An analytical protocol is described which allows parallel quantification of sewage, oil and PAH pollution on the same samples, thus maximizing the information gained for the effort expended. Capillary gas chromatography-flame ionization detection (GC-FID), now a routine technique in many laboratories, has been selected as the method for quantification. The protocol described is evaluated, and analyses of sediments from estuaries of the Rivers Mersey, Dee and Tamar, UK, are given as examples of how to interpret results achieved using the technique.