Optimization of Davies and Gray/NBL method used for determination of total uranium concentration in the safeguards destructive analysis

One important activity conducted by the Brazilian State System of Accounting for and Control of Nuclear Materials - SSAC is to verify inventories of the nuclear facilities by nondestructive analysis and destructive analysis. For destructive analysis, the Safeguards Laboratory of Brazilian Nuclear Energy Commission - LASAL/CNEN has been applying the 'Davies and Gray/NBL' method in samples taken during inspections at nuclear facilities since 1984 in Brazil and Argentina. This method consists of the determination of total uranium concentration by potentiometric titration of uranium (IV) with a standard solution of potassium dichromate as oxidizing agent. This solution is prepared using a K2Cr2O7 SRM 136e standard reference material (99.984 ±0.010) wt% certified by National Institute of Standard and Technology - NIST. The procedure also includes the calibration with primary uranium standards reference material (NBL CRM 112A). In order to reduce the consumption of K2Cr2O7 and the other reagent involved in the procedure, without any loss in the performance of the method, a K2Cr2O7 solution with half the regular concentration was prepared and used to test the uranium concentration in several aliquots with a content between 30 mg to 40 mg of uranium per gram of solution. After optimizing the parameters and procedure, it was possible to get the same performance as well. As a consequence, decreasing of the cost, the amount of waste and also a reduction in the titration time of each aliquot was achieved. Thus, this work describes all details in this research as well as the results and its evaluation. (author)