An automated cleanup system (Power-Prep , Fluid Management Systems, Inc.) was evaluated for the analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/PCDF) in environmental samples. The study was firstly carried out against standard mixtures containing labeled and unlabeled PCDD/PCDF and a certified reference material (fly ash CRM 490). Next, a comparison between a conventional cleanup procedure and the new automated system for PCDD/PCDF analysis in environmental samples such as flue gas emissions, fly ashes, sludges, ambient air and soils was also made. The suitability of the system was finally assessed from the participation in an interlaboratory exercise. Owing to its capability to successfully perform the sample cleanup the Power-Prep apparatus is an alternative to the conventional methods.