This paper reports the study of the free water determination in CaSO4. 2H2O, Ca(H2PO4). H2O, CaHPO4.2H2O, (NH4)2HPO4, NaCl and in urea by the classical method of ovendryxng at 100-105°C and by the vacuumdessication method at 50°C in oven under vacuum of 20 inches. The vacuum-dessication method gave best results than the oven-drying (100-105ºC) method when the hydrated salts were analysed.