Nickel aluminide (Ni3Al) intermetallic compound was prepared by a conventional powder metallurgy technique. Ni and Al powder were mixed in a ball mill for 4 hours at 350 rpm. The mixed sample was then compacted using a hydraulic press at 400Mpa for 15 minutes. The formation of Ni3Al was monitored by the presence of a 'large' exothermic peak of the differential thermal analysis curve, which occurred around 648degreesC. The Ni3Al formation was also monitored by X-Ray Diffraction (XRD) measurements. The intensity of the XRD peak observed at 36degrees increases indicating the formation of gamma-Al2O3. The saturation magnetization (Ms) of the sample sintered for 5 samples was reduced to a very low value indicating the presence of a low amount of elemental Ni. The Ms however, increased drastically when the sample sintered for 7 hours because of the formation of a large amount of gamma-Al2O3 leaving more Ni unreacted.