A comparative Study was carried out for highly ordered mesoporous materials using high resolution thermogravimetry (HR-TG) and adsorption techniques. These materials were synthesized with mixed surfactants of various alkyl chain lengths. For thermogravimetry measurements n-butanol was used to probe the adsorbent surface and high-resolution TG curves as well as their 1st and 2nd derivatives were obtained for this probe molecule. It is shown that the values of the mesopore volume and specific surface area evaluated from TG data are in a good agreement with those evaluated from low-temperature nitrogen adsorption isotherms. This comparative study was performed to confirm the usefulness of the HR-TG technique as, an alternative method for evaluation of the mesopore volume and specific surface area of ordered mesoporous materials. (c) 2005 Elsevier Inc. All rights reserved.