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This International Standard specifies a nondestructive method for the simultaneous determination of volumetric uranium and plutonium concentrations in nitric acid feed solutions from reprocessing plants. The method is directly applicable, without interference, to the original feed solution, which typically contains about 150 g.l−1 to 300 g.l−1 uranium and 1 g.l−1 to 2,5 g.l−1 plutonium in the presence of fission products with a total β,γ-activity of up to 10 TBq.l−1.