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LAB-SCALE DEMONSTRATION OF PLUTONIUM PURIFICATION BY ANION EXCHANGE, PLUTONIUM (IV) OXALATE PRECIPITATION, AND CALCINATION TO PLUTONIUM OXIDE TO SUPPORT THE MOX FEED MISSION

Description: H-Canyon and HB-Line are tasked with the production of PuO{sub 2} from a feed of plutonium metal. The PuO{sub 2} will provide feed material for the MOX Fuel Fabrication Facility. After dissolution of the Pu metal in H-Canyon, the solution will be transferred to HB-Line for purification by anion exchange. Subsequent unit operations include Pu(IV) oxalate precipitation, filtration and calcination to form PuO{sub 2}. This report details the results from SRNL anion exchange, precipitation, filtration, calcination, and characterization tests, as requested by HB-Line1 and described in the task plan. This study involved an 80-g batch of Pu and employed test conditions prototypical of HB-Line conditions, wherever feasible. In addition, this study integrated lessons learned from earlier anion exchange and precipitation and calcination studies. H-Area Engineering selected direct strike Pu(IV) oxalate precipitation to produce a more dense PuO{sub 2} product than expected from Pu(III) oxalate precipitation. One benefit of the Pu(IV) approach is that it eliminates the need for reduction by ascorbic acid. The proposed HB-Line precipitation process involves a digestion time of 5 minutes after the time (44 min) required for oxalic acid addition. These were the conditions during HB-line production of neptunium oxide (NpO{sub 2}). In addition, a series of small Pu(IV) oxalate precipitation tests with different digestion times were conducted to better understand the effect of digestion time on particle size, filtration efficiency and other factors. To test the recommended process conditions, researchers performed two nearly-identical larger-scale precipitation and calcination tests. The calcined batches of PuO{sub 2} were characterized for density, specific surface area (SSA), particle size, moisture content, and impurities. Because the 3013 Standard requires that the calcination (or stabilization) process eliminate organics, characterization of PuO{sub 2} batches monitored the presence of oxalate by thermogravimetric analysis-mass spectrometry (TGA-MS). To use the TGA-MS for carbon or oxalate content, ...
Date: August 22, 2012
Creator: Crowder, M. & Pierce, R.
Partner: UNT Libraries Government Documents Department

PLUTONIUM LOADING CAPACITY OF REILLEX HPQ ANION EXCHANGE COLUMN - AFS-2 PLUTONIUM FLOWSHEET FOR MOX

Description: Radioactive plutonium (Pu) anion exchange column experiments using scaled HB-Line designs were performed to investigate the dependence of column loading performance on the feed composition in the H-Canyon dissolution process for plutonium oxide (PuO{sub 2}) product shipped to the Mixed Oxide (MOX) Fuel Fabrication Facility (MFFF). These loading experiments show that a representative feed solution containing {approx}5 g Pu/L can be loaded onto Reillex{trademark} HPQ resin from solutions containing 8 M total nitrate and 0.1 M KF provided that the F is complexed with Al to an [Al]/[F] molar ratio range of 1.5-2.0. Lower concentrations of total nitrate and [Al]/[F] molar ratios may still have acceptable performance but were not tested in this study. Loading and washing Pu losses should be relatively low (<1%) for resin loading of up to 60 g Pu/L. Loading above 60 g Pu/L resin is possible, but Pu wash losses will increase such that 10-20% of the additional Pu fed may not be retained by the resin as the resin loading approaches 80 g Pu/L resin.
Date: July 26, 2012
Creator: Kyser, E.; King, W. & O'Rourke, P.
Partner: UNT Libraries Government Documents Department

DECONTAMINATION OF PLUTONIUM FOR FLUORIDE AND CHLORIDE DURING OXALATE PRECIPITATION, FILTRATION AND CALCINATION PROCESSES

Description: Due to analytical limitations for the determination of fluoride (F) and chloride (Cl) in a previous anion exchange study, an additional study of the decontamination of Pu from F and Cl by oxalate precipitation, filtration and calcination was performed. Anion product solution from the previous impurity study was precipitated as an oxalate, filtered, and calcined to produce an oxide for analysis by pyrohydrolysis for total Cl and F. Analysis of samples from this experiment achieved the purity specification for Cl and F for the proposed AFS-2 process. Decontamination factors (DF's) for the overall process (including anion exchange) achieved a DF of {approx}5000 for F and a DF of {approx}100 for Cl. Similar experiments where both HF and HCl were spiked into the anion product solution to a {approx}5000 {micro}g /g Pu concentration showed a DF of 5 for F and a DF of 35 for Cl across the combined precipitation-filtration-calcination process steps.
Date: July 25, 2012
Creator: Kyser, E.
Partner: UNT Libraries Government Documents Department

TECHNICAL BASIS FOR DOE STANDARD 3013 EQUIVALENCY SUPPORTING REDUCED TEMPERATURE STABILIZATION OF OXALATE-DERIVED PLUTONIUM OXIDE PRODUCED BY THE HB-LINE FACILITY AT SAVANNAH RIVER SITE

Description: The HB-Line (HBL) facility at the Savannah River Site (SRS) is designed to produce high-purity plutonium dioxide (PuO{sub 2}) which is suitable for future use in production of Mixed Oxide (MOX) fuel. The MOX Fuel Fabrication Facility (MFFF) requires PuO{sub 2} feed to be packaged per the U.S. Department of Energy (DOE) Standard 3013 (DOE-STD-3013) to comply with the facility's safety basis. The stabilization conditions imposed by DOE-STD-3013 for PuO{sub 2} (i.e., 950 C for 2 hours) preclude use of the HBL PuO{sub 2} in direct fuel fabrication and reduce the value of the HBL product as MFFF feedstock. Consequently, HBL initiated a technical evaluation to define acceptable operating conditions for production of high-purity PuO{sub 2} that fulfills the DOE-STD-3013 criteria for safe storage. The purpose of this document is to demonstrate that within the defined operating conditions, the HBL process will be equivalent for meeting the requirements of the DOE-STD-3013 stabilization process for plutonium-bearing materials from the DOE complex. The proposed 3013 equivalency reduces the prescribed stabilization temperature for high-purity PuO{sub 2} from oxalate precipitation processes from 950 C to 640 C and places a limit of 60% on the relative humidity (RH) at the lowest material temperature. The equivalency is limited to material produced using the HBL established flow sheet, for example, nitric acid anion exchange and Pu(IV) direct strike oxalate precipitation with stabilization at a minimum temperature of 640 C for four hours (h). The product purity must meet the MFFF acceptance criteria of 23,600 {micro}g/g Pu (i.e., 2.1 wt %) total impurities and chloride content less than 250 {micro}g/g of Pu. All other stabilization and packaging criteria identified by DOE-STD-3013-2012 or earlier revisions of the standard apply. Based on the evaluation of test data discussed in this document, the expert judgment of the authors supports packaging ...
Date: July 2, 2012
Creator: Duffey, J.; Livingston, R.; Berg, J. & Veirs, D.
Partner: UNT Libraries Government Documents Department

SMALL-SCALE TESTING OF PLUTONIUM (IV) OXALATE PRECIPITATION AND CALCINATION TO PLUTONIUM OXIDE TO SUPPORT THE MOX FEED MISSION

Description: The H-Canyon facility will be used to dissolve Pu metal for subsequent purification and conversion to plutonium dioxide (PuO{sub 2}) using Phase II of HB-Line. To support the new mission, SRNL conducted a series of experiments to produce calcined plutonium (Pu) oxide and measure the physical properties and water adsorption of that material. This data will help define the process operating conditions and material handling steps for HB-Line. An anion exchange column experiment produced 1.4 L of a purified 52.6 g/L Pu solution. Over the next nine weeks, seven Pu(IV) oxalate precipitations were performed using the same stock Pu solution, with precipitator feed acidities ranging from 0.77 M to 3.0 M nitric acid and digestion times ranging from 5 to 30 minutes. Analysis of precipitator filtrate solutions showed Pu losses below 1% for all precipitations. The four larger precipitation batches matched the target oxalic acid addition time of 44 minutes within 4 minutes. The three smaller precipitation batches focused on evaluation of digestion time and the oxalic acid addition step ranged from 25-34 minutes because of pump limitations in the low flow range. Following the precipitations, 22 calcinations were performed in the range of 610-690 C, with the largest number of samples calcined at either 650 or 635 C. Characterization of the resulting PuO{sub 2} batches showed specific surface areas in the range of 5-14 m{sup 2}/g, with 16 of the 22 samples in the range of 5-10 m2/g. For samples analyzed with typical handling (exposed to ambient air for 15-45 minutes with relative humidities of 20-55%), the moisture content as measured by Mass Spectrometry ranged from 0.15 to 0.45 wt % and the total mass loss at 1000 C, as measured by TGA, ranged from 0.21 to 0.58 wt %. For the samples calcined between 635 and 650 C, ...
Date: June 25, 2012
Creator: Crowder, M.; Pierce, R.; Scogin, J.; Daniel, G. & King, W.
Partner: UNT Libraries Government Documents Department

THE APPARENT SOLUBILITY OF ALUMINUM(III) IN HANFORD HIGH-LEVEL WASTE TANKS

Description: The solubility of aluminum in Hanford nuclear waste impacts on the process ability of the waste by a number of proposed treatment options. For many years, Hanford staff has anecdotally noted that aluminum appears to be considerably more soluble in Hanford waste than the simpler electrolyte solutions used as analogues. There has been minimal scientific study to confirm these anecdotal observations, however. The present study determines the apparent solubility product for gibbsite in 50 tank samples. The ratio of hydroxide to aluminum in the liquid phase for the samples is calculated and plotted as a function of total sodium molarity. Total sodium molarity is used as a surrogate for ionic strength, because the relative ratios of mono, di and trivalent anions are not available for all of the samples. These results were compared to the simple NaOH-NaAl(OH{sub 4})H{sub 2}O system, and the NaOH-NaAl(OH{sub 4})NaCl-H{sub 2}O system data retrieved from the literature. The results show that gibbsite is apparently more soluble in the samples than in the simple systems whenever the sodium molarity is greater than two. This apparent enhanced solubility cannot be explained solely by differences in ionic strength. The change in solubility with ionic strength in simple systems is small compared to the difference between aluminum solubility in Hanford waste and the simple systems. The reason for the apparent enhanced solubility is unknown, but could include. kinetic or thermodynamic factors that are not present in the simple electrolyte systems. Any kinetic explanation would have to explain why the samples are always supersaturated whenever the sodium molarity is above two. Real waste characterization data should not be used to validate thermodynamic solubility models until it can be confirmed that the apparent enhanced gibbsite solubility is a thermodynamic effect and not a kinetic effect.
Date: June 20, 2012
Creator: JG, REYNOLDS
Partner: UNT Libraries Government Documents Department

REVISED GUIDELINES FOR USING CELLULOSE DEGRADATION PRODUCT-IMPACTED KD VALUES FOR PERFORMANCE ASSESSMENTS AND COMPOSITE ANALYSES

Description: Cellulosic materials include wood, paper, rags, and cardboard products. These materials are co-disposed with radiological waste at the Savannah River Site's (SRS) E-Area Low-Level Waste Facility (ELLWF). Cellulosic materials readily degrade in the environment to form cellulose degradation products (CDP) that will partition to the sediment or remain mobile in the groundwater. Savannah River National Lab (SRNL) has conducted studies to estimate the impact of CDP on radionuclide sorption to SRS sediments (Kd values). It was found that CDP impact on radionuclide sorption varies with radionuclide and CDP concentration. Furthermore, it was found that the amount of carbon (C) in the system could increase or decrease Kd values with respect to the base case of when no CDP was added. Throughout the expected pH range of the ELLWF, a low concentration of CDP in the system would increase Kd values (because C would sorb to the sediment and provide more exchange sites for radionuclides to sorb), whereas greater concentrations of CDP ({ge}20 mg/L C) would decrease Kd values (because C would remain in solution and complex the radionuclide and not permit the radionuclide to sorb to the sediment). A review of >230 dissolved organic carbon (DOC) groundwater concentrations in the Old Radioactive Waste Burial Ground (ORWBG) at the SRS indicated that the average DOC concentration, a gross measure of CDP, was 5 mg/L C. At approximately this DOC concentration, the laboratory studies demonstrated that no anions (Tc, I, or Se) or cations (Ni, Sr, Ce, Eu, Zr, or Th) have decreased sorption in the presence of carbon (an analogue for CDP).
Date: May 14, 2012
Creator: Kaplan, D.
Partner: UNT Libraries Government Documents Department

HB-LINE ANION EXCHANGE PURIFICATION OF AFS-2 PLUTONIUM FOR MOX

Description: Non-radioactive cerium (Ce) and radioactive plutonium (Pu) anion exchange column experiments using scaled HB-Line designs were performed to investigate the feasibility of using either gadolinium nitrate (Gd) or boric acid (B as H{sub 3}BO{sub 3}) as a neutron poison in the H-Canyon dissolution process. Expected typical concentrations of probable impurities were tested and the removal of these impurities by a decontamination wash was measured. Impurity concentrations are compared to two specifications - designated as Column A or Column B (most restrictive) - proposed for plutonium oxide (PuO{sub 2}) product shipped to the Mixed Oxide (MOX) Fuel Fabrication Facility (MFFF). Use of Gd as a neutron poison requires a larger volume of wash for the proposed Column A specification. Since boron (B) has a higher proposed specification and is more easily removed by washing, it appears to be the better candidate for use in the H-Canyon dissolution process. Some difficulty was observed in achieving the Column A specification due to the limited effectiveness that the wash step has in removing the residual B after {approx}4 BV's wash. However a combination of the experimental 10 BV's wash results and a calculated DF from the oxalate precipitation process yields an overall DF sufficient to meet the Column A specification. For those impurities (other than B) not removed by 10 BV's of wash, the impurity is either not expected to be present in the feedstock or process, or recommendations have been provided for improvement in the analytical detection/method or validation of calculated results. In summary, boron is recommended as the appropriate neutron poison for H-Canyon dissolution and impurities are expected to meet the Column A specification limits for oxide production in HB-Line.
Date: April 25, 2012
Creator: Kyser, E. & King, W.
Partner: UNT Libraries Government Documents Department

LABORATORY REPORT ON THE REMOVAL OF PERTECHNETATE FROM TANK 241-AN-105 SIMULANT USING PUROLITE A530E

Description: This report documents the laboratory testing and analyses as directed under the test plan, LAB-PLN-11-00010, Evaluation of Technetium Ion Exchange Material against Hanford Double Shell Tank Supernate Simulate with Pertechnetate. Technetium (Tc-99) is a major fission product from nuclear reactors, and because it has few applications outside of scientific research, most of the technetium will ultimately be disposed of as nuclear waste. The radioactive decay of Tc-99 to ruthenium 99 (Ru-99) produces a low energy {beta}{sup -} particle (0.1 MeV max). However, due to its fairly long half-life (t{sub 1/2} = 2.13E05 years), Tc-99 is a major source of radiation in low-level waste (UCRL-JRNL-212334, Current Status of the Thermodynamic Data for Technetium and its Compounds and Aqueous Species). Technetium forms the soluble oxy anion, TcO{sub 4}{sup -} under aerobic conditions. This anion is very mobile in groundwater and poses a health risk (ANL, Radiological and Chemical Fact Sheets to Support Health Risk Analyses for Contaminated Areas). It has been demonstrated that Purolite{reg_sign} A530E is highly effective in removing TcO{sub 4}{sup -} from a water matrix (RPP-RPT-23199, The Removal of Technetium-99 from the Effluent Treatment Facility Basin 44 Waste Using Purolite A-530E, Reillex HPQ, and Sybron IONAC SR-7 Ion Exchange Resins). Purolite{reg_sign} A530E is the commercial product of the Oak Ridge National Laboratory's Biquat{trademark} resin (Gu, B. et. ai, Development of Novel Bifunctional Anion-Exchange Resins with Improved Selectivity for Pertechnetate Sorption from Contaminated Groundwater). Further work has demonstrated that technetium-loaded A530E achieves a leachability index in Cast Stone of 12.5 (ANSI/ASN-16.1-2003, Measurement of the Leachability of Solidified Low-Level Radioactive Wastes by a Short-term Test Procedure) as reported in RPP-RPT-39195, Assessment of Technetium Leachability in Cement-Stabilized Basin 43 Groundwater Brine. This effort falls under the technetium management initiative and will provide data for those who will make decisions on the handling and ...
Date: April 17, 2012
Creator: JB, DUNCAN; HAGERTY KJ, MOORE WP & JM, JOHNSON
Partner: UNT Libraries Government Documents Department

APPLICATION OF COLUMN EXTRACTION METHOD FOR IMPURITIES ANALYSIS ON HB-LINE PLUTONIUM OXIDE IN SUPPORT OF MOX FEED PRODUCT SPECIFICATIONS

Description: The current mission at H-Canyon involves the dissolution of an Alternate Feedstocks 2 (AFS-2) inventory that contains plutonium metal. Once dissolved, HB-Line is tasked with purifying the plutonium solution via anion exchange, precipitating the Pu as oxalate, and calcining to form plutonium oxide (PuO{sub 2}). The PuO{sub 2} will provide feed product for the Mixed Oxide (MOX) Fuel Fabrication Facility, and the anion exchange raffinate will be transferred to H-Canyon. The results presented in this report document the potential success of the RE resin column extraction application on highly concentrated Pu samples to meet MOX feed product specifications. The original 'Hearts Cut' sample required a 10000x dilution to limit instrument drift on the ICP-MS method. The instrument dilution factors improved to 125x and 250x for the sample raffinate and sample eluent, respectively. As noted in the introduction, the significantly lower dilutions help to drop the total MRL for the analyte. Although the spike recoveries were half of expected in the eluent for several key elements, they were between 94-98% after Nd tracer correction. It is seen that the lower ICD limit requirements for the rare earths are attainable because of less dilution. Especially important is the extremely low Ga limit at 0.12 {mu}g/g Pu; an ICP-MS method is now available to accomplish this task on the sample raffinate. While B and V meet the column A limits, further development is needed to meet the column B limits. Even though V remained on the RE resin column, an analysis method is ready for investigation on the ICP-MS, but it does not mean that V cannot be measured on the ICP-ES at a low dilution to meet the column B limits. Furthermore, this column method can be applicable for ICP-ES as shown in Table 3-2, in that it trims the sample of ...
Date: March 20, 2012
Creator: Jones, M.; Diprete, D. & Wiedenman, B.
Partner: UNT Libraries Government Documents Department

Numerical Modeling of 90Sr and 137Cs Transport from a Spill in the B-Cell of the 324 Building, Hanford Site 300 Area

Description: To characterize the extent of contamination under the 324 Building, a pit was excavated on the north side of the building in 2010 by Washington Closure Hanford LLC (WCH). Horizontal closed-end steel access pipes were installed under the foundation of the building from this pit and were used for measuring temperatures and exposure rates under the B-Cell. The deployed sensors measured elevated temperatures of up to 61 C (142 F) and exposure rates of up to 8,900 R/hr. WCH suspended deactivation of the facility because it recognized that building safety systems and additional characterization data might be needed for remediation of the contaminated material. The characterization work included additional field sampling, laboratory measurements, and numerical flow and transport modeling. Laboratory measurements of sediment physical, hydraulic, and geochemical properties were performed by Pacific Northwest National Laboratory (PNNL) and others. Geochemical modeling and subsurface flow and transport modeling also were performed by PNNL to evaluate the possible extent of contamination in the unsaturated sand and gravel sediments underlying the building. Historical records suggest that the concentrated 137Cs- and 90Sr-bearing liquid wastes that were spilled in B-Cell were likely from a glass-waste repository testing program associated with the Federal Republic of Germany (FRG). Incomplete estimates of the aqueous chemical composition (no anion data provided) of the FRG waste solutions were entered into a geochemical speciation model and were charge balanced with nitrate to estimate waste composition. Additional geochemical modeling was performed to evaluate reactions of the waste stream with the concrete foundation of the building prior to the stream entering the subsurface.
Date: March 19, 2012
Creator: Rockhold, Mark L.; Bacon, Diana H.; Freedman, Vicky L.; Lindberg, Michael J. & Clayton, Ray E.
Partner: UNT Libraries Government Documents Department

STATISTICAL ANALYSIS OF TANK 5 FLOOR SAMPLE RESULTS

Description: Sampling has been completed for the characterization of the residual material on the floor of Tank 5 in the F-Area Tank Farm at the Savannah River Site (SRS), near Aiken, SC. The sampling was performed by Savannah River Remediation (SRR) LLC using a stratified random sampling plan with volume-proportional compositing. The plan consisted of partitioning the residual material on the floor of Tank 5 into three non-overlapping strata: two strata enclosed accumulations, and a third stratum consisted of a thin layer of material outside the regions of the two accumulations. Each of three composite samples was constructed from five primary sample locations of residual material on the floor of Tank 5. Three of the primary samples were obtained from the stratum containing the thin layer of material, and one primary sample was obtained from each of the two strata containing an accumulation. This report documents the statistical analyses of the analytical results for the composite samples. The objective of the analysis is to determine the mean concentrations and upper 95% confidence (UCL95) bounds for the mean concentrations for a set of analytes in the tank residuals. The statistical procedures employed in the analyses were consistent with the Environmental Protection Agency (EPA) technical guidance by Singh and others [2010]. Savannah River National Laboratory (SRNL) measured the sample bulk density, nonvolatile beta, gross alpha, radionuclide, inorganic, and anion concentrations three times for each of the composite samples. The analyte concentration data were partitioned into three separate groups for further analysis: analytes with every measurement above their minimum detectable concentrations (MDCs), analytes with no measurements above their MDCs, and analytes with a mixture of some measurement results above and below their MDCs. The means, standard deviations, and UCL95s were computed for the analytes in the two groups that had at least some measurements ...
Date: March 14, 2012
Creator: Shine, E.
Partner: UNT Libraries Government Documents Department

Nevada National Security Site 2011 Data Report: Groundwater Monitoring Program Area 5 Radioactive Waste Management Site

Description: This report is a compilation of the groundwater sampling results from the Area 5 Radioactive Waste Management Site (RWMS). The data have been collected since 1993 and include calendar year 2011 results. During 2011, groundwater samples were collected and static water levels were measured at the three pilot wells surrounding the Area 5 RWMS. Samples were collected at UE5PW-1 on March 8, August 2, August 24, and October 19, 2011; at UE5PW-2 on March 8, August 2, August 23, and October 19, 2011; and at UE5PW-3 on March 8, August 2, August 23, and October 19, 2011. Static water levels were measured at each of the three pilot wells on March 1, June 7, August 1, and October 17, 2011. Groundwater samples were analyzed for the following indicators of contamination: pH, specific conductance, total organic carbon, total organic halides, and tritium. Indicators of general water chemistry (cations and anions) were also measured. Initial total organic carbon and total organic halides results for samples collected in August 2011 were above previous measurements and, in some cases, above the established investigation limits. However, after field sample pumps and tubing were disinfected with Clorox solution, the results returned to normal levels. Final results from samples collected in 2011 were within the limits established by agreement with the Nevada Division of Environmental Protection for each analyte. These data indicate that there has been no measurable impact to the uppermost aquifer from the Area 5 RWMS. There were no significant changes in measured groundwater parameters compared to previous years. The report contains an updated cumulative chronology for the Area 5 RWMS Groundwater Monitoring Program and a brief description of the site hydrogeology.
Date: February 27, 2012
Creator: National Security Technologies, LLC
Partner: UNT Libraries Government Documents Department

DISSOLUTION OF PLUTONIUM METAL IN 8-10 M NITRIC ACID

Description: The H-Canyon facility will be used to dissolve Pu metal for subsequent purification and conversion to plutonium dioxide (PuO{sub 2}) using Phase II of HB-Line. To support the new mission, the development of a Pu metal dissolution flowsheet which utilizes concentrated (8-10 M) nitric acid (HNO{sub 3}) solutions containing potassium fluoride (KF) is required. Dissolution of Pu metal in concentrated HNO{sub 3} is desired to eliminate the need to adjust the solution acidity prior to purification by anion exchange. The preferred flowsheet would use 8-10 M HNO{sub 3}, 0.015-0.07 M KF, and 0.5-1.0 g/L Gd to dissolve the Pu up to 6.75 g/L. An alternate flowsheet would use 8-10 M HNO{sub 3}, 0.1-0.2 M KF, and 1-2 g/L B to dissolve the Pu. The targeted average Pu metal dissolution rate is 20 mg/min-cm{sup 2}, which is sufficient to dissolve a 'standard' 2250-g Pu metal button in 24 h. Plutonium metal dissolution rate measurements showed that if Gd is used as the nuclear poison, the optimum dissolution conditions occur in 10 M HNO{sub 3}, 0.04-0.05 M KF, and 0.5-1.0 g/L Gd at 112 to 116 C (boiling). These conditions will result in an estimated Pu metal dissolution rate of {approx}11-15 mg/min-cm{sup 2} and will result in dissolution times of 36-48 h for standard buttons. The recommended minimum and maximum KF concentrations are 0.03 M and 0.07 M, respectively. The maximum KF concentration is dictated by a potential room-temperature Pu-Gd-F precipitation issue at low Pu concentrations. The purpose of the experimental work described in this report was two-fold. Initially a series of screening experiments was performed to measure the dissolution rate of Pu metal as functions of the HNO{sub 3}, KF, and Gd or B concentrations. The objective of the screening tests was to propose optimized conditions for subsequent flowsheet demonstration tests. ...
Date: February 21, 2012
Creator: Rudisill, Tracy S. & Pierce, R.
Partner: UNT Libraries Government Documents Department

ADVANCES IN HEXAVALENT CHROMIUM REMOVAL AT HANFORD

Description: At the Hanford Site, chromium was used as a corrosion inhibitor in the reactor cooling water and was introduced into the groundwater as a result of planned and unplanned discharges from reactors during plutonium production since 1944. Beginning in 1995, groundwater treatment methods were evaluated leading to the use of pump and treat facilities with ion exchange using Dowex 21 K, a regenerable strong base anion exchange resin. This required regeneration of the resin, which is currently performed offsite. Resin was installed in a 4 vessel train, with resin removal required from the lead vessel approximately once a month. In 2007, there were 8 trains (32 vessels) in operation. In 2008, DOE recognized that regulatory agreements would require significant expansion in the groundwater chromium treatment capacity. Previous experience from one of the DOE project managers led to identification of a possible alternative resin, and the contractor was requested to evaluate alternative resins for both cost and programmatic risk reductions. Testing was performed onsite in 2009 and 2010, using a variety of potential resins in two separate facilities with groundwater from specific remediation sites to demonstrate resin performance in the specific groundwater chemistry at each site. The testing demonstrated that a weak base anion single-use resin, ResinTech SIR-700, was effective at removing chromium, had a significantly higher capacity, could be disposed of efficiently on site, and would eliminate the complexities and programmatic risks from sampling, packaging, transportation and return of resin for regeneration. This resin was installed in Hanford's newest groundwater treatment facility, called 100-DX, which began operations in November, 2010, and used in a sister facility, 100-HX, which started up in September of 2011. This increased chromium treatment capacity to 25 trains (100 vessels). The resin is also being tested in existing facilities that utilize Dowex 21 K for conversion ...
Date: January 30, 2012
Creator: Neshem, D. O. & Riddelle, J.
Partner: UNT Libraries Government Documents Department

GAMA-LLNL Alpine Basin Special Study: Scope of Work

Description: For this task LLNL will examine the vulnerability of drinking water supplies in foothills and higher elevation areas to climate change impacts on recharge. Recharge locations and vulnerability will be determined through examination of groundwater ages and noble gas recharge temperatures in high elevation basins. LLNL will determine whether short residence times are common in one or more subalpine basin. LLNL will measure groundwater ages, recharge temperatures, hydrogen and oxygen isotopes, major anions and carbon isotope compositions on up to 60 samples from monitoring wells and production wells in these basins. In addition, a small number of carbon isotope analyses will be performed on surface water samples. The deliverable for this task will be a technical report that provides the measured data and an interpretation of the data from one or more subalpine basins. Data interpretation will: (1) Consider climate change impacts to recharge and its impact on water quality; (2) Determine primary recharge locations and their vulnerability to climate change; and (3) Delineate the most vulnerable areas and describe the likely impacts to recharge.
Date: December 12, 2011
Creator: Singleton, M J; Visser, A; Esser, B K & Moran, J E
Partner: UNT Libraries Government Documents Department

Materials Characterization Laboratory (Fact Sheet)

Description: This fact sheet describes the purpose, lab specifications, applications scenarios, and information on how to partner with NREL's Materials Characterization Laboratory at the Energy Systems Integration Facility. The Materials Characterization Laboratory at NREL's Energy Systems Integration Facility (ESIF) research focus is the physical and photoelectrochemical characterization of novel materials. In this laboratory unknown samples are characterized by identifying and quantifying molecular species present through the implementation of a suite of analytical instrumentation and techniques. This leads to the ability to deconvolute decomposition routes and elucidate reaction mechanisms of materials through thermal and evolved gas analysis. This aids in the synthesis of next generation materials that are tailored to optimize stability and performance. These techniques and next generation materials will have many applications. One particular focus is the stable and conductive tetherable cations for use as membrane materials in anion exchange membrane fuel cells. Another is to understand the leachant contaminants derived from balance of plant materials used in proton exchange membrane fuel cell vehicles. Once identified and quantified, these organic and ionic species are dosed as contaminants into ex/in-situ fuel cell tests, to determine the effect on durability and performance. This laboratory also acts in support of fuel cell catalysis, manufacturing, and other related projects. The Materials Characterization Laboratory will cover multiple analytical operations, with the overall goal of troubleshooting synthetic materials or process streams to improve performance. Having novel evolved gas analysis and other analytical capabilities; this laboratory provides a viable location to analyze small batch samples, whereas setting up these types of capabilities and expertise would be cost and time prohibitive for most institutions. Experiments that can be performed include: (1) Evolved gas analysis; (2) Heterogeneous catalysis; (3) Trace level contaminants analysis; (4) Catalyst characterization; (5) Kinetics and stability; (6) Hyphenated techniques; and (7) Isotopic analysis for elucidating ...
Date: October 1, 2011
Partner: UNT Libraries Government Documents Department

Secondary Waste Form Down Selection Data Package – Ceramicrete

Description: As part of high-level waste pretreatment and immobilized low activity waste processing, liquid secondary wastes will be generated that will be transferred to the Effluent Treatment Facility on the Hanford Site for further treatment. These liquid secondary wastes will be converted to stable solid waste forms that will be disposed in the Integrated Disposal Facility. Currently, four waste forms are being considered for stabilization and solidification of the liquid secondary wastes. These waste forms are Cast Stone, Ceramicrete, DuraLith, and Fluidized Bed Steam Reformer. The preferred alternative will be down selected from these four waste forms. Pacific Northwest National Laboratory is developing data packages to support the down selection process. The objective of the data packages is to identify, evaluate, and summarize the existing information on the four waste forms being considered for stabilization and solidification of the liquid secondary wastes. The information included will be based on information available in the open literature and from data obtained from testing currently underway. This data package is for the Ceramicrete waste form. Ceramicrete is a relatively new engineering material developed at Argonne National Laboratory to treat radioactive and hazardous waste streams (e.g., Wagh 2004; Wagh et al. 1999a, 2003; Singh et al. 2000). This cement-like waste form can be used to treat solids, liquids, and sludges by chemical immobilization, microencapsulation, and/or macroencapsulation. The Ceramicrete technology is based on chemical reaction between phosphate anions and metal cations to form a strong, dense, durable, low porosity matrix that immobilizes hazardous and radioactive contaminants as insoluble phosphates and microencapsulates insoluble radioactive components and other constituents that do not form phosphates. Ceramicrete is a type of phosphate-bonded ceramic, which are also known as chemically bonded phosphate ceramics. The Ceramicrete binder is formed through an acid-base reaction between calcined magnesium oxide (MgO; a base) and potassium ...
Date: August 31, 2011
Creator: Cantrell, Kirk J. & Westsik, Joseph H.
Partner: UNT Libraries Government Documents Department

TANK 26F SUPERNATANT AND 2F EVAPORATOR EDUCTOR PUMP SAMPLE CHARACTERIZATION RESULTS

Description: In an effort to understand the reasons for system plugging problems in the SRS 2F evaporator, supernatant samples were retrieved from the evaporator feed tank (Tank 26F) and solids were collected from the evaporator eductor feed pump for characterization. The variable depth supernatant samples were retrieved from Tank 26F in early December of 2010 and samples were provided to SRNL and the F/H Area laboratories for analysis. Inspection and analysis of the samples at SRNL was initiated in early March of 2011. During the interim period, samples were frequently exposed to temperatures as low as 12 C with daily temperature fluctuations as high as 10 C. The temperature at the time of sample collection from the waste tank was 51 C. Upon opening the supernatant bottles at SRNL, many brown solids were observed in both of the Tank 26F supernatant samples. In contrast, no solids were observed in the supernatant samples sent to the F/H Area laboratories, where the analysis was completed within a few days after receipt. Based on these results, it is believed that the original Tank 26F supernatant samples did not contain solids, but solids formed during the interim period while samples were stored at ambient temperature in the SRNL shielded cells without direct climate control. Many insoluble solids (>11 wt. % for one sample) were observed in the Tank 26F supernatant samples after three months of storage at SRNL which would not dissolve in the supernatant solution in two days at 51 C. Characterization of these solids along with the eductor pump solids revealed the presence of sodium oxalate and clarkeite (uranyl oxyhydroxide) as major crystalline phases. Sodium nitrate was the dominant crystalline phase present in the unwashed Eductor Pump solids. Crystalline sodium nitrate may have formed during the drying of the solids after filtration or ...
Date: August 23, 2011
Creator: King, W.; Hay, M. & Coleman, C.
Partner: UNT Libraries Government Documents Department

OXALATE MASS BALANCE DURING CHEMICAL CLEANING IN TANK 6F

Description: The Savannah River Remediation (SRR) is preparing Tank 6F for closure. The first step in preparing the tank for closure is mechanical sludge removal. Following mechanical sludge removal, SRS performed chemical cleaning with oxalic acid to remove the sludge heel. Personnel are currently assessing the effectiveness of the chemical cleaning to determine whether the tank is ready for closure. SRR personnel collected liquid samples during chemical cleaning and submitted them to Savannah River National Laboratory (SRNL) for analysis. Following chemical cleaning, they collected a solid sample (also known as 'process sample') and submitted it to SRNL for analysis. The authors analyzed these samples to assess the effectiveness of the chemical cleaning process. Analysis of the anions showed the measured oxalate removed from Tank 6F to be approximately 50% of the amount added in the oxalic acid. To close the oxalate mass balance, the author collected solid samples, leached them with nitric acid, and measured the concentration of cations and anions in the leachate. Some conclusions from this work are: (1) Approximately 65% of the oxalate added as oxalic acid was removed with the decanted liquid. (2) Approximately 1% of the oxalate (added to the tank as oxalic acid) formed precipitates with compounds such as nickel, manganese, sodium, and iron (II), and was dissolved with nitric acid. (3) As much as 30% of the oxalate may have decomposed forming carbon dioxide. The balance does not fully account for all the oxalate added. The offset represents the combined uncertainty in the analyses and sampling.
Date: July 22, 2011
Creator: Poirier, M. & Fink, S.
Partner: UNT Libraries Government Documents Department

Alpha Heating in ITER L-mode and H-mode Plasma

Description: There are many uses of predictions of ITER plasma performance. One is assessing requirements of different plasma regimes. For instance, what current drive and control are needed for steady state. The heating, current drive, and torque systems planned for initial DT operation are negative ion neutral beam injection (NB), ion cyclotron resonance (IC), and electron cyclotron resonance (EC). Which combinations of heating are optimal. What are benefits of the torques, current drive, and fueling using NB. What are the shine-through power and optimum voltage for the NB? What are optimal locations and aiming of the EC launchers? Another application is nuclear licensing (e.g. System integrity, how many neutrons).
Date: July 18, 2011
Creator: Budny, R.V.
Partner: UNT Libraries Government Documents Department

Oxalate Mass Balance During Chemical Cleaning in Tank 5F

Description: The Savannah River Site (SRS) is preparing Tank 5F for closure. The first step in preparing the tank for closure is mechanical sludge removal. Following mechanical sludge removal, SRS performed chemical cleaning with oxalic acid to remove the sludge heel. Personnel are currently assessing the effectiveness of the chemical cleaning to determine whether the tank is ready for closure. SRS personnel collected liquid samples during chemical cleaning and submitted them to Savannah River National Laboratory (SRNL) for analysis. Following chemical cleaning, they collected a solid sample (also known as 'process sample') and submitted it to SRNL for analysis. The authors analyzed these samples to assess the effectiveness of the chemical cleaning process. Analysis of the anions showed the measured oxalate removed from Tank 5F to be approximately 50% of the amount added in the oxalic acid. To close the oxalate mass balance, the author collected solid samples, leached them with nitric acid, and measured the concentration of cations and anions in the leachate.
Date: July 8, 2011
Creator: Poirier, M. & Fink, S.
Partner: UNT Libraries Government Documents Department

Analysis of the Tank 5F Feed and Bleed Residual Solids

Description: Savannah River Remediation (SRR) is preparing Tank 5F for closure. As part of Tank 5F Closure Mechanical Cleaning, SRR conducted a 'Feed and Bleed' process in Tank 5F. Following this 'Feed and Bleed' Mechanical Cleaning in Tank 5F, SRR collected two tank heel samples (referred to as sample 1 and sample 2) under Riser 5 to determine the composition of the material remaining in the tanks. This document describes sample analysis results. The conclusions from this analysis follow. (1) The anions measured all had a concentration less than 250 mg/kg, except for oxalate, which had a concentration of 2100-2400 mg/kg. (2) The measured cations with the highest concentration were iron (432,000-519,000 mg/kg), nickel (54,600-69,300 mg/kg), and manganese (35,200-42,100 mg/kg). All other cations measured less than 13,000 mg/kg. (3) The radionuclides present in the highest concentration are {sup 90}Sr (3.0 x 10{sup 10} dpm/g), {sup 137}Cs (6.8 x 10{sup 8} dpm/g), and {sup 241}Am (1.4 x 10{sup 8} - 1.8 x 10{sup 8} dpm/g). (4) The particle size analysis shows a large fraction of particles greater than 100 {micro}.
Date: July 7, 2011
Creator: Poirier, M.; Diprete, D.: Coleman, C. & Washington, A.
Partner: UNT Libraries Government Documents Department

Qualification of the First ICS-3000 ION Chromatograph for use at the Defense Waste Processing Facility

Description: The ICS-3000 Ion Chromatography (IC) system installed in 221-S M-13 has been qualified for use. The qualification was a head to head comparison of the ICS-3000 with the currently used DX-500 IC system. The crosscheck work included standards for instrument calibration and calibration verifications and standards for individual anion analysis, where the standards were traceable back to the National Institute of Standards and Technology (NIST). In addition the crosscheck work included the analysis of simulated Sludge Receipt Adjustment Tank (SRAT) Receipt, SRAT Product, and Slurry Mix Evaporator (SME) samples, along with radioactive Sludge Batch 5 material from the SRAT and SME tanks. Based upon the successful qualification of the ICS-3000 in M-13, it is recommended that this task proceed in developing the data to qualify, by a head to head comparison of the two ICS-3000 instruments, a second ICS-3000 to be installed in M-14. The Defense Waste Processing Facility (DWPF) requires the analysis of specific anions at various stages of its processing of high level waste (HLW). The anions of interest to the DWPF are fluoride, formate, chloride, nitrite, nitrate, sulfate, oxalate, and phosphate. The anion analysis is used to evaluate process chemistry including formic acid/nitric acid additions to establish optimum conditions for mercury stripping, reduction-oxidation (REDOX) chemistry for the melter, nitrite destruction, organic acid constituents, etc. The DWPF Laboratory (Lab) has been using Dionex DX-500 ion chromatography (IC) systems since 1998. The vendor informed DWPF in 2006 that the instruments would no longer be supported by service contracts after 2008. DWPF purchased three new ICS-3000 systems in September of 2006. The ICS-3000 instruments are (a) designed to be more stable using an eluent generator to make eluent, (b) require virtually no daily chemical handling by the analysts, (c) require less line breaks in the hood, and (d) generally require ...
Date: July 5, 2011
Creator: Edwards, T & Mahannah, R.
Partner: UNT Libraries Government Documents Department