A rapid, non-destructive method is presented for the determination molybdenum and cobalt in hydrodesulfurization catalysts employing a PDP-11/05 computer-base radioisotope x-ray fluorescence technique. Precision for molybdenum and cobalt better than 2.5% and 4.0%, respectively, are achieved in 100 sec of fluorescent time. The values obtained by this method are in agreement with values from atomic absorption and neutron activation methods. Besides being nondestructive, only about 50 mg of sample is needed, and no time-consuming acid dissolution is required as in atomic absorption and colorimetric methods. The results for six different commercial catalysts are compared with determinations by atomic absorption, neutron activation analysis methods as well as an x-ray fluorescence system with manual calculations of the percentage of molybdenum and cobalt.