Sulfated zirconia catalysts with surface areas in excess of 200 m(2)/g have been prepared by refluxing pH adjusted freshly precipitated hydrous zirconia for 20 h at 90 degrees C followed by sulfuric acid treatment. Calcination at 550 degrees C results in a sulfated zirconia catalyst possessing n-butane isomerization activity superior to conventional ambient preparations. The X-ray diffraction patterns of these high surface area catalysts contained only a broad, low-intensity reflection in place of the distinct (111) peak of tetragonal zirconia normally observed in conventional sulfated zirconia catalysts.