Solid-phase extraction (SPE) protocols were developed for the determination of oil and grease in waste water. SPE was found to be an efficient alternative to standard methods. Both synthetically spiked samples and environmentally contaminated samples were examined. Analysis times and organic solvent consumption were decreased by the SPE procedure compared with liquid–liquid extraction (LLE). Recovery and variability studies of environmentally contaminated samples indicated that SPE results using methylene chloride as an extractant were comparable to those obtained by continuous liquid–liquid extraction using a chlorofluorocarbon (CFC). Extractions performed by manually shaken separating funnel LLE with CFCs were found to be matrix dependent when compared with SPE results. Suitable alternative elution solvent systems for SPE, including hexane, hexane–diethyl ether, ethyl acetate and methyl tert-butyl ether, were also examined.