Concentrations, loads, and yields of particle-associated (hydrophobic) contaminants (PACs) in urban runoff in creeks in Austin, Texas, were characterized using an innovative approach: large-volume suspended-sediment sampling. This approach isolates suspended sediment from the water column in quantities sufficient for direct chemical analysis of PACs. During 1999-2004, samples were collected after selected rain events from each of five stream sites and Barton Springs for a study by the U.S. Geological Survey, in cooperation with the City of Austin. Sediment isolated from composited samples was analyzed for major elements, metals, organochlorine compounds, and polycyclic aromatic hydrocarbons (PAHs). In addition, at the Shoal Creek and Boggy Creek sites, individual samples for some events were analyzed to investigate within-event variation in sediment chemistry. Organochlorine compounds detected in suspended sediment included chlordane, dieldrin, DDD, DDE, DDT, and polychlorinated biphenyls (PCBs). Concentrations of PACs varied widely both within and between sites, with higher concentrations at the more urban sites and multiple nondetections at the least-urban sites. Within-site variation for metals and PAHs was smaller than between-site variation, and concentrations and yields of these and the organochlorine compounds correlated positively to the percentage of urban land use in the watershed. Loads of most PACs tested correlated significantly with suspended-sediment loads. Concentrations of most PACs correlated strongly with three measures of urban land use. Variation in suspended-sediment chemistry during runoff events was investigated at the Shoal and Boggy Creek sites. Five of the eight metals analyzed, dieldrin, chlordane, PCBs, and PAHs were detected at the highest concentrations in the first sample collected at the Shoal Creek site, a first-flush effect, but not at the Boggy Creek site. Temporal patterns in concentrations of DDT and its breakdown products varied from one event to the next. In spite of the first-flush effect in concentrations at the Shoal Creek site, most of the contaminant load was transported at peak discharge, when suspended-sediment concentration and load are maximum.