Title: Preparation and certification of Large-Sized Dried (LSD) spike - IRMM-1027o
Publisher: Publications Office of the European Union
Publication Year: 2013
JRC N°: JRC80163
ISBN: 978-92-79-28942-2
ISSN: 1831-9424
Other Identifiers: EUR 25857
URI: http://publications.jrc.ec.europa.eu/repository/handle/JRC80163
DOI: 10.2787/7785
Type: EUR - Scientific and Technical Research Reports
Abstract: IRMM Large-Sized Dried (LSD) Spikes are a fundamental part of the fissile material control of irradiated nuclear fuel, 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-1027o 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 a synthetic nitrate solution. This solution was dispensed by means of an automated robot system into individual units (penicillin vials) and dried down. An organic material, cellulose acetate butyrate (CAB), was dried on the spike material as a stabilizer to retain the dried material at the bottom of the penicillin 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 nitrate solution, taking into account the mass, purity and isotopic abundances of the starting materials, the mass of the nitrate solution, and the mass of an aliquot of a nitrate solution in individual unit. The certified values were confirmed by isotope dilution thermal ionisation mass spectrometry (ID-TIMS) as independent confirmation method (measurements within the scope of accreditation to ISO/IEC 17025:2005). Uncertainties of the certified values were calculated in compliance with the Guide to the Expression of Uncertainty in Measurement (GUM)and include uncertainties related to possible in homogeneity, and to characterisation. These spikes are applied to measure the uranium and plutonium amount content of dissolved fuel solutions using isotope dilution mass spectrometry (IDMS). The CRM is available in penicillin vials, each containing about 50 mg of uranium with a 235U relative mass fraction of 19.3% and 1.9 mg of plutonium with a 239Pu relative mass fraction of 97.8% as dried nitrate in CAB. The whole amount of sample per unit has to be used for analysis.
JRC Directorate:Health, Consumers and Reference Materials

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