The increasing presence of siloxanes in waste activated sludge (WAS) considerably hampers the energy use of the biogas obtained during the anaerobic digestion of the sludge when concentrations exceed critical limits. To prevent the occurrence of unacceptable operating conditions, it is hence necessary to have a reliable analysis method for determining the siloxane content of the sludge. This paper describes and validates such a method, consisting of the extraction of the siloxanes using n-hexane and a subsequent analysis of the extract using GC-FID. The validation procedure confirms the excellent recovery and repeatability of the proposed method. (c) 2007 Elsevier B.V. All rights reserved.