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This document specifies a method for the determination of the isotopic and elemental uranium and plutonium concentrations of nuclear materials in nitric acid solutions by thermal-ionization mass spectrometry. The method applies to uranium and plutonium isotope composition and concentration measurement of irradiated Magnox and light water reactor fuels (boiling water reactor or pressurized water reactor), in final products at spent-fuel reprocessing plants, and in feed and products of MOX and uranium fuel fabrication. The method is applicable to other fuels, but the chemical separation and spike solution are, if necessary, adapted to suit each type of fuel.