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Preparation and certification of Large-Sized Dried (LSD) Spike - IRMM-1027p

IRMM Large-Sized Dried (LSD) Spikes are widely used as a fundamental part of the fissile material control of irradiated nuclear fuel and have been provided on a regular basis to safeguards authorities and industry for more than 10 years. This report describes the preparation and certification of a new batch of LSD Spikes. IRMM-1027p is a dried nitrate material in cellulose acetate butyrate (CAB), certified for the mass of uranium and plutonium and isotope amount ratios per unit. The material was produced following ISO Guide 34:2009. The certified reference materials uranium metal EC NRM 101, enriched uranium metal NBL CRM-116 and plutonium metal CETAMA MP2 were used as starting materials to prepare the mother solution. This solution was dispensed by means of an automated robot system into individual units and dried down. A solution of an organic substance, cellulose acetate butyrate (CAB), was dried on the spike material as a stabiliser to retain the dried material at the bottom of the vial. Between unit-homogeneity was quantified and stability during dispatch and storage were assessed in accordance with ISO Guide 35:2006. The certified values were obtained from the gravimetric preparation of the mother solution, taking into account the mass, purity and isotopic abundances of the starting materials, the mass of the mother solution, and the mass of an aliquot in each individual unit. The certified values were confirmed by isotope dilution thermal ionisation mass spectrometry (ID-TIMS) and thermal ionisation mass spectrometry (TIMS) as independent confirmation methods. Uncertainties of the certified values were estimated in compliance with the Guide to the Expression of Uncertainty in Measurement (GUM) and include uncertainties related to possible inhomogeneity and to characterisation. This spike CRM is applied as a calibrant to measure the uranium and plutonium amount content of dissolved spent nuclear fuel solutions using isotope dilution mass spectrometry (IDMS). Each unit contains about 50 mg of uranium with a relative mass fraction m(235U)/m(U) of 17.4 % and 1.8 mg of plutonium with a relative mass fraction m(239Pu)/m(Pu) of 97.8 % as dried nitrates in CAB. The whole amount of sample per unit has to be used for analysis.