ZrO2-SO4 powders have been prepared by following a single-step sol-gel preparative route using zirconium propoxide as the starting compound. Sulfuric acid was employed both as the sulfating agent and as the catalyst of the polycondensation reaction in the gel formation. Two different series of dried precursors were obtained by either evaporating the solvent in an oven at 100 degreesC (xerogels) or in supercritical conditions (aerogels). All the samples were calcined at three temperatures (470, 550, and 630 degreesC) for the same time length (5 h). The powders were characterized for phase composition-crystallinity, surface area-porosity, sulfur content and surface state (XPS). The catalytic activity of the calcined samples was tested in the isomerization of n-butane in a continuous system at 150 degreesC in absence of H-2 and 250 degreesC in presence of H-2. The role played by the conditions of the solvent elimination, at the end of the sol-gel reaction, in affecting the physicochemical and catalytic properties of the powders is discussed.