Tungsten (VI) oxide, WO 3 nanoparticles were synthesized by colloidal gas aphrons (CGAs) technique. The resultant WO 3 nanoparticles were characterized by thermogravimetric-differential thermal analysis (TG-DTA) and X-Ray diffraction (XRD) measurements in order to determine the phase transitions, the crystallinity and the size of the WO 3 nanoparticles. As a comparison, transmission electron microscope (TEM) was used to investigate the size of the WO 3 nanoparticles. The result from XRD and DTA show that the formation of polymorphs WO 3 nanoparticles have the following sequence: orthorhombic (-WO 3 ) monoclinic (-WO 3 ) triclinic (-WO 3 ) monoclinic (-WO 3 ) with respect to the calcination temperature of 400, 500, 600 and 700C. No diffraction peaks were found in the X-Ray diffraction measurements for the sample heat treated at 300C (as-prepared), suggesting that an amorphous structure was obtained at this temperature whereas the crystallinity had been obtained by the other samples of the WO 3 nanoparticles at the calcination temperatures of 400, 500, 600 and 700C. It is also found that the X-Ray diffraction measurements produced an average diameter of (30 5), (50 5), (150 10) and (200 10) nm at calcination temperatures of 400, 500, 600 and 700C respectively by using Debye-Scherrer formula. The TG curve revealed that the WO 3 nanoparticles is purely anhydrous since the weight loss is insignificant (0.3 -1.4) % from 30 until 600C for the WO 3 nanoparticles calcined at 400C. Finally, the composition and the purity of the WO 3 nanoparticles have been examined by X-Ray photoelectron spectroscopy (XPS). The results indicate no significant changes to the composition and the purity of the WO 3 nanoparticle produced due to the temperature variations.