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DOE OSTI2018

Maximum Potential Hydrogen Gas Retention in the sRF Resin Ion Exchange Column for the LAWPS Process

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DOE OSTI2018

Gas Retention, Gas Release, and Fluidization of Spherical Resorcinol-Formaldehyde (sRF) Ion Exchange Resin

The Low-Activity Waste Pretreatment System (LAWPS) is being developed to provide treated supernatant liquid from the Hanford tank farms directly to the Low-Activity Waste (LAW) Vitrification Facility at the Hanford Tank Waste Treatment and Immobilization Plant. The design and development of the LAWPS is being conducted by Washington River Protection Solutions, LLC. A key process in LAWPS is the removal of radioactive Cs from LAW liquids using ion exchange (IX) columns filled with spherical resorcinol-formaldehyde (sRF) resin. When loaded with radioactive Cs, radiolysis of water in the LAW liquid will generate hydrogen gas. In normal operations, the generated hydrogen is expected to remain dissolved in the liquid and be continuously removed by liquid flow. One accident scenario being evaluated is the loss of liquid flow through the sRF resin bed after it has been loaded with radioactive Cs and hydrogen gas is being generated by radiolysis. For an accident scenario with a loss of flow, hydrogen gas can be retained within the IX column both in the sRF resin bed and below the bottom screen that supports the resin within the column, which creates a hydrogen flammability hazard. Because there is a potential for a large fraction of the retained hydrogen to be released over a short duration as a gas release event, there is a need to quantify the size and rate of potential gas release events. Due to the potential for a large, rapid gas release event, an evaluation of mitigation methods to eliminate the hydrogen hazard is also needed. One method being considered for mitigating the hydrogen hazard during a loss of flow accident is to have a secondary flow system, with two redundant pumps operating in series, that re-circulates liquid upwards through the bed and into a vented break tank where hydrogen gas is released from the liquid and removed by venting the headspace of the break tank. The mechanism for inducing release of gas from the sRF bed is to fluidize the bed, which should allow retained bubbles to rise and be carried to the break tank. Currently, neither the ability of fluidizing a settled sRF bed to release gas nor the quantity of hydrogen gas that can be retained and the corresponding potential for large, rapid gas release events has been tested and evaluated. Accordingly, the purpose of this study was to conduct experiments and develop models that evaluate the ability of a re-circulating flow system to fluidize an sRF resin bed as a method to release retained hydrogen gas and maintain hydrogen gas retention at low levels, thereby avoiding conditions where hydrogen gas poses a flammability hazard. The purpose of the study was also to determine if effective hydrogen gas release would occur using a single constant fluidization velocity, because this is the most simple safety system to implement, for the range of fluid and sRF resin conditions anticipated in the column (because a velocity that is effective for one fluid/resin pair can be ineffective for different resin/fluid pairs). Finally, the study also included quantifying the volume of gas that can be retained in an sRF bed and the behavior of spontaneous, rather than fluidization-induced, gas release events.

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DOE OSTI2024

Evaluation of the Potential for Precipitation of Solids during Storage of Non-Aluminum SNF Solutions

Non-aluminum clad spent nuclear fuels (NASNF) stored in the L-Area basin will be dissolved in H-Canyon using the 6.3D electrolytic dissolver. The solutions will be stored in either the hot or warm canyon until the preparation of a sludge batch for the Defense Waste Processing Facility. Spent nuclear fuel solutions could be stored for 1-2 years before transfer to the H-Area Tank Farm depending on the interval between sludge batches. The solution level in the storage tanks will be maintained; therefore, precipitation of solids due to evaporation is not an issue. However, the precipitation of solids from completely dissolved SNF due to solution instabilities has been observed during intermediate storage of solutions generating hydrated oxides.The presence of fissile material in these solids is generally associated with zirconium molybdate, which is known to act as a host lattice for Pu and can carry the actinides upon precipitation. The formation of zirconium molybdate solids which carry fissile material is a potential concern for the storage of NASNF solutions. To address this concern, the Savannah River National Laboratory performed a literature review to identify knowledge gaps which may require experimental work to determine if the formation of solids is a concern during storage of these solutions. Based on the literature review, the precipitation of zirconium molybdate solids from the Campaign 1 NASNF solutions during intermediatestorage is expected. This conclusion is supported by the identification of zirconium molybdate solids found on the H-Canyon 6.1D Dissolver MK-12 insert spacer. The formation of the zirconium molybdate solids is attributed to hydrolysis and radiolytic processes in the nitric acid solution. As the molybdate solids form, U and Pu can substitute for Zr in the crystal lattice resulting in co-precipitation. Generally, the Pu substitutes directly into the crystal lattice during precipitation while the U associated with the molybdate solids more likely absorbs from the solution. The U in the NASNF solutions is present as uranyl nitrate, a 2+ cation which will not substitute as easily into the molybdate crystal lattice for the Zr 4+ ion.

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DOE OSTI2016

SRS SWPF Construction Completion

Now that construction is complete, DOE and construction contractor Parsons, are focusing on testing the Savannah River Site’s Salt Waste Processing Facility (SWPF) systems and training the workforce to operate the plant in preparation for the start of operations. Once in operation, the SWPF will significantly increase processing rates at SRS tank farms in an effort to empty the site’s high-level radioactive waste tanks.

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DOE OSTI2019

BY-110 Headspace Sampling Comparison Test: Volume 1

The Hanford Tank Operations Contractor, Washington River Protection Solutions, conducted comparison tests of two Hanford Waste tank vapor sampling systems to determine the relative differences in quantifying Chemicals of Potential Concern (COPC) while sampling the same waste tank. The systems are the traditional in situ, inline headspace sampling (HS) method and the recently developed slipstream sampling unit for testing respirator chemical cartridges known as the cartridge test (CT) rig. The comparison test was performed to determine if results obtained using the CT rig are similar to results obtained using the traditional HS method. Using the CT rig would provide efficiencies in headspace vapors sampling such as applying ALARA principles, minimizing worker entries to the tank farms, and eliminating the physical strain of manually lowering the headspace sampling bundles into the waste tanks. Six sampling events were conducted during January and February 2018 to collect headspace vapor samples from Hanford tank BY-110 with the two systems. Pacific Northwest National Laboratory was tasked with conducting an analysis of the analytical results to assess the comparability of the sampling methods and make recommendations on future testing or deployment of the CT method.

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DOE OSTI2019

BY-110 Headspace Sampling Comparison Test: Volume 2: Raw Data

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DOE OSTI2020

History of Ultrasonic Inspection of High-Level Waste Tanks at SRS - 20220

The Liquid Waste Disposition Projects (LWDP) Structural Authority and Inspection Engineering Support Group has teamed with the Materials Science and Technology Non-destructive Evaluation Group of Savannah River National Laboratory (SRNL) to implement a comprehensive In-Service Inspection (ISI) program for the High-Level Waste (HLW) tanks in the sites tank farms. The purpose of this program is to demonstrate the structural and leak integrity of the tanks to maintain the function of waste containment throughout the desired service life. Four types of waste tanks were constructed at Savannah River Site (SRS) from 1951 thru 1981 to store radioactive nuclear waste from the separations process. The Type I, II and III are carbon steel cylindrical tanks with varying degrees of access to the side walls and very limited access to the tank bottom. The tanks contain 750,000 to 1.3 million gallons of waste and are buried or backfilled with soil. The tanks are 75'-85' in diameter and 24'-33' from tank bottom to the tank roof. Inspection of the HLW tanks is made difficult by radiation, contamination, and small access openings. Through the years these challenges have been overcome by progressive improvements to programs and equipment resulting in the sophisticated wall crawler Ultrasonic Testing (UT) technology of today. A formal inspection program was developed and put in service in 1972. UT thickness measurements were first made in 1967 and 1969 of selected waste tanks using an analog-type instrument to measure the thickness of the carbon steel walls. Routine inspections for thinning were performed from 1972-1985 and then discontinued because no thinning had been observed and this technique could not detect pitting or cracking. UT inspections resumed in 1994 using a sophisticated robotic wall crawler with UT technology capable of detecting thinning, cracking and pitting. The current program focuses on the newer Type III tanks that are used primarily for storage. The program was upgraded in 2003 to include selected regions of the tank wall, secondary wall and annulus floor on a 7 to 10-year frequency. The facility is currently in its third cycle of tank inspections. Thus far, there have been no reportable indications of service induced degradation. This result provides assurance that the chemistry control program has been effective at mitigating corrosion and that the tanks remain structurally sound even after more than 40 years of service. This paper will present the UT technology first used at SRS and the evolution to the current systems and their capabilities. Additionally, plans for equipment upgrades that will improve the extent of inspection will be discussed. (authors)

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DOE OSTI2020

Assessment of the Corrosion Risks to a Double Shell Tank During the Selective Removal of a Cesium-rich Supernate Layer - 20227

The Direct Feed Low Activity Waste (DF-LAW) activity will provide the initial feed to the Waste Treatment and Immobilization Plant at the Hanford Tank Farm facility. Feed preparation for DF-LAW will be carried out in multiple double shell waste tanks (DST) utilizing the Tank Side Cesium Removal (TSCR) process. Tank AP-106 will be an integral part of the TSCR process and hence key to the DFLAW activity. Prior to being utilized for this purpose, the Cs-137 concentration levels in the AP-106 supernate must be reduced significantly. The AP-106 re-purposing process manages normal waste tank addition procedures such that waste acceptance criteria objectives for Cs-137 removal are achieved. As this process was being developed, several concerns regarding tank integrity during and after repurposing of Tank AP-106, and the associated tanks (i.e., AP-102, AN-101, and AP-108), were addressed. The potential corrosion degradation mechanisms identified based on process knowledge included: general and pitting corrosion, caustic stress corrosion cracking, concentration cell corrosion, and microbiologically induced corrosion (MIC). A systematic approach was undertaken to assess the risk of corrosion during the AP-106 re-purposing process. The assessment considered the initial and present condition of the tank, the service history of the tank, the environmental conditions created in each tank during each stage of the process, process timing, and corrosion testing and modeling that approximated tank conditions. Based on this information, recommendations were provided to minimize the exposure of the tank to corrosive conditions. These recommendations included time limits for each stage of the process, staging of corrosion inhibitor solutions should process delays occur, and waste sampling with potential chemistry adjustments at defined steps in the process. Additionally, recommendations for post-process supernate chemistry adjustments and tank inspections were put forth. The greatest risk for this process occurs during the manipulation of large quantities of Columbia River water (i.e., greater than 450,000 gallons) within AP-106, the associated tanks and the supporting infrastructure (i.e., transfer line piping). This risk becomes more pronounced if there is a process upset and the tank walls remain exposed to a corrosive condition longer than intended. As long as the river water is blended into the supernate in a timely fashion, and the waste is adjusted appropriately with corrosion inhibitors, corrosion may be minimized and the final condition of the supernate in AP-106 and the associated tanks is expected to be in compliance with corrosion chemistry requirements. Contingency plans will be made to minimize the impact of a process upset. (authors)

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DOE OSTI2013

Hanford Single-Shell Tank Leak Causes and Locations - 241-BY and 241-TY Farm

This document identifies 241-BY Tank Farm (BY Farm) and 241-TY Tank Farm (TY Farm) leak causes and locations for the 100-series leaking tanks in BY and TY Farm. The leak causes and locations report for all of the 100-series single-shell leaking tanks is one of the targets (M-045-91-T04) in the Hanford Federal Facility Agreement and Consent Order milestone M-045-91F. The T04 target requires that the Department of Energy provide to State of Washington, Department of Ecology (Ecology) a report on the 100-series single-shell tanks which have been or will be identified as having leaked in RPP-32681, Rev. 0, Process to Assess Tank Farm Leaks in Support of Retrieval and Closure Planning, leak assessment reports. The leak assessment report for BY Farm, RPP-RPT-43704, Rev. 0A, Hanford BY-Farm Leak Assessments Report, lists one 100-series tank that either continues to be or is recommended to be classified as a leaking tank in BY Farm, 241-BY-103 (BY-103). The leak assessment report for TY Farm, RPP-RPT-42296, Rev, 0, Hanford TY-Farm Leak Assessments Report, lists four 100-series tanks that either continue to be or are recommended to be classified leaking tanks in TY Farm, 241-TY-103 (TY-103), 241-TY-104 (TY-104), 241-TY-105 (TY-105), and 241-TY-106 (TY-106). All of the other eleven 100-series tanks in BY Farm and two 100-series tanks in TY Farm are classified as “sound” or are identified in RPP-RPT-43704, Rev. 0A, and RPP-RPT-42296, Rev. 0, respectively, as requiring re-assessment of their classification per TFC-ENG-CHEM-D-42, Tank Leak Assessment Process. The TFC-ENG-CHEM-D-42 assessments are not part of the M-045-91-T04 target. This BY and TY Farm leak causes and locations document is part of a series of tank farm reports that identify leak causes and locations for 100-series leaking tanks. A summary and conclusions document will be issued, RPP-RPT-54909, Hanford Single-Shell Tank Leak Causes and Locations – Summary, that compiles the results from all of the leak causes and locations tank farm reports when they have been issued which will fulfill the T04 target requirements. The identification of four of the five leaking BY and TY Farm tank leak locations focused on the first indication of radiation detected in drywells as well as liquid level decreases as appropriate, with the exception of tank TY-104 which could not be identified. Leak detection laterals were not installed underneath the BY and TY Farm tanks. For TY Farm, direct pushes were installed in 2005 to further characterize the tank leaks which were used to collaborate with the drywell data. The BY and TY Farm leaking tanks were likely due to chemistry-corrosion from the storage of Tri-butyl phosphate (TBP) waste which is conducive to stress corrosion cracking and pitting. Thermal shock (rate of temperature rise) and tank construction conditions (cold weather ductile-to-brittle transition temperature impact effects) were also likely to have affected tank integrity. There appears to be very little contribution from tank design and liner bulging. However, some or all of the factors can act serially or together to contribute to tank liner failure. The leaking BY and TY Farm tanks all stored undiluted TBP waste whereas the sound tanks stored diluted TBP waste as well as other waste types.

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DOE OSTI2013

Transuranic Waste Processing Center (TWPC) Legacy Tank RH-TRU Sludge Processing and Compliance Strategy - 13255

The U.S. Department of Energy (DOE) needs to safely and efficiently treat its 'legacy' transuranic (TRU) waste and mixed low-level waste (LLW) from past research and defense activities at the Oak Ridge National Laboratory (ORNL) so that the waste is prepared for safe and secure disposal. The TWPC operates an Environmental Management (EM) waste processing facility on the Oak Ridge Reservation (ORR). The TWPC is classified as a Hazard Category 2, non-reactor nuclear facility. This facility receives, treats, and packages low-level waste and TRU waste stored at various facilities on the ORR for eventual off-site disposal at various DOE sites and commercial facilities. The Remote Handled TRU Waste Sludge held in the Melton Valley Storage Tanks (MVSTs) was produced as a result of the collection, treatment, and storage of liquid radioactive waste originating from the ORNL radiochemical processing and radioisotope production programs. The MVSTs contain most of the associated waste from the Gunite and Associated Tanks (GAAT) in the ORNL's Tank Farms in Bethel Valley and the sludge (SL) and associated waste from the Old Hydro-fracture Facility tanks and other Federal Facility Agreement (FFA) tanks. The SL Processing Facility Build-outs (SL-PFB) Project is integral to the EM cleanup mission at ORNL and is being accelerated by DOE to meet updated regulatory commitments in the Site Treatment Plan. To meet these commitments a Baseline (BL) Change Proposal (BCP) is being submitted to provide continued spending authority as the project re-initiation extends across fiscal year 2012 (FY2012) into fiscal year 2013. Future waste from the ORNL Building 3019 U-233 Disposition project, in the form of U-233 dissolved in nitric acid and water, down-blended with depleted uranyl nitrate solution is also expected to be transferred to the 7856 MVST Annex Facility (formally the Capacity Increase Project (CIP) Tanks) for co-processing with the SL. The SL-PFB project will construct and install the necessary integrated systems to process the accumulated MVST Facilities SL inventory at the TWPC thus enabling safe and effective disposal of the waste. This BCP does not include work to support current MVST Facility Surveillance and Maintenance programs or the ORNL Building 3019 U-233 Disposition project, since they are not currently part of the TWPC prime contract. The purpose of the environmental compliance strategy is to identify the environmental permits and other required regulatory documents necessary for the construction and operation of the SL- PFB at the TWPC, Oak Ridge, TN. The permits and other regulatory documents identified are necessary to comply with the environmental laws and regulations of DOE Orders, and other requirements documented in the SL-PFB, Safety Design Strategy (SDS), SL-A-AD-002, R0 draft, and the Systems, Function and Requirements Document (SFRD), SL-X-AD-002, R1 draft. This compliance strategy is considered a 'living strategy' and it is anticipated that it will be revised as design progresses and more detail is known. The design basis on which this environmental permitting and compliance strategy is based is the Wastren Advantage, Inc., (WAI), TWPC, SL-PFB (WAI-BL-B.01.06) baseline. (authors)

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DOE OSTI2016

Low Activity Waste Pretreatment System (LAWPS) Conceptual Design Approach - 16568

The Low Activity Waste Pretreatment System (LAWPS) will be capable of providing the Waste Treatment and Immobilization Project's (WTP) Low Activity Waste Facility (LAW) the feed material needed to operate both of the LAW melters at full capacity. LAWPS will receive supernatant from the Hanford AP tank farm, filter solids from the waste, remove cesium from the waste, and then stage the feed in storage tanks for supplying the LAW facility. The LAWPS project team is currently executing the preliminary design phase of the project leading to Critical Decision 2 (CD-2). CD-2 is the approval of the performance baseline. The Critical Decision 1 (CD-1) package was approved by the Department of Energy Deputy Under Secretary in May 2015. This paper will focus on creating and gaining approval of the CD-1 package and initiating execution of the preliminary design work. The intent of the paper will be to highlight the activities that facilitated achievement of the goals and present key activities that have been performed to increase the likelihood of preliminary design success. Initiating the immobilization of Hanford tank waste will be a tremendous accomplishment. LAWPS is one of the key projects required to achieve this accomplishment. (authors)

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DOE OSTI2020

Crystalline Silicotitanate Batch Contact Testing with Ba, Ca, Pb, and Sr

Washington River Protection Solutions is working to support initial production of immobilized low-activity waste (LAW) by feeding Hanford tank supernate from tank farms to the Hanford Waste Treatment and Immobilization Plant (WTP) LAW Facility. This goal incorporates the design of a Tank Side Cesium Removal system, which filters tank waste supernate to remove suspended solids and then removes Cs by processing it through crystalline silicotitanate (CST) ion exchange media manufactured by Honeywell UOP, LLC. The 137 Cs-depleted product is intended to be sent to the WTP for vitrification. Processing of actual tank waste supernate showed effectively complete uptake of Sr and Ba by CST and significant uptake of Ca. Further, Campbell et al. (2019) analyzed CST post-column testing and found significant (>1E-2 mmoles/g) uptake of Ca and Pb along with some Ba, Cd, Fe, Sr, and U. This led to concern that selected metals, particularly the +2 cations, Ca, Sr, Ba, and Pb may be consuming Cs exchange sites and possibly reducing CST capacity for Cs. Exchange of +2 cations was assumed to be associated with the M(OH) + species for the metal (M) ion in the caustic solution. A series of batch contact testing was conducted to evaluate the exchange behavior of Ba, Ca, Pb, and Sr onto CST. The Cs exchange behavior was also tested as a benchmark for direct comparisons. The CST was provided in the sodium form by Honeywell UOP, as IONSIV TM R9140-B, Lot 2002009604, 18 x 50 mesh. A <30-mesh aliquot was collected to match the sieve fraction expected for use in upcoming small column test configurations. Kinetic exchange rate and isotherms were measured at metal concentrations benchmarked from the AP-107 tank waste feed composition and as limited by the metal solubility in the alkaline solution. Two simplified matrices were tested: 1) 1.0 M NaOH/4.6 M NaNO 3 and 2) 0.1 M NaOH/5.5 M NaNO 3 ; these matrices represented the expected 5.6 M Na concentration of process feed and served to address the hydroxide concentration effect on exchange behavior.

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DOE OSTI2020

Spent Crystalline Silicotitanate Storage Study

Washington River Protection Solutions is working to support initial production of immobilized low-activity waste (LAW) by feeding Hanford tank supernate from tank farms to the Hanford Waste Treatment and Immobilization Plant (WTP) LAW Facility. This goal incorporates the design of a Tank-Side Cesium Removal (TSCR) system, which filters tank waste supernate to remove suspended solids and then removes Cs by processing it through crystalline silicotitanate (CST) ion exchange media manufactured by Honeywell UOP, LLC. The 137 Cs-depleted product is intended to be sent to the WTP for vitrification. The Cs-loaded CST columns will be stored indefinitely, with a goal of eventual CST removal and treatment. Thus, the spent CST needs to be recoverable. The testing described herein looks to potential upset process conditions where CST storage may be required before various rinse steps are completed. This study evaluated upset conditions at three sequential processing steps envisioned for TSCR (feed, 0.1 M NaOH rinse, water rinse), and in-column drying with compressed air (normal end step) to assess impacts on the nature of the CST bed. Testing was conducted at the small scale (12-mL bed volume); simulated AP-105 tank waste was used as the feed. Following process disruption, the CST bed was dried in place at 70 °C. Post-dried CST bed physical properties (angle of repose, penetration depth, particle morphological changes) were measured to evaluate how CST moved and flowed. The testing is intended to provide a preliminary assessment of issues that may arise from desiccation of CST with the indicated salt solutions in place. Since these were small-scale tests, the processing conditions will not match full scale conditions exactly; however, the tests do provide insight into the impact of stopping processing at an earlier step than normal. Except for the feed that was dried in-place, all other process stop-conditions showed the CST bed flowed well after drying. At this small scale, CST beds would not present an issue for retrievability. The feed that was dried in place had solidified into a rock-hard monolith with no movement possible. Samples had to be chipped from the surface.

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DOE OSTI2015

Applying Hanford Tank Mixing Data to Define Pulse Jet Mixer Operation

Pulse jet mixed (PJM) process vessels are being developed for storing, blending, and chemical processing of nuclear waste slurries at the Waste Treatment and Immobilization Plant (WTP) to be built at Hanford, Washington. These waste slurries exhibit variable process feed characteristics including Newtonian to non-Newtonian rheologies over a range of solids loadings. Waste feed to the WTP from the Hanford Tank Farms will be accomplished via the Waste Feed Delivery (WFD) system which includes million-gallon underground storage double-shell tanks (DSTs) with dual-opposed jet mixer pumps. Experience using WFD type jet mixer pumps to mobilize actual Hanford waste in DSTs may be used to establish design threshold criteria of interest to pulse jet mixed process vessel operation. This paper describes a method to evaluate the pulse jet mixed vessel capability to process waste based on information obtained during mobilizing and suspending waste by the WFD system jet mixer pumps in a DST. Calculations of jet velocity and wall shear stress in a specific pulse jet mixed process vessel were performed using a commercial computational fluid dynamics (CFD) code. The CFD-modelled process vessel consists of a 4.9-m- (16-ft-) diameter tank with a 2:1 semi-elliptical head, a single, 10-cm (4-in.) downward facing 60-degree conical nozzle, and a 0.61-m (24-in.) inside diameter PJM. The PJM is located at 70% of the vessel radius with the nozzle stand-off-distance 14 cm (6 in.) above the vessel head. The CFD modeled fluid velocity and wall shear stress can be used to estimate vessel waste-processing performance by comparison to available actual WFD system process data. Test data from the operation of jet mixer pumps in the 23-m (75-ft) diameter DSTs have demonstrated mobilization, solid particles in a sediment matrix were moved from their initial location, and suspension, mobilized solid particles were moved to a higher elevation in the vessel than their initial location, of waste solids. Jet mixer pumps were used in Hanford waste tank 241-AZ-101, and at least 95% of the 0.46-m (18-in.) deep sediment, with a shear strength of 1,500 to 4,200 Pa, was mobilized. Solids with a median particle size of 43 μm, 90th percentile of 94μm, were suspended in tank 241-AZ-101 to at least 5.5 m (216 in.) above the vessel bottom. Analytical calculations for this jet mixer pump test were used to estimate the velocities and wall shear stress that mobilized and suspended the waste. These velocities and wall shear stresses provide design threshold criteria which are metrics for system performance that can be evaluated via testing. If the fluid motion in a specific pulse jet mixed process vessel meets or exceeds the fluid motion of the demonstrated performance in the WFD system, confidence is provided that that vessel will similarly mobilize and suspend those solids if they were within the WTP. The single PJM CFD-calculated jet velocity and wall shear stress compare favorably with the design threshold criterion estimated for the tank 241-AZ-101 process data. Therefore, for both mobilization and suspension, the performance data evaluated from the WFD system testing increases confidence that the performance of the pulse jet mixed process vessels will be sufficient to process that waste even if that waste is not fully characterized.

mixing' slurry↗

DOE OSTI2020

Characterization and CST Batch Contact Equilibrium Testing of Modified Tank 9H Process Supernate Samples in Support of TCCR

The Tank Closure Cesium Removal (TCCR) system uses ion exchange columns filled with crystalline silicotitanate (CST) media to process radioactive waste solutions for the removal of ¹³⁷Cs. TCCR currently focuses on dissolving Savannah River Site (SRS) radioactive tank waste (primarily sodium saltcake solids) within Tank 10H followed by at-tank ion exchange column treatment. Two supernate batches from Tank 10H have been processed through the TCCR unit and processing of a third batch is expected soon. After processing of this supernate batch, plans are to replace the CST columns and process dissolved salt solution from Tank 9H through Tank 10H and then through the new CST columns installed in the TCCR unit. The new columns are expected to contain either a media similar to an archived CST batch (IE-911) or the R9120-B CST media used in the current TCCR columns (the two materials are fundamentally the same; just different specifications, product names, and preconditioning steps). Samples of Tank 9H dissolved saltcake were received at the Savannah River National Laboratory (SRNL) and characterized. The Tank 9H supernate contained a high sodium concentration (~9.6 M Na⁺) and will require dilution to near 6 M [Na⁺] prior to processing through the TCCR unit. The cesium concentration in Tank 9H is currently significantly higher than was observed with Tank 10H. Three dilutions of the Tank 9H supernate were conducted to mimic possible dilutions that could be conducted in the tank farm prior to TCCR processing using inhibited water, sodium hydroxide, and sodium nitrate solutions. Dilution #1 was prepared by diluting the Tank 9H supernate by a factor of 1.6 with inhibited water, Dilution #2 was prepared by diluting the Tank 9H supernate by a factor of 3.7 with a mixed sodium hydroxide/sodium nitrate diluent, and Dilution #3 was prepared by also diluting by a factor of 3.7 but with sodium hydroxide only. All three dilutions have similar Na⁺ concentrations (~6 M), but Dilutions #2 and #3 contain significantly less cesium. Major and key minor components of the diluted Tank 9H supernate samples are provided in Table ES-1. Batch contact equilibrium tests were conducted with the Tank 9H dilutions and the two different CST media batches being considered for use in the new TCCR columns. Results are summarized in Table ES-2 and compared to ZAM model predictions. The highest cesium distribution coefficient and percent removal were observed with Dilution #3. IE-911 CST (an archived CST media batch) was more effective at removing cesium than the more recently prepared R9120-B CST media, though both media samples removed >88% of the cesium and the differences may not be statistically different considering the overall uncertainty. Based on the results, maximum cesium loadings were calculated for each CST media type and Tank 9H dilution. In general, maximum cesium loadings from dilutions of this supernate batch are quite high (approaching 0.1 mmol total Cs⁺/g CST for Dilution #1). The highest calculated maximum ¹³⁷Cs loading for the Tank 9H dilutions using the ZAM model with input of the tank compositions and batch contact results was 207 Ci/kg CST (Dilution #1 with IE-911 CST). In all cases, higher maximum cesium loading values were predicted for IE-911 CST versus R9120-B, although the differences varied considerably between the dilutions. The maximum loading value for IE-911 CST with Tank 9H Dilution #1 was only 7% higher than the maximum loading for R9120-B. The maximum loading value for IE-911 CST with Dilution #3 was 24% higher than the maximum loading for R9120-B. Dilution #2 was intermediate between these values. Note that these maximum loading values are the theoretical calculated values, and actual operating conditions will cause differences. A CST binder dilution (correction) factor near 0.7 (relative to pure powder CST) was required for each batch contact test with IE-911 engineered CST using the three Tank 9H dilutions. Correction factors calculated for R9120-B CST ranged from 0.56 to 0.66 for the three dilutions. Following the batch contact tests, the CST samples were isolated from the Tank 9H solution, washed, dried, and digested in acid following established procedures. The analysis results are provided in Table ES-3. Total cesium loading values determined by CST digestion were similar to the calculated loading values based on solution analysis (Table ES-2) for all samples. In addition, the CST was observed to load calcium (R9120-B sample only), iron, strontium, lead, uranium, and plutonium after contact with the waste supernate, as has been observed previously.

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DOE OSTI2016

Mercury speciation comparison. BrooksApplied Laboratories and Eurofins Frontier Global Sciences

The Savannah River National Laboratory (SRNL) was tasked with preparing and shipping samples for Hg speciation by Eurofins Frontier Global Sciences (FGS), Inc. in Bothell, WA on behalf of the Savannah River Remediation (SRR) Mercury Program Team. These samples were analyzed for seven species including: total mercury, dissolved mercury, inorganic mercury ((Hg(I) and Hg(II)), elemental mercury, methylmercury, ethylmercury, and dimethylmercury, with an eighth species, particulate mercury, calculated from the difference between total and dissolved mercury after subtracting the elemental mercury. The species fraction of total mercury measured has ranged broadly from a low of 32% to a high of 146%, though the vast majority of samples have been <100%. This can be expected since one is summing multiple values that each have at least a ± 20% measurement uncertainty. Two liquid waste tanks particularly important to understanding the distribution of mercury species in the Savannah River Site (SRS) Tank Farm were selected for a round robin analysis by Eurofins FGS and BrooksApplied Laboratories (BAL). The analyses conducted by BAL on the Tank 22 and 38 samples and their agreement with those obtained from Eurofins FGS for total mercury, dissolved mercury, methylmercury, ethylmercury, and dimethylmercury provide a strong degree of confidence in these species measurements

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DOE OSTI2019

Cesium Ion Exchange Testing Using a Three-Column System with Crystalline Silicotitanate and Hanford Tank Waste 241-AP-107

Washington River Protection Solutions (WRPS) is working to support early production of immobilized low-activity waste by feeding Hanford tank supernate from tank farms to the Hanford Waste Treatment and Immobilization Plant (WTP) Low-Activity Waste (LAW) facility. This goal incorporates the design of a Tank-Side Cesium Removal (TSCR) system, which in effect filters tank waste supernate and processes it through a cesium ion exchange medium to remove 137Cs. The 137Cs-depleted product is sent to the WTP for vitrification. Rovira et al. (2018) reported the successful Cs removal from Hanford tank 241-AP-107 waste (hereafter called AP-107) using crystalline silicotitanate (CST) ion exchange media manufactured by Honeywell UOP, LLC (product IONSIVTM R9140-B, Batch 2081000057) in a lead-lag column system. Since that testing, WRPS has changed the column design to a three-column system. WRPS requested a repeated study with AP-107 tank waste using a different batch of IONSIVTM R9140-B, Lot 2002009604, in a three-column format. A small-scale test platform was constructed to demonstrate solids filtration, Cs removal, and LAW vitrification and installed at Pacific Northwest National Laboratory. This report describes the small-scale ion exchange testing system component of the test platform and the processing of approximately 8.55 L of filtered AP-107 supernate using CST, Lot 8056262-999, that passed through a 25-mesh filter. This report also describes the Cs ion exchange batch contact testing to determine the Cs distribution coefficient and the maximum Cs loading capacity in the AP-107 tank waste matrix. Batch contact testing helps to evaluate CST performance on tank waste supernate and is often used prior to processing tank waste through ion exchange columns to assess some performance metrics (e.g., 50% Cs breakthrough). Batch contact tests were performed with the filtered AP-107 tank waste at four Cs concentrations at a phase ratio of 200 (liquid volume to exchanger mass). The distribution coefficient (K d ) at the equilibrium condition of 9.2 µg Cs/mL (AP-107 feed condition) was determined to be 806 mL AP 107/g CST. With a CST bed density of 1.01 g/mL (<25 mesh CST), this K d corresponded to a predicted 50% Cs breakthrough of 814 bed volumes (BVs). The Cs load capacity at the equilibrium feed condition was determined to be 8.3 mg Cs/g dry CST. The three-column format testing was prototypic to the intended TSCR operations, albeit on a small scale with 10-mL CST beds. Flowrate was adjusted to match the CST contact time expected for the full-scale operation, i.e., matched bed volumes per hour (BV/h) flow rate. The feed was processed downflow through the lead column, then through the middle column, and then through the polish column. Loading continued at an average of 1.88 BV/h (1.83 to 2.04 BV/h range) until the entire available AP-107 feed was processed. The Cs-decontaminated product will be provided for vitrification testing. The lead column only reached 45% Cs breakthrough after processing 855 BVs of feed. The 50% Cs breakthrough was extrapolated to occur at ~900 BVs. This extrapolated 50% Cs breakthrough value differed from the batch contact estimate (814 BVs) by 13%. The waste acceptance criteria (WAC) or contract limit for the WTP LAW vitrification facility is 3.18E-5 Ci 137 Cs per mole Na. For the AP-107 tank waste, only 0.127% of the influent 137 Cs concentration may be delivered to the WTP; this required a Cs decontamination factor of 787. The Cs effluent from the middle column reached the WAC after processing 590 BVs. Cs breakthrough from the polish column began at 590 BVs, reaching 6.3E-3 µCi/mL or 4.3E-3% Cs breakthrough after processing 844 BVs of feed.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2019

Waste Chemistry Envelope for the Determination of Pitting Corrosion Susceptibility - 19554

Liquid radioactive wastes at the Hanford and Savannah River sites are stored in large underground carbon steel tanks. The high-level wastes are processed in several of the tanks and then transferred by piping to other site facilities for further processing before they are stabilized in a vitrified or grout waste form. Based on waste removal and processing schedules, many of the tanks, will be required to be in service for times exceeding the initial intended life (i.e., greater than 60 years). Until the waste is removed from storage, transferred, and processed, the materials and structures of the tanks must maintain a confinement function by providing a barrier to the environment and by maintaining acceptable structural stability during design basis events, which include loadings from both normal service and abnormal (e.g., earthquake) conditions. Administrative programs are in place to mitigate potential corrosion mechanisms and thereby maintain the structural and leak integrity functions of these waste tanks throughout their intended service life. Waste chemistry and temperature control are the means by which corrosion degradation of the waste tanks is minimized. Chemistry controls are based on in-situ coupon tests, waste tank experience, and laboratory testing. These requirements comprise the technical standards for corrosion control. The standards are utilized then as guidelines for operational procedures. The present waste chemistry controls for the Hanford DSTs were established in the 1980's in response to tank failures caused by stress corrosion cracking (SCC) at the DOE Savannah River Site (SRS). Portions of the SRS chemistry limits, which were developed at the Savannah River National Laboratory (SRNL) were coupled with corrosion testing results from Pacific Northwest National Laboratories (PNNL) and adopted for corrosion control of the double-shell tank (DST) waste at the Hanford Site. Since that time, the temperatures of the waste in the DSTs have decreased to less than 50 deg. C in most cases as the radioactive material has decayed. As a consequence, new chemistry controls were formulated for SCC in 2010. This testing however, did not address that potential for pitting in the supernatant and at the liquid-air interface. Indeed, initial tests indicated that the inhibitor requirements for SCC would be insufficient for the prevention of pitting. In addition to lower waste temperatures, future retrieval and process changes may impact the DST waste chemistry. Initial projections suggest that the waste chemistry of the DSTs may shift to a broader range of pH and higher aggressive anion concentrations (e.g., chloride, sulfate, etc.) than the wastes that are presently stored. Additionally, processes within the vitrification facility may result in streams that are returned to the tank farm for evaporation. These streams may also contain high concentrations of aggressive species. SRNL investigated the propensity for pitting of the carbon steel waste tanks at current and projected DST waste chemistries. A statistically designed series of tests provided a pitting factor that relates the ratio of the inhibitor species to the aggressive species and the probability of observing pitting. An acceptable pitting factor was determined and was utilized for the development of a new chemistry envelope. The new chemistry envelope was compared to the envelope that was established for SCC and was determined to be bounding. Validation of the new chemistry envelope was performed via model simulations and comparison with historical experimental results and approaches to establishing chemistry envelopes. The new chemistry envelope will eventually be part of an overall assessment of the condition of the tanks and any changes made to the overall structural integrity program for the Hanford DSTs. (authors)

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