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SANTANA, Luciana V. Preparation and characterization of a candidate for uranium silicide reference material U3Si2. 2019. 137 p. Thesis (Doctorate in Nuclear Technology) Institute of Energy and Nuclear Research IPEN-CNEN / SP. Sao Paulo. According to CNEN-NN-2.02.1999, Brazilian nuclear facilities must use measurement systems that allow the determination of their nuclear material inventories and also evaluate and verify the quality of their measurement systems through the participation of laboratories. Involved in intercomparison programs, in addition to the use of reference materials and certified reference materials. In this context, this study reports the efforts to ensure the preparation and characterization of the first reference material for uranium silicate matrix that aims to guarantee the quality of nuclear fuel produced in Brazil. Uranium, silicon and impurities contents were investigated in 8 samples analyzed in triplicate for the homogeneity study and 12 samples for the stability study. Variance analysis was used to provide information on mass variability and degree of inhomogeneity. The characterization of the material was made through a comparative study between 3 independent laboratories. The characterization of nuclear material was performed by applying potentiometric titration by "Davies & Gray / NBL" for determination of uranium concentrations and gravimetric determination for silicon concentrations, methods recommended by the International Atomic Energy Agency. The impurity content was determined by induced plasma source emission spectrometry (ICPOES) after prior matrix separation. By comparison, the energy dispersive X-ray fluorescence (WDXRF) technique was applied. Certified values were those whose concentration results were obtained with relative expanded uncertainties of less than 20%. This limit was chosen as appropriate for the intended use of the reference material and for the determination of elements in the matrix under the conditions of this study.

Preparo e caracterização de um candidato a material de referência de siliceto de urânio - U>sub<3>/subsub<2>/sub<