A non-destructive simultaneous method has been developed for the rapid determination of Al, Si and K in WO3 powders and W metal powders. The samples were activated by 14 MeV neutrons and the radioactive isotopes identified by their γ-ray spectra with a 3″×3″ NaI(Tl) detector. Quantitative analysis was carried out by measuring the full energy peak areas. The determined concentrations of Al, Si and K were above 100, 100 and 500 ppm, the sensitivities being about 20, 10 and 100 ppm, respectively.