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Co 3 (PO 4 ) 2 , AlPO 4 and the binary system Co 3 (PO 4 ) 2 -AlPO 4 with different compositions were prepared by the coprecipitation method. The structural properties of these samples were determined using XRD, DTA and FT-IR techniques. The textural properties were determined from the adsorption of nitrogen at 77 K. The surface acidity was measured by a calorimetric titration method. The samples were tested as catalysts in the dehydration of ethanol and isopropanol using a pulse microcatalytic technique. The data obtained from XRD and FT-IR indicate the amorphous structures of the prepared catalysts. An increase in Co 3 (PO 4 ) 2 content led to a decrease in the surface area and in the total pore volume and an increase in the mean pore radius. The surface acidity of the catalyst depends on the chemical composition; the surface acidity increased with an increase in the AlPO 4 content. The dehydration temperature and the distribution of acid sites are important parameters in determining the selectivity and activity of the catalyst.