A rapid method has been developed for the selective determination of molybdenum in uranium-molybdenum alloy by derivative spectrophotometry without any need for the separation of the matrix element. The measurements were carried out at 376 nm in presence of hydrogen peroxide, without any interference from uranium. The determination of titanium in uranium-titanium alloy was carried out by normal spectrophotometry at 510 nm using hydrogen peroxide as the chromophoric reagent without any interference from uranium. The proposed methods are precise and accurate besides being very simple and rapid.