Dissolution experiments were performed on actual samples of NWCF Run H-4 radioactive calcine in fiscal years 1998 and 1999. Run H-4 is an aluminum/sodium blend calcine. Typical dissolution data indicates that between 90-95 wt% of H-4 calcine can be dissolved using 1gram of calcine per 10 mLs of 5-8M nitric acid at boiling temperature. Two liquid raffinate solutions composed of a WM-188/aluminum nitrate blend and a WM-185/aluminum nitrate blend were converted into calcine at the NWCF. Calcine made from each blend was collected and transferred to RAL for dissolution studies. The WM-188/aluminum nitrate blend calcine was dissolved with resultant solutions used as feed material for separation treatment experimentation. The WM-185/aluminum nitrate blend calcine dissolution testing was performed to determine compositional analyses of the dissolved solution and generate UDS for solid/liquid separation experiments. Analytical fusion techniques were then used to determine compositions of the solid calcine and UDS from dissolution. The results from each of these analyses were used to calculate elemental material balances around the dissolution process, validating the experimental data. This report contains all experimental data from dissolution experiments performed using both calcine blends.

Palladium used at Savannah River (SR) for process tritium storage is currently obtained from a commercial source. In order to understand the processes involved in preparing this material, SR is supporting investigations into the chemical reactions used to synthesize this material. The material specifications are shown in Table 1. An improved understanding of the chemical processes should help to guarantee a continued reliable source of Pd in the future. As part of this evaluation, a work-for-others contract between Westinghouse Savannah River Company and Ames Laboratory (AL) was initiated. During FY98, the process for producing Pd powder developed in 1986 by Dan Grove of Mound Applied Technologies, USDOE (the Mound muddy water process) was studied to understand the processing conditions that lead to changes in morphology in the final product. During FY99 and FY00, the process for producing Pd powder that has been used previously at Sandia and Los Alamos National Laboratories (the Sandia/LANL process) was studied to understand the processing conditions that lead to changes in the morphology of the final Pd product. During FY01, scale-up of the process to batch sizes greater than 600 grams of Pd using a 20-gallon Pfaudler reactor was conducted by the Iowa State University …