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A sample of from the Defense Waste Processing Facility (DWPF) Precipitate Reactor Feed Tank (PRFT) was pulled and sent to the Savannah River National Laboratory (SRNL) in June of 2013. The PRFT in DWPF receives Actinide Removal Process (ARP)/ Monosodium Titanate (MST) material from the 512-S Facility via the 511-S Facility. This 2.2 L sample was to be used in small-scale DWPF chemical process cell testing in the Shielded Cells Facility of SRNL. A 1L sub-sample portion was characterized to determine the physical properties such as weight percent solids, density, particle size distribution and crystalline phase identification. Further chemical analysis of the PRFT filtrate and dissolved slurry included metals and anions as well as carbon and base analysis. This technical report describes the characterization and analysis of the PRFT sample from DWPF. At SRNL, the 2.2 L PRFT sample was composited from eleven separate samples received from DWPF. The visible solids were observed to be relatively quick settling which allowed for the rinsing of the original shipping vials with PRFT supernate on the same day as compositing. Most analyses were performed in triplicate except for particle size distribution (PSD), X-ray diffraction (XRD), Scanning Electron Microscopy (SEM) and thermogravimetric analysis (TGA).more » PRFT slurry samples were dissolved using a mixed HNO3/HF acid for subsequent Inductively Coupled Plasma Atomic Emission Spectroscopy (ICPAES) and Inductively Coupled Plasma Mass Spectroscopy (ICP-MS) analyses performed by SRNL Analytical Development (AD). Per the task request for this work, analysis of the PRFT slurry and filtrate for metals, anions, carbon and base were primarily performed to support the planned chemical process cell testing and to provide additional component concentrations in addition to the limited data available from DWPF. Analysis of the insoluble solids portion of the PRFT slurry was aimed at detailed characterization of these solids (TGA, PSD, XRD and SEM) in support of the Salt IPT chemistry team. The overall conclusions from analyses performed in this study are that the PRFT slurry consists of 0.61 Wt.% insoluble MST solids suspended in a 0.77 M [Na+] caustic solution containing various anions such as nitrate, nitrite, sulfate, carbonate and oxalate. The corresponding measured sulfur level in the PRFT slurry, a critical element for determining how much of the PRFT slurry gets blended into the SRAT, is 0.437 Wt.% TS. The PRFT slurry does not contain insoluble oxalates nor significant quantities of high activity sludge solids. The lack of sludge solids has been alluded to by the Salt IPT chemistry team in citing that the mixing pump has been removed from Tank 49H, the feed tank to ARP-MCU, thus allowing the sludge solids to settle out. The PRFT aqueous slurry from DWPF was found to contain 5.96 Wt.% total dried solids. Of these total dried solids, relatively low levels of insoluble solids (0.61 Wt.%) were measured. The densities of both the filtrate and slurry were 1.05 g/mL. Particle size distribution of the PRFT solids in filtered caustic simulant and XRD analysis of washed/dried PRFT solids indicate that the PRFT slurry contains a bimodal distribution of particles in the range of 1 and 6 μm and that the particles contain sodium titanium oxide hydroxide Na2Ti2O4(OH)2 crystalline material as determined by XRD. These data are in excellent agreement with similar data obtained from laboratory sampling of vendor supplied MST. Scanning Electron Microscopy (SEM) combined with Energy Dispersive X-ray Spectroscopy (EDS) analysis of washed/dried PRFT solids shows the particles to be like previous MST analyses consisting of irregular shaped micron-sized solids consisting primarily of Na and Ti. Thermogravimetric analysis of the washed and unwashed PRFT solids shows that the washed solids are very similar to MST solids. The TGA mass loss signal for the unwashed solids shows similar features to TGA performed on cellulose nitrate filter paper indicating significant presence of the deteriorated filter in this unwashed sample. Neither the washed nor unwashed PRFT solids TGA traces showed any features that would indicate presence of sodium oxalate solids. The PRFT Filtrate elemental analysis shows that Na, S and Al are major soluble species with trace levels of B, Cr, Cu, K, Li, Si, Tc, Th and U present. Nitrate, nitrite, sulfate, oxalate, carbonate and hydroxide are major soluble anion species. There is good agreement between the analyzed TOC and the total carbon calculated from the sum of oxalate and minor species formate. Comparison of the amount and speciation of the carbon species between filtrate and slurry indicates no significant carbon-containing species, e.g., sodium oxalate, are present in the slurry solids. Dissolution of the PRFT slurry and subsequent analysis shows that Na, Ti, Si and U are the major elements present on a Wt.% total dried solids basis with 30, 5.8 and 0.47 and 0.11 Wt.% total dried solids, respectively. The amount of Al in the dissolved PRFT slurry is less than that calculated from the PRFT filtrate alone which suggests that the mixed acid digestion used in this work is not optimized for Al recovery. The concentrations of Ca, Fe, Hg and U are all low (at or below 0.11 wt%) and there is no detectable Mn or Ni present which indicates no significant HLW sludge solids are present in the PRFT slurry sample.« less
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Savannah River Site (SRS), Aiken, SC (United States)
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United States