Abstract In the present work is reported the synthesis and characterization (by infrared spectroscopy, X-ray diffractometry. X-rayfluorescence and SEM microscopy) of the vanadylphospahtes: VOPO4.2H2O, VOHPO4.0.5H2O, CoVOPO4.2H2O, MnVOPO4.3H2O, CrVOPO4.2H2O and AlVOPO4.2H2O. The prepared matrices had their adsorption capacities towards ammonia tested. The obtained adsorption capacities (mg/g) are as follows: 112.1, 96.6, 125.1, 200.4, 145.1 and 216.8, respectively.