Standard methods for chemical, mass spectrometric, spectrochemical, nuclear, and radiochemical analysis of nuclear-grade uranyl nitrate solutions

Procedures are given in detail for the analysis of solutions of uranyl nitrate for U content, specific gravity, free acid, isotopic content, and impurities. Uranium may be determined by titration with K2Cr2O7 after reduction with Fe2+ or gravimetrically by ignition to U3O8. In solutions containing a molar ratio of free acid to U of up to 5:1, the free acid can be determined by oxalate complexation. Soluble C in the uranyl nitrate solution is determined by persulfate oxidation to CO2. After steam distillation to separate the halogens, F- is measured using a specific-ion electrode, and Cl-, Br-, and I- are determined by amperometric microtitrimetry. A mass spectrophotometric method is used to determine the isotopic composition. The total α activity of the solution and the 232U content are determined by α spectroscopy, while fission products are determined by γ or β spectroscopy. Emission spectrographic methods and mass spectroscopic methods are described for the determination of some trace elements in the solutions. Th, Cr, Mo, Br2, S, P, and Si are determined spectrophotometrically