Thermodesorption of n-hexane and n-nonane from the acidic and non-acidic zeolites ZSM-5 and Y was studied by means of the thermogravimetric temperature programmed equilibrated desorption (TPED) and quasi-equilibrated temperature programmed desorption and adsorption (QE-TPDA). Micropore volumes determined from the adsorption capacity of n-hexane were close to those determined by N-2 adsorption. Content and strength of acid sites in the acidic zeolites estimated by fitting the Arrhenius equation to the high temperature parts of QE-TPDA profiles of n-hexane attributed to its cracking were in agreement with their acidity characteristics obtained by IR spectroscopy of chemisorbed pyridine. The mesopore volume was determined from the QE-TPDA profiles of n-nonane. Coking observed only for QE-TPDA of n-nonane on H-USY zeolite resulted in blocking the micropores without affecting the mesopores.