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This part of ISO 15366 describes procedures to chemically separate and purify uranium and plutonium in dissolved solutions of irradiated light water reactor fuels and in samples of high active liquid waste of spent fuel reprocessing plants, prior to their isotopic analysis by e.g. mass spectrometric method (see ISO 8299[1]) or alpha spectrometry (see ISO 11483[2]).This part of ISO 15366, describes a technique for the separation of uranium and plutonium in spent fuel type samples based on chromatographic method. The procedure applies to samples containing 1 µg to 150 µg Pu (IV) and (VI) and 0,1 mg to 2 mg U (IV) and (VI) in up to 2 ml of 3 mol·l-1 nitric acid solution. It is applicable to mixtures of uranium and plutonium in which the U/Pu-ratio can range from 0 up to 200.