Separation of molybdenum and vanadium from hydrochloric and sulfuric acid solution containing 0.2 g/L Mo (VI) and 0.2 g/L V (V) was tried by ion exchange. Loading behavior of the two metals from moderate to strong acid solution was investigated using cationic (Diphonix) and anionic (AG1-x8) resins. The highest separation factor was obtained by ion exchange with AG1-x8 from sulfuric acid solution at pH 1.2, where no V was loaded. The loading capacity of AG1-x8 for Mo from sulfuric acid solution at pH 1.2 was 176 mg/g. Continuous column experiments demonstrated complete separation of the metals by selectively loading Mo from the feed. The molybdenum in the loaded resin was eluted by the use of NaOH solution.