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DOE OSTI2022

Characterization of the Sulfur-Saturated Melt Versions of the LAW HPVR Glasses

This report provides the results from the chemical analyses of a sulfur-saturated melt versions of the Low-Activity Waste High PCT and VHT Response study glasses, which are a series of simulated nuclear waste glasses designed and fabricated at Pacific Northwest National Laboratory. These data will be used in the development, validation, and implementation of enhanced property/composition models for waste glass vitrification at Hanford. Chemical analyses were performed on a representative sample of each of the sulfur-saturated melt versions of the glasses to allow for comparisons with targeted compositions, as well as the measured compositions of the quenched glasses. The relative differences between the targeted and measured concentrations of B 2 O 3 , K 2 O, Li 2 O, V 2 O 5 , and ZrO 2 for several of the glasses were greater than ±10%. The relative difference between the targeted and measured concentrations of SO 3 were greater than 10% for all study glasses. The wash solutions contained mainly sodium, sulfur, and sulfate ions.

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DOE OSTI2023

Modeling of Chemical Slurry Rheology in DWPF Sludge Batch (SB) 10 Simulants

The Defense Waste Processing Facility (DWPF) treats high-activity radionuclides from sludge through a process called vitrification. This process converts radioactive liquid waste currently stored in tank farms into a solid glass form that is suitable for long-term storage and disposal. Due to the complexities involved in vitrifying this waste within each operation of the Chemical Processing Cell (CPC), waste rheology is studied to characterize the fluid-mechanical properties as it passes through the CPC and into the Melter. To better understand the waste and validate flow behavior, slurry rheology of simulants that represents the waste was studied at various acid stoichiometry percentages and solids concentrations to determine the simulant’s yield stress and viscosity. This research work has been supported by the DOE-FIU Science & Technology Workforce Development Initiative, an innovative program developed by the U.S. Department of Energy’s Office of Environmental Management (DOE-EM) and Florida International University’s Applied Research Center (FIU-ARC). During the spring of 2022, a DOE Fellow intern, Brendon Cintas, spent 10 weeks doing a summer internship at Savannah River National Laboratory (SRS) under the supervision and guidance of Dan Lambert, Chemical Flowsheet Development. The intern’s project was initiated on June 6, 2022, and continued through August 11, 2022 with the objective of assisting scientists at SRNL’s Rheology and Grout Laboratory at Aiken Country Technology Lab (ACTL) better understand the sludge composition on the rheology of a simulant slurry using a HAAKE RheoStress 6000 rheometer and extrapolate the results to the real-waste data.

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DOE OSTI2023

Technical Evaluation of Accelerated Basin De-Inventory Material Addition to Sludge Batch 11

Savannah River Nuclear Solutions has a need to discard spent nuclear fuel (SNF), currently stored in L Basin, to the Defense Waste Processing Facility (DWPF) for vitrification. The Department of Energy (DOE) has approved the Accelerated Basin De-inventory (ABD) Program for discarding SNF via transfers from H-Canyon to the Savannah River Site (SRS) Liquid Waste (LW) system. The first ABD discards will occur during the preparation of Sludge Batch (SB) 11. An initial impact evaluation of the LW flowsheet was performed by the Savannah River National Laboratory (SRNL) prior to the approval of the ABD Program. This evaluation addressed the LW downstream facilities based on the current H-Canyon flowsheet sequence for the average ABD discard. The flowsheet evaluation only included aluminum-clad SNF, specifically Materials Test Reactor (MTR) fuel and High Flux Isotope Reactor (HFIR) fuel similar to the planned SB11 discard. Following this evaluation, the flowsheet has been slightly altered to address (i) new nuclear criticality safety controls for DWPF that credit a higher amount of gadolinium as a neutron poison for all of the enriched uranium contained in a SB and (ii) potential additions of the H-Canyon neutralized fuel stream prior to the Low Temperature Aluminum Dissolution (LTAD) process in Tank 51. The early introduction of ABD material into the SB assembly process is being investigated to provide flexibility regarding transfer opportunities for H-Canyon to Tank 51 for SB11 and future sludge batches.

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DOE OSTI2023

Decoding Zeolite Crystallization and Stage III in Nuclear Waste Glasses by Coupled Modeling and Experiments

Under specific conditions of pH and temperature, nuclear waste immobilization borosilicate glasses may exhibit a sudden acceleration in their corrosion kinetics (stage III)—a behavior that has been associated with the formation of zeolite crystals. Such accelerated dissolution may compromise the integrity of nuclear wasteforms placed in geological depositories. However, thus far, none of the available models is able to predict the thermodynamic propensity and kinetics of zeolite precipitation as a function of the solution conditions due to (i) a lack of fundamental knowledge regarding the nucleation & growth mechanisms of zeolitic phases, (ii) uncertainty regarding the compositions (types) of zeolites that may form and the rate-limiting step in their precipitation as a function of the solution conditions, and (iii) the complexities that arise due to the vast parametric space (i.e., solution chemistry, temperature, number of secondary phases, etc.) that encompass these systems under conditions of environmental exposure. To resolve these challenges, this project aimed to unambiguously identify the thermodynamic propensity for zeolite precipitation and the kinetics thereof as a function of the solution conditions (composition, pH, and temperature). To achieve this goal: 1) We identified the solution conditions and zeolite phases relevant to nuclear glass dissolution. 2) We performed a series of ab initio molecular dynamics (AIMD) simulations to compute the thermodynamic properties of a group of characteristic zeolites that features a large range of compositions, various hydration levels, a wide range of framework structures, and partial atomic site occupancies. 3) We released a first-of-a-kind self-consistent thermodynamic database that can be used to assess the kinetics and the stability fields of zeolitic phases within a Gibbs energy minimization (GEM) framework. 4) We developed a robust geochemical modeling method allowing us to predict the stability of secondary phases (including zeolites, calcium–silicate–hydrate gels, and clays) upon the dissolution of nuclear waste immobilization glasses. 5) We introduced a model that predicts the dissolution kinetics of a series of borosilicate nuclear waste immobilization glasses in terms of the topology of their atomic network. 6) We investigated the roles of the solution composition on the crystallization kinetics of phillipsite zeolites and tobermorite silicate hydrates. Via PNNL’s collaboration and engagement, this project directly supports DOE’s nuclear waste immobilization activities by offering a technical, science-based foundation that will (i) facilitate predictions of the long-term corrosion rates and extents of existing nuclear waste immobilization glasses to help ensure safe and successful vitrification operations, (ii) inform the development of advanced glass formulations with enhanced durability, and, (iii) enable cost-savings that result from making more decisive and hence less conservative predictions while offering higher levels of nuclear waste embedment in smaller, more compact glass volumes.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2023

Characterization of the Sulfur-Saturated Melt Versions of the HLW HAlG Glasses

This report provides the results from the chemical analyses of a series of sulfur-saturated melt versions of the High-Level Waste High-Aluminum Glass study glasses, a series of simulated nuclear waste glasses designed and fabricated at Pacific Northwest National Laboratory. These data will be used in the development, validation, and implementation of enhanced property/composition models for waste glass vitrification at Hanford. Chemical analyses were performed on a representative sample of each of the sulfur-saturated melt versions of the glasses to allow for comparisons with targeted compositions as well as the measured compositions of the quenched glasses. The relative differences between the targeted and measured concentrations of B 2 O 3 , Cr 2 O 3 , K 2 O, Li 2 O, Na 2 O, and P 2 O 5 for several of the glasses were greater than ±10%. The relative differences between the targeted and measured concentrations of Al 2 O 3 and ZrO 2 for one of the glasses were greater than ±10%. As expected, the measured concentrations of SO 3 in most of the glasses were higher than targeted due to the use of the sulfur saturation method in fabricating these glasses. The wash solutions contained mainly sodium, sulfur, and sulfate ions.

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DOE OSTI2021

Measurement of Iodine, Iodide, and Iodate in Hanford Tank Waste: Technology Transfer from PNNL to Hanford 222-S Laboratory

This report summarizes the measurement of the inorganic chemical forms of iodine in Hanford tank waste. The Hanford tank wastes have roughly a part per million iodine. Part of the iodine is the long-lived beta emitter 129I, and the rest is stable 127I. Because tank waste iodine is radioactive and radiotoxic, its chemical form must be known so that its behavior in the vitrification process can be reliably known and anticipated in various waste streams (glass, secondary liquid and solid waste, and offgas emissions) at Hanford. Iodine in tank wastes exists in the inorganic chemical forms iodide and iodate (and possibly also periodate) and also as organic forms such as alkyl iodides. The measurement of organic iodides is very different from the measurement of inorganic forms and is outside the scope of this report. The inorganic chemical forms are chemically separated, in sequence, from the raw tank waste using solvent extractions and several redox reactions, then measured by ICP-MS. The inorganic chemical forms of iodine are chemically reactive, and so is the tank waste. The chemistry must be carefully designed to avoid unintended reactions that could convert one form of iodine to another during the analysis, which would skew the data and report iodine in the wrong chemical form. This iodine analysis, developed at PNNL, is being transferred to the DOE 222-S Laboratory on the Hanford Site, in Washington State, for implementation during waste processing operations.

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DOE OSTI2023

Product Consistency Test Results for the LAW HPVR Glasses

This report summarizes the chemical analysis of Product Consistency Test (PCT) leachates received from Pacific Northwest National Laboratory (PNNL). The leachates are from a series of simulated nuclear waste glasses designated Low-Activity Waste High PCT and VHT Response (LAW HPVR) glasses that were designed and fabricated at PNNL. The glasses included both quenched and canister centerline cooled glasses. The reported data will be used in the development, validation, and implementation of enhanced property/composition models for waste glass vitrification at Hanford. The elemental release for the study glasses is reported as normalized concentration (NC i ). NC i of several elements was computed for both the target and measured glass compositions, which were similar, resulting in no significant differences when computing the NC i values. The majority of the glasses exhibited NC B , NC Na , and NC Si values that were greater than the Hanford Tank Waste Treatment Plant (WTP) low-activity waste constraint of 4 g/L. Several blank solutions included with the study glasses had K, Na, and Si concentrations above the analytical detection limit. Additionally, several of the reference glasses that were included with the study glasses had Na concentrations that were higher than expected. The unexpected analyte concentrations in the reference glass and blank solutions were insignificant with respect to the reported NC i values, and are noted for completeness and their experimental relevance.

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DOE OSTI2023

Technical Evaluation of Accelerated Basin De-Inventory Material Addition to Sludge Batch 11 (Rev. 1)

The Accelerated Basin De-inventory (ABD) program involves discarding spent nuclear fuel that is currently stored in L-Basin to the Defense Waste Processing Facility (DWPF) for vitrification. The first ABD discards will occur during the preparation of Sludge Batch (SB) 11. Savannah River Mission Completion has requested that the Savannah River National Laboratory assess the technical gaps related to the increased gadolinium poisoning requirement and the impacts of performing the Low Temperature Aluminum Dissolution (LTAD) process in Tank 51 with H-Canyon discards present. The following summarizes the evaluation of the impacts of increasing the quantity of gadolinium (and related topics) from what was previously evaluated in the SRNL studies of gadolinium-poisoned ABD material solubility, the overall ABD flowsheet review, and increasing the fissile mass loading in glass: 1) Based on literature surveys, there is no indication that organic interactions with gadolinium will be significant at the high pH (typically >13) conditions of the Concentration, Storage, and Transfer Facilities. Any interactions of gadolinium with organics in DWPF are not expected to adversely impact DWPF or downstream facilities. Thus, there is little-to-no residual risk from organic interactions with gadolinium [Gap closed]; 2) Adding depleted uranium to ABD material, targeting 235 U enrichment of 4.90% within each transfer window, will mitigate potential impacts from an increase in soluble 235 U enrichment during sludge washing and LTAD. The plan to take advantage of previous transfers and allow 235 U enrichment of >5% during the final transfer window carries a risk that Tank 51 supernate will have a 235 U enrichment of >5%, which should be evaluated for acceptance; 3) Increasing the gadolinium mass ratio to 3.0:1 Gd: 235 U(eq SLU ) should lead to the same or higher partitioning of gadolinium into the solid phase within the DWPF Chemical Process Cell, resulting in both liquid and solid phases with expected partitioning of Gd consistent with the prior solubility study [Gap closed for SB11]; 4) There are no expected impacts on DWPF melt temperature and melter operations due to the minimal ~0.2 weight percent (wt%) increase in Gd concentration relative to previous sludge batches [Gap closed for SB11]; 5) As observed previously, Gd is expected to enter the off-gas system via physical entrainment, but at a slightly higher concentration than what was observed for SB9 melter off-gas pluggage deposits (0.07 wt%) [Gap closed for SB11] ; 6) There are no expected impacts on DWPF recycle or the Recycle Collection Tank glycolate destruction process. [Gap closed for SB11]; 7) Gd is projected to be a trace component in the SB11 glass (<0.5 wt%) and can be ignored for process control. Trace components do not significantly impact glass durability, thus the conclusions of the previous Product Consistency Test evaluation at a fissile mass loading of 2,500 g fissile/m3 glass still applies to SB11. The ~0.1 wt% increase in Gd2O3 concentration relative to the previous study will not impact the predictability of SB11 glass with the DWPF Product Composition Control System (PCCS) models for durability or the acceptability of glass according to the Waste Acceptance Product Specifications (WAPS) criterion for product consistency [Gap closed for SB11]; 8) No additional Toxicity Characteristic Leaching Procedure testing is necessary for SB11 and the hazardous waste specification of the SB11 DWPF waste form is unchanged after the addition of the ABD stream [Gap closed for SB11]. The following summarizes the evaluation of the impacts of adding two-thirds of the ABD material to Tank 51 prior to LTAD: 1) The addition of two-thirds of the ABD increases overall aluminum mass from 1.39×10 4 kg to 1.64×10 4 kg (15.5% ABD Al). The form of the insoluble portion of the Al resulting from ABD addition should be the more readily dissolved Al(OH) 3 and amorphous forms. The portion of the ABD aluminum that is processed by LTAD is expected to be completely soluble, thus requiring that less of the boehmite in the sludge be dissolved to reach the same Al target in the SB. [Gap closed for SB11]; The expected LTAD impact on other components, as related primarily to the components in ABD, are discussed. Gd is expected to remain insoluble during LTAD and not impact the solubility of other components. [Gap closed for SB11]; The addition of two-thirds of the ABD increases overall projected SB11 uranium mass from 4,740 kg to 13,100 kg (63% ABD U) and the projected plutonium mass from 86.0 kg to 89.5 kg (3.9% ABD Pu). The addition of all of the ABD increases overall projected SB11 uranium mass from 4,740 kg to 16,100 kg (70% ABD U) and the projected plutonium mass from 86.0 kg to 90.4 kg (5.3% ABD Pu). The 235 U enrichment will be ≤5%. The fissile uranium will be adequately poisoned by Gd and the fissile Pu will be adequately poisoned by Fe from the sludge. [Gap closed for SB11]; There is a low risk that ABD addition will impact the rheology or pumpability of the slurry. There is a low but higher risk of ABD addition prior to LTAD impacting the settling rate; Based on the evaluation of adding two-thirds of the ABD material and all of the ABD material prior to the LTAD process, there is no volume or mass limit that would need to be imposed on ABD additions prior to LTAD. [Gap closed for SB11]. Revision 1 of this report addresses a variation on the ABD additions and LTAD strategy where sodium hydroxide additions for LTAD may be performed intermittently or concurrently with an ABD addition window. The proposed change does not alter the conclusions of this evaluation.

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DOE OSTI2023

Product Consistency Test Results for the LAW ML1 Glasses

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DOE OSTI2023

Composition Measurements of the LAW ML1 Glasses

This report provides the results from the chemical analyses of the glass compositions of the quenched Low Activity Waste Machine Learning study glasses, a series of simulated nuclear waste glasses designed and fabricated at Pacific Northwest National Laboratory. These data will be used in the development, validation, and implementation of enhanced property/composition models for waste glass vitrification at Hanford. Chemical analyses were performed on a representative sample of each of the quenched glasses to allow for comparisons with target compositions. The relative differences between the target and measured concentrations of F - for one glass, P 2 O 5 for two glasses, SO 3 for three glasses, and ZrO 2 for two of the glasses were greater than 10%. These results can be used in further characterization of this series of glasses, including the normalization of Product Consistency Test results.

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DOE OSTI2023

Product Consistency Test Results for the LAW Phase 5 Rerun Leachates

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DOE OSTI2023

Phosphate and Fluoride Processing Options for Hanford Sludge

The Direct Feed High-Level Waste (DFHLW) strategy represents an alternative flowsheet to bypass the Hanford Waste Treatment and Immobilization Plant (WTP) Pretreatment Facility. Key processing functions previously captured during baseline pretreatment operations include leaching and washing prior to solids concentration and should be considered in the new DFHLW flowsheet to maximize waste feed loading, minimize high-level waste (HLW) volume, and mitigate corrosion challenges associated with vitrification of high phosphate and fluoride concentrations. The effectiveness and efficiency of sludge washing can have a substantial impact on DST space and mission duration. Two target species that benefit significantly from washing are phosphate and fluoride. Commonly present in many high-level wastes at Hanford, phosphate and fluoride are found predominately in the form of salt precipitates and can have adverse and detrimental effects on glass waste loading. Additionally, fluoride produces melter off-gas that creates corrosion risks in the off-gas system piping. Determining the solubilities of fluoride and phosphate salts, as well as the dissolution kinetics under potential HLW processing conditions will help to mitigate future operational risks and mature flowsheet technical bases.

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DOE OSTI2023

Characterization of the Sulfur-Saturated Melt Versions of the LAW ML1 Glasses

This report provides the results from the chemical analyses of the sulfur-saturated melt versions of the Low-Activity Waste Machine Learning study glasses, a series of simulated nuclear waste glasses designed and fabricated at Pacific Northwest National Laboratory. These data will be used in the development, validation, and implementation of enhanced property/composition models for waste glass vitrification at Hanford. Chemical analyses were performed on a representative sample of each of the sulfur-saturated melt versions of the glasses to allow for comparisons with targeted compositions as well as the measured compositions of the quenched glasses. The relative differences between the targeted and measured concentrations of F- for one glass, K 2 O for one glass, Na 2 O, for one glass, P 2 O 5 for one glass, and ZrO 2 for several of the glasses were greater than ±10%. As expected, the measured concentrations of SO 3 in most of the glasses were higher than targeted due to the use of the sulfur saturation method in fabricating these glasses.

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DOE OSTI2023

Product Consistency Test Results for the HLW HAlG Glasses

This report summarizes the chemical analysis of Product Consistency Test leachates received from Pacific Northwest National Laboratory (PNNL). The leachates are from a series of quenched simulated nuclear waste glasses designated High-Level Waste High Aluminum Glass that were designed and fabricated at PNNL. The reported data is provided to be used in the development, validation, and implementation of enhanced property/composition models for waste glass vitrification at Hanford. The elemental release for the study glasses is reported as normalized concentration NCi. NCi of several elements was computed for both the target and measured glass compositions. Several of the glasses exhibited NC B , NC Li , and/or NC Na values that were greater than the Environmental Assessment (EA) benchmark values. Several of the leachates from approved reference material (ARM) glasses included with the study glasses had elemental concentrations greater than the expected ranges. Two water blanks contained measurable amounts of Si; measurements confirmed by rerun samples. One water blank also contained a measurable amount of Na.

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DOE OSTI2023

Modelling the Liquid Waste Operation at the Savannah River Site

Modeling Successes Dounreay – Site Closure Optimization and Risk Reduction Re-structuring and streamlining a complex project plan to achieve site decommissioning in reduced time and at reduced cost, through automated task prioritization. Idaho AMWTP – Multi-stream Optimization Speeding up a complex facility with many process lines, by utilizing all of the process lines more efficiently and reducing overall plant downtime, by coordinating repairs and shutdowns. AWE –Waste Repackaging and Relocation Relocating schedule for waste material from an old storage facility to a new purpose-built one, safely, and in a timely fashion that removed the need to reassure the safety of the old facility. Sellafield – Effluent, Sludge and HAW Treatment Improving a wide range of chemical engineered processes including aqueous effluent treatment, chemically-reactive sludge management and waste vitrification processing. Strategic Petroleum Reserve – Cavern Management Linking chemistry models of petroleum prediction, through engineering cavern management to financial modeling of gasoline sales to benefit US government

Jung, Andrew W.↗

DOE OSTI2023

Organic Evaporation, Oxidation, and Hydrolysis Testing in Support of Hanford Sample-and-Send

The Hanford site has approximately 56 million gallons of radioactive mixed waste stored in 156 unretrieved underground storage tanks. The Hanford Waste Treatment and Immobilization Plant (WTP) is being built to treat and immobilize the tank waste. The baseline method for immobilization of Low Activity Waste (LAW) through the WTP is vitrification, but additional immobilization capacity is needed to supplement the initial LAW melters. An alternative cementitious waste form is being investigated for that future immobilization method. However, one impediment to a cementitious waste form is the presence of Land Disposal Restricted (LDR) organic chemicals in tank waste, which are regulated on a concentration-based standard in the final waste form. Hence, if the quantity of organics in LAW is high enough, they must be destroyed or removed to make a waste form compatible with disposal in a mixed low level waste landfill. This work evaluates potential avenues for treatment of LDR organics to eliminate the impediment and permit possible use of a cementitious waste form.

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DOE OSTI2023

Composition Measurements of the HLW APPS Glasses

This report provides the results from the chemical analyses of the glass compositions of the High Activity Waste Aspen Process Performance Simulation (HLW APPS) study glasses, a series of simulated nuclear waste glasses designed and fabricated at Pacific Northwest National Laboratory. These data will be used in the development, validation, and implementation of enhanced property/composition models for waste glass vitrification at Hanford. Chemical analyses were performed on a representative sample of each of the quenched glasses to allow for comparisons with targeted compositions. The relative differences between the targeted and measured concentrations of F- for three glasses and B 2 O 3 for five glasses were greater than 10%. These results can be used in further characterization of this series of glasses, including the normalization of Product Consistency Test results.

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DOE OSTI2024

Improving Efficiency of DWPF Operations via Automating Process Calculations and Vitrifying High-Curie Feed- 24529

The Liquid Waste Organization (LWO) at the Savannah River Site (SRS) uses a “Power As One®” motto to process and dispose of radioactive waste. The Defense Waste and Processing Facility (DWPF) treats the high-level waste through a process of vitrification. The DWPF receives three incoming waste streams that are added to the Sludge Receipt and Adjustment Tank (SRAT): sludge, Monosodium Titanate/Sludge Solids (MST/SS), and Strip Effluent (SE). The liquid waste is mixed with pre-fabricated frit and treated with high temperatures in the melter prior to being poured into stainless steel canisters. The liquid cools to form solid glass within these canisters that are suitable for long-term storage and disposal. Savannah River Mission Completion (SRMC), the SRS liquid waste contractor for the U.S. Department of Energy, has implemented several facility improvements to further enhance the operations to support the Liquid Waste Operation (LWO) mission. Two of these operational enhancements include implementing the electronic Material Tracking Program Calculator (eMTPC)software and increasing the DWPF canister heat rate limit.

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