Abstract: A method for determination of molybdenum in molybdenum-iron alloys by inductively coupled plasma-atomic emission spectrometry has been developed. Compared with the classical chemical methods, the new method provides the advanges of high accuracy, high precision, high efficiency and low labor intensity. The method has replaced the original chemical methods and has been applied to routine analysis of molybdenum in molybdenumiron alloys with satisfactory results.