A volumetric experimental set-up used for the characterisation of hydrogen storage by adsorption in carbon materials will be presented. The measurement method has been designed for a realistic carbon storage evaluation for automotive industrial application (large volume and ambient temperature). The experimental set-up was validated and calibrated following a specific experimental protocol. Limitations and dimensioning will also be given and explained, as well as the experimental conditions for a proper use of the test bench. In addition to this, two definitions of the weight percent of hydrogen stored in a carbon material that will be used during future experiments will be given and detailed. (c) 2006 International Association for Hydrogen Energy. Published by Elsevier Ltd. All fights reserved.