TANK 40 FINAL SB5 CHEMICAL CHARACTERIZATION RESULTS PRIOR TO NP ADDITION

A sample of Sludge Batch 5 (SB5) was pulled from Tank 40 in order to obtain radionuclide inventory analyses necessary for compliance with the Waste Acceptance Product Specifications (WAPS). This sample was also analyzed for chemical composition including noble metals. Prior to radionuclide inventory analyses, a final sample of the H-canyon Np stream will be added to bound the Np addition anticipated for Tank 40. These analyses along with the WAPS radionuclide analyses will help define the composition of the sludge in Tank 40 that is currently being fed to DWPF as SB5. At the Savannah River National Laboratory (SRNL) the 3-L Tank 40 SB5 sample was transferred from the shipping container into a 4-L high density polyethylene vessel and solids allowed to settle overnight. Supernate was then siphoned off and circulated through the shipping container to complete the transfer of the sample. Following thorough mixing of the 3-L sample, a 239 g sub-sample was removed. This sub-sample was then utilized for all subsequent analytical samples. Eight separate aliquots of the slurry were digested, four with HNO{sub 3}/HCl (aqua regia) in sealed Teflon{reg_sign} vessels and four in Na{sub 2}O{sub 2} (alkali or peroxide fusion) using Zr crucibles. Due to the use of Zr crucibles and Na in the peroxide fusions, Na and Zr cannot be determined from this preparation. Additionally, other alkali metals, such as Li and K that may be contaminants in the Na{sub 2}O{sub 2} are not determined from this preparation. Three Analytical Reference Glass - 14 (ARG-1) standards were digested along with a blank for each preparation. The ARG-1 glass allows for an assessment of the completeness of each digestion. Each aqua regia digestion and blank was diluted to 1:100 mL with deionized water and submitted to Analytical Development (AD) for inductively coupled plasma - atomic emission spectroscopy (ICPAES) analysis, inductively coupled plasma - mass spectrometry (ICP-MS) analysis of masses 81-209 and 230-252, and cold vapor atomic absorption (CV-AA) analysis for Hg. Equivalent dilutions of the peroxide fusion digestions and blank were submitted to AD for ICP-AES analysis. Tank 40 SB5 supernate was collected from a mixed slurry sample in the SRNL Shielded Cells and submitted to AD for ICP-AES. Weighted dilutions of slurry were submitted for ion chromatography (IC), total inorganic carbon/total organic carbon (TIC/TOC), and total base analyses. The following conclusions were drawn from the analytical results reported here: (1) The elemental ratios of the major elements for the SB5 WAPS sample, whose major Tank 51 Qualification sample component underwent Al dissolution, are similar to those measured for the SB4 WAPS sample. (2) The elemental composition of this sample and the analyses conducted here are reasonable and consistent with DWPF batch data measurements in light of DWPF pre-sample concentration and SRAT product heel contributions to the DWPF SRAT receipt analyses. (3) Fifty percent of the sulfur in the SB5 WAPS sample is insoluble, and this represents a significantly larger fraction than that observed in previous sludge batches. (4) The noble metal and Ag concentrations predicted from the measured values for the Tank 51 Confirmation sample and Tank 40 SB4 WAPS sample using a two-thirds Tank 51, one-third Tank 40 heel blend ratio used to arrive at the final SB5 composition, agree with the values for the Tank 40 SB5 WAPS sample measured for this report