Analytical Sciences

Preparation, Certification and Validation of a Stable Solid Spike of Uranium and Plutonium Coated with a Cellulose Derivative for the Measurement of Uranium and Plutonium Content in Dissolved Nuclear Fuel by Isotope Dilution Mass Spectrometry

Naoki SURUGAYA,* Toshiaki HIYAMA,* André VERBRUGGEN,** and Roger WELLUM**

*Japan Atomic Energy Agency, 4-33 Muramatsu, Tokai, Naka, Ibaraki 319-1194, Japan
**European Commission, Joint Research Center, Institute for Reference Materials and Measurements, Retiesweg 111, 2440 Geel, Belgium

A stable solid spike for the measurement of uranium and plutonium content in nitric acid solutions of spent nuclear fuel by isotope dilution mass spectrometry has been prepared at the European Commission Institute for Reference Materials and Measurements in Belgium. The spike contains about 50 mg of uranium with a 19.838% ²³⁵U enrichment and 2 mg of plutonium with a 97.766% ²³⁹Pu abundance in each individual ampoule. The dried materials were covered with a thin film of cellulose acetate butyrate as a protective organic stabilizer to resist shocks encountered during transportation and to eliminate flaking-off during long-term storage. It was found that the cellulose acetate butyrate has good characteristics, maintaining a thin film for a long time, but readily dissolving on heating with nitric acid solution. The solid spike containing cellulose acetate butyrate was certified as a reference material with certified quantities: ²³⁵U and ²³⁹Pu amounts and uranium and plutonium amount ratios, and was validated by analyzing spent fuel dissolver solutions of the Tokai reprocessing plant in Japan. This paper describes the preparation, certification and validation of the solid spike coated with a cellulose derivative.

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