ranged between 1.39 and 11.93 parts per billion, by volume (ppbv). Ambient air levels of halogenated hydrocarbons appeared to exhibit unique spatial variations, and no single factor seemed to explain trends for this group of compounds. The highest halogenated hydrocarbon concentrations ranged from 0.24 ppbv for methylene chloride to 1.22 ppbv for chloromethane. At participating urban locations for the year of data considered, levels of carbonyls were higher than the level of the other organic compound groups, suggesting that emissions from motor vehicles and photochemical reactions strongly influence ambient air concentrations of carbonyls. Of the most prevalent carbonyls, formaldehyde and acetaldehyde were the dominant compounds, ranging from 1.5-7.4 ppbv for formaldehyde, to 0.8-2.7 ppbv for acetaldehyde.