Carbon aerogels were prepared by the solgel polymerization of petroleum pitches followed by ambient-pressure drying and then carbonization. Furfural and sulfuric acid were found to be the best crosslinking agent and best catalyst for the reaction system, respectively. It was necessary to add acetic acid as a cosolvent, and the volume ratio of toluene to acetic acid played an important role in the mass densities of the samples. The average diameters of the nanonetwork particles of the typical carbon aerogels thus obtained were about 30-40 nm, and their surface areas were over 360 m(2)/g. (c) 2008 Wiley Periodicals, Inc. J Appl Polym Sci 112: 309-314, 2009