High resolution K X-ray spectrometry preceded by activation with deuterons is an unexplored area in the field of activation analysis. This work describes the capabilities of this technique and evaluates its analytical potential for the specific determination of transition metals in small samples. Detection of the delayed X-rays coupled with their rate of decay provided a unique indication of the target component and its concentration. Analytical conditions are demonstrated for the elements of interest and the potential for application to the general routine determination of the transition metals and some of their isotopes, is discussed.