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DOE OSTI2024

A banner year for solar balloon technology

Solar-powered stratospheric balloons achieved major advancements in test flights, developmental milestones, and operational achievements this year. A solar-powered stratospheric balloon system known as the heliotrope, has emerged as a low-cost platform capable of carrying several pounds of scientific payload to altitudes ranging from 50,000 to 75,000 feet (Bowman et al., 2020; Image 1) for multi-hour level flights. This innovative system has facilitated groundbreaking scientific discoveries in areas such as infrasound and atmospheric composition. Unlike sealed weather balloons that burst, these balloons remain buoyant by retaining hot air within their open envelopes. Because they are solar-powered, they remain aloft as long as the sun remains unobscured.

14 SOLAR ENERGY↗
DOE OSTI2024

HERO CarbonSAFE Phase 2 Project in the Columbia River Basalt Group

The Hermiston, Oregon Basalt CarbonSAFE Phase II project (HERO CarbonSAFE) seeks to accelerate the deployment of commercial carbon dioxide (CO2) storage projects in basaltic rocks. Basalt CO2 storage has several advantages to conventional saline storage reservoirs including 1. The potential for rapid mineralization of CO2, 2. Associated decreases in pressure and CO2 migration risks, 3. Reduced long-term monitoring requirements with respect to plume tracking, 4. Widespread geographic distribution and, 5. Large storage potential due to thickness, porosity, and CO2 interactions with basalt. And for locations such as the Pacific Northwest, Hawaii, Iceland, India and Japan, basalts may offer the only economically feasible option for local CO2 storage. However, there are limited field-scale assessments of CO2 storage in basalt, and current carbon capture utilization and storage (CCUS) permitting and regulatory frameworks were developed for conventional saline reservoirs. HERO CarbonSAFE is designed to address research gaps and uncertainties associated with basalt storage. Specifically, the project will assess the feasibility of CO2 injection in the deep layered basalts, long-term storage (mineralization), practical approaches for large-scale implementation (50+ million metric tons of CO2 over 30 years), lithology-specific risks, and the technoeconomic potential for CO2 storage in basalts. The HERO CarbonSAFE project will assess feasibility of developing a commercial-scale (50+ million metric tons of CO2) geological storage complex within the Columbia River Basalt Group (CRBG), a layered continental flood basalt complex that underlies Calpine’s natural gas-fired Hermiston Power Project (HPP) in Hermiston, OR (Figure 1). Under this 2-year CarbonSAFE Phase II project, the HERO team will conduct a data acquisition campaign that includes drilling a stratigraphic well to a total depth of ~1,500 m into the thick layered basalts proximal to HPP. A comprehensive well logging and hydrologic testing program will be augmented with new core collected from flow zones and sealing units, and comprehensive laboratory testing to help refine the kinetic rates of mineralization. The newly acquired information will be integrated with existing data from regional wells to correlate basalt injection zone properties to develop storage hub/commercial-scale models. Using these models, the project team will evaluate injection scenarios to define the technical and economic potential for storing a minimum of 50 million metric tons of CO2 over a 30-year period, along with a robust sensitivity analysis on key parameters governing reservoir viability for sustainable injection over a commercial project lifetime. Specific technical objectives of HERO are: (1) assessing the reservoir response of a series of stacked layered reservoir flowtop sequences occurring in this area of the CRBG to commercial-scale injection volumes; (2) extending prior efforts by the project team to characterize the deep layered basalts encountered in regional studies, to leverage prior investments by U.S. Department of Energy’s (DOE) Carbon Storage program; (3) leveraging DOE’s mineralization characterization efforts to advance model parametrization for commercial scale injection of CO2 in basalts; (4) conducting risk assessments associated with scaling up to commercial storage hub injection goals, while validating DOE’s National Risk Assessment Partnership (NRAP) tools, to identify potential constraints that would prevent the CRBG from serving as a commercial-scale storage complex; (5) developing mitigation plans to address identified risks; (6) developing a commercial-scale injection and monitoring, verification and accounting (MVA) strategy; (7) utilizing computational models to define and minimize, if possible, the Area of Review (AoR) under Class VI regulations; and (8) developing a robust CO2 management strategy for CRBG that also considers a regional source/sink approach that is responsive to stakeholder needs and industrial demand. Specific institutional objectives are: (1) identifying and developing plans to mitigate the nontechnical challenges associated with the build-out of a commercial-scale storage complex within the CRBG with integrated CO2 sources; (2) implementing the community outreach plan; (3) conducting regulatory research, including a survey of issues related to pore space ownership, MVA and long-term assurance of mineralization-based storage, to support an eventual application for a UIC Class VI permit; (4) advancing the project’s plan for CO2 liability management; and (5) continuing to refine and update the project’s economic model. The final objective is the preparation of a comprehensive Site Characterization Plan that draws upon the technical and institutional feasibility assessments to prepare the project for future commercialization efforts.

58 GEOSCIENCES↗
DOE OSTI2024

Field Validation of MVA Technology for Offshore CCS: Novel Ultra-High-Resolution 3D Marine Seismic Technology (P-Cable) (Final Report)

The objectives of the proposed study were to deploy and validate a specific monitoring technology, high-resolution 3D marine seismic (HR3D), appropriate for large-demonstration and commercial-scale offshore CCS sites. The project accomplished successful acquisition two HR3D seismic surveys. The first HR3D dataset was over the offshore injection site of the Tomakomai, Japan integrated pilot CCS project, which at the time of survey acquisition was actively injecting CO 2 . The first survey also represented a successful international collaboration between the DOE NETL program and Japan’s national CCS program and was the first successful acquisition and use of HR3D over an active CO 2 injection site (Meckel, Feng et al. 2019). The Tomakomai HR3D survey successfully tested a novel 4-streamer HR3D system array in which, for the first time, no cross-cable (aka “P-Cable”) was utilized and only four GeoEel streamers were used instead of the standard 12-streamer configuration. Consequently, this was not, strictly speaking, a deployment of the “P-Cable” system of (Planke and Berndt 2004) but rather a modified version, thereof, and it is the first known demonstration of the modified system configuration. One very positive outcome from the Japanese collaboration earlier in the project was the ability to learn from the Japanese how they used tail buoys with GPS to determine the position of the seismic source and receivers in time and space. Based on that experience, GCCC designed and built six GPS receivers that could be used to position the streamer receivers and the seismic source via tail buoys. A fundamental advance that was made on the original design, was the ability to directly power the tail buoy GPS units and transfer data through the streamers (i.e., vs. the batteries used at Tomakomai). The bulkiness of the GPS batteries caused drag and episodic surging of the buoys, which affected data quality by lifting up the tail end of the streamers so the receivers were not at the same depth. The units were tested onshore for accuracy and functionality, and the design was subsequently and successfully tested in marine acquisition mode during the SLP survey acquisition. The marine acquisition test and survey satisfied Subtasks 2.2.2, Novel Positioning Technology Selection and Subtask 2.2.3, Novel Positioning Technology Deployment. Results of the novel positioning technology selection (Subtask 2.2.2) were considered successful and will be incorporated in future HR3D seismic acquisition projects to reduce costs, improve deployment safety at sea, and integrate both seismic and data recording via a single data transfer through the streamers to the recording system. The project also established a permitting process through NETL NEPA compliance, which included an Environmental Assessment in a marine setting and is required for conducting these types of surveys using Federal funding. The permitting process charted a “boilerplate,” which can allow future surveys related to other funded projects to move forward more expeditiously. Future improvements that could be considered are more robust seals on the GPS module and stronger materials (especially joints) on tail buoy fabrication. These would increase fixed costs, but would be advisable and probably more economic long-term if multiple HR3D surveys are planned. Project Accomplishments include: • Pre-survey Sensitivity Study • Marine geochemistry methods and data analysis • Successful HR3D seismic dataset acquired @ Tomakomai active CO 2 injection marine site • Developed advanced seismic processing techniques • No NRMS anomalies detected in overburden; Demonstration of containment • Repeatability study • Second survey collected @ San Luis Pass, TX • 4D application using positioning techniques developed in the project for monitoring were successful

3D seismic GPS positioning↗
DOE OSTI2024

Mini-Canister Radiolysis Testing of ASNF Materials and Surrogates

An experimental irradiation campaign to investigate radiolysis behavior of ASNF was conducted using in situ gas monitoring of small, sealed stainless-steel vessels (mini-canisters) containing aluminum samples with adherent (oxy)hydroxide films under helium backfill. The samples were irradiated with gamma radiation from a Co-60 irradiator. The samples tested included aluminum plate assemblies with lab-grown (oxy)hydroxides as surrogates for fuel as well as an end cropping from an actual ASNF assembly retrieved from long-term wet storage. These experiments enabled investigation of the impacts of various fuel drying approaches on the radiolytic generation rate and measurement of the H 2 yield associated with a reactor exposed sample with reactor-formed (oxy)hydroxide. The resulting data can be incorporated into model development for ASNF in dry storage. This report presents the cumulative results from four surrogate assemblies tested after application of different preparation (drying) conditions as well as the ASNF cropping; some post-irradiation testing was included. The mini-canister results are compared to data from related experimental campaigns that also tested the impact of drying conditions using samples irradiated in glass ampoules and discusses implications of the combined data

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Results from an Aeromagnetic Survey to Detect Steel-Cased Wells at a Marcellus Shale Well Site in Washington County, Pennsylvania

Pennsylvania has a 150-year history of oil and gas production—the longest of any state—and this enduring activity has resulted in the drilling of more than 300,000 recorded wells. However, unknown wells likely exist because innumerable wells were drilled during Pennsylvania’s intense early oil and gas history when incomplete records were kept of well locations. There is concern that early wells are likely to be ineffectively sealed because there were no laws that required plugging when the wells were abandoned. Today, many undocumented and unplugged wells are thought to be in areas of emerging shale gas and shale oil development where open wellbores can provide a pathway for undesired upward migration of fluids and gas from hydraulically fractured reservoirs. Due to this concern, Pennsylvania regulators have asked operators to locate orphaned and abandoned wells within a 1,000-ft buffer of proposed new wells. The objective of this report is to demonstrate that high-resolution aeromagnetic surveys, historic air photos, and Light Detection and Ranging (LiDAR) imagery can be rapid and effective methods to reconnoiter large, forested areas of moderate terrain for the presence of abandoned wells. These well-finding methods were evaluated at a proposed Marcellus Shale gas drilling site in Washington County, Pennsylvania, where the methods collectively located 18 confirmed wells: 15 wells were identified from aeromagnetic surveys, two wells were identified from inspection of historical air photos, and one well was identified by evaluation of state-wide LiDAR imagery. Only six wells were previously known, and their locations, as recorded in Pennsylvania’s statewide oil and gas wells database (PA/IRIS/WIS), were often too inaccurate for the wells to be found in the dense underbrush. Twelve wells identified in this study were abandoned, unmarked, and undocumented. Aeromagnetic surveys locate wells by detecting the unique magnetic signature of vertical, steel well casing, which is depicted on magnetic maps as a “bull’s eye” type anomaly that is centered directly over the well. However, when wells were drilled and found to be sub-economic, their casing was sometimes pulled and salvaged for reuse. Such wellbores provide no magnetic response and go undetected if all casing was removed. Oftentimes attempts to retrieve well casing were not 100% successful. For example, historical records for one well in the study area indicate that the well was completed in 1902 as a dry hole and that, to the extent possible, the casing was pulled for reuse. However, a section of 10-in. diameter steel casing was not recovered and remains at an unknown depth in the wellbore. This well was easily detected by the aeromagnetic survey although only deep casing remained in the well. To mitigate for the likelihood that wellbores exist where most or all casing has been removed, this study augmented aeromagnetic data with historic air photos and digital terrain models generated from LiDAR datasets—both databases are publicly available at no cost for areas within Pennsylvania. These complementary methods located three wells where the aeromagnetic anomaly, although present, was subtle and overlooked. Together, these methods determined accurate locations for six known wells within the study area and located 12 previously unknown wells. Although it is not certain that these methods successfully located all wells in the study area, the application of these methods does represent a significant improvement over relying on existing databases for well locations. For the Appendix to the report, see: https://www.netl.doe.gov/energy-analysis/details?id=b46c417a-7c9e-4d25-b810-e6248b0217f4</p>

04 OIL SHALES AND TAR SANDS↗
DOE OSTI2024

Flow Sensor Test Article (F-STAr) - Water Testing and Commissioning Report for FY2024

Argonne National Laboratory’s Mechanism Engineering Test Loop (METL) facility is developing new experimental testing capabilities with the Flow Sensor Test Article (F-STAr). F-STAr’s mission is to provide high flowrate, sodium submersible testing capabilities to support the development of sodium cooled nuclear fission reactors. Figure 1 shows a model of F-STAr (left) and a photo of the partially assembled test article (right) with several of the main components labeled. The system currently includes a large pump with desired flowrates of up to 100 GPM; an immersion heater with a maximum power of 5 kW; an immersion cooler with an estimated maximum cooling power of 2 kW; and an experimental test section to support sub-test articles. Initially, F-STAr will be setup for testing flow sensors, specifically Eddy Current Flow Sensors (ECFS). However, the system can be reconfigured to support a wide range of testing needs. For example, F-STAr could be setup to complete testing of hydraulic components, heat exchangers, hydrodynamic bearings, seals, and more. This report will provide an update on the development of F-STAr with a focus on the water testing and commissioning activities during Fiscal Year 2024 (FY24). First, the report will focus on describing the pump development. Specifically, updates will be provided on troubleshooting the pump’s excessive vibrational issues. In addition to updates on the pump, pressure-flowrate performance testing in water will be described. Furthermore, updates will be provided on a pump shaft bushing development as well as rigging procedures. Future work and paths forward for F-STAr will be described. Finally, a short summary on the ECFS development will be described at the end of the report.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
DOE OSTI2024

DECOVALEX-2023: Task B Final Report

In all repository concepts for the geological disposal of radioactive waste, an engineered barrier system (EBS) is used to encapsulate the waste canister, or, to act as borehole or gallery seals. These systems are often based on bentonite clays due to their low permeability and high swelling capacity enabling the closure of engineering voids. However, in all repository concepts gases will be generated through the corrosion of metallic materials (under anoxic conditions), the radioactive decay of waste and the radiolysis of water. Thus, understanding the processes and mechanisms controlling the advective movement of gas (as a discrete phase) in clay-based materials is a key aspect when assessing the impact of gas flow in a repository safety case.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

DECOVALEX-2023: Task F2 Salt Final Report

The subject of Task F of DECOVALEX-2023 concerns performance assessment modelling of radioactive waste disposal in deep mined repositories. The primary objectives of Task F are to build confidence in the models, methods, and software used for performance assessment (PA) of deep geologic nuclear waste repositories, and/or to bring to the fore additional research and development needed to improve PA methodologies. In Task F2- (salt), these objectives have been accomplished through staged development and comparison of the models and methods used by participating teams in their PA frameworks. Coupled-process submodels and deterministic simulations of the entire PA model for a reference scenario for waste disposal in domal salt have been conducted. The task specification has been updated continuously since the initiation of the project to reflect the staged development of the conceptual repository model and performance metrics. Thermal, hydrological, mechanical, and chemical properties of individual components of the engineered and natural system were chosen for relevance by participating teams. The salt reference case system was characterized using data and measurements collected at relevant underground research laboratories (URLs), field sites, and simulation results from teams with specialized modelling capability. Participating teams made a wide range of model assumptions from compartmentalized networks to full 3D models of the salt formation. No single contributed model includes full-fidelity representation of all the features, events, and processes (FEPs) detailed in the task specification, but almost all features and processes are represented in at least one model. Despite differences in the modelling strategies developed by participating teams, all models indicate that salt compaction and radionuclide diffusion are key processes in the repository, and for the FEPs and model scenario considered, little of the disposed radionuclides will migrate beyond the repository seal over the 100,000 year simulations. In general, the model output quantities have the largest differences over the short term and near the waste. The models tend to be more similar further from waste and at later time. Disparities between the models are believed to be due to differing simplifications from the task specification, some of which are chosen simplifications to reduce complexity, and some are restrictions imposed by the modelling tools. A second round of this task has been accepted for DECOVALEX-2027 in conjunction with Task F1 on crystalline PA modelling. The future round includes waste package heating, improved modelling of salt creep closure, additional comparisons of coupled-process sub-models, and the impact of repository engineering design on radionuclide migration in the repository. Participants will also propose and finalize a set of uncertain inputs for the reference case simulations, propagate these uncertainties in a set of realizations, and conduct sensitivity analyses on the simulation results.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2024

Managing Subsurface Pressure Buildup and Interference in Commercial-Scale CO 2 Storage Project with Proximal Injection Wells

Large-scale decarbonization using carbon capture and storage (CCS) is likely to involve many commercial-scale CO 2 storage projects located in close proximity to each other. This close proximity raises concerns over pressure interference among the storage projects. Pressure interference between injection and storage efforts can reduce the practicable CO 2 storage resource and force wells to inject CO 2 at a lower rate to avoid the fracture pressure thresholds per United States Environmental Protection Agency (EPA) Class VI well regulations to preserve injection and confining zone integrity and potentially mitigate against inducing seismic activity. These analyses employ numerical full-physics reservoir modeling to evaluate how pressure buildup fronts and CO 2 plumes evolve under commercial-scale injection volumes of CO 2 in which multiple storage sites located in close proximity occur in tandem. The simulation models mimic injection at pseudo basin-scale and assume homogeneous saline formation(s) as storage targets with a pair of upper and lower homogeneous seal layer/s. These analyses specifically investigate the efficacy of two basin-wide reservoir pressure management strategies in addressing the technical challenges associated with pressure buildup and CO 2 plume commingling. The strategies explored include: 1) enlarging the area of injection well spacing (WS) and 2) storing CO 2 in a stacked sequence (SSS) of saline formations compared to a single formation. The storage and confining zones properties assumed were held common across the scenarios, unless specified otherwise. Analyses results show that after injecting 4 million tons per year for 30 years using 4 separate wells (each injecting 1 million metric tons per year), the radius of CO 2 plume extends to a mere 3 km or less from injection wells. Meanwhile, the radius of pressure buildup ranges on the order of tens to a few hundreds of kilometers, depending on the magnitude of pressure buildup threshold that one would use to define the front. CO 2 plume commingling from different injection wells appears to occur 50 years post-injection, especially under scenarios with narrowly spaced (i.e., < 5 km apart) injection well locations. Findings from sensitivity cases on the well spacing suggest that storage formations modeled would require different well spacing to avoid fracture pressure thresholds. For instance, modeled storage formations with high fracture gradients (i.e., 0.8 psi/ft) would need less than 5–km well spacing, whereas those with lower fracture gradients (i.e., 0.7 psi/ft) would need approximately 20–km well spacing, based on assumed modeling parameters. Under stacked injection, the pressure challenges (described above) still exist but are more alleviated due to distributing the same injection volume across more available reservoir volume. These analyses demonstrate that stacked-sequence storage can effectively address the challenges, while still providing the same target CO 2 storage volumes and allowing a large number of storage projects to be deployed in the same basin by better utilizing the available storage resource across different reservoir depths. Among cases modeled, the resulting pressure buildup front is most suppressed when each storage project distributes injection volumes over several wells, each of which injects a portion of the total CO 2 across the stacked sequence. This strategy results in the smallest CO 2 aerial footprint amongst scenarios evaluated but also shows the largest reduction in the pressure buildup at the top of perforation at the injection wells (upwards of approximately 42 percent compared to the commercial-scale single-formation storage), the result of which is crucial to maintain caprock integrity. The findings presented by this research draw attention to the importance of greater coordination among storage operators and regulatory stakeholders to foster the upscaling and deployment of CCS. These analyses provide insights into required decision-making when considering multi-project deployment in a shared basin. Because these analyses evaluate a very specific geologic situation, they bear further investigations across other geologic situations.

42 ENGINEERING↗
DOE OSTI2024

TCF - Sustainable Well Cement for Geothermal, Thermal Recovery, and Carbon Storage wells

Primary cementing is the most important operation performed on a subterranean well. Cement, placed in the annulus between the casing and the formations, serves as a hydraulic seal preventing fluids and gas migrations, protecting steel casing from corrosion, and supporting the well structure. Poor cementing jobs can be directly responsible for wells not reaching their full capacity, casing corrosion, compromised well integrity and, in the worst-case scenarios, well collapse. Geothermal, thermal recovery, and carbon storage wells offer environments that are especially difficult for cements to survive while the required lifespan of these wells can be years. In these wells currently used cements cannot provide durable well integrity, and new solutions are necessary. The necessity of stabilizing the electric grid, increasing its flexibility, and providing energy on demand will further expand the market of durable cement solutions for applications in high-temperature underground reservoir thermal energy storage wells (HT RTES). The design challenges of special cement systems for such wells originate from chemistry limitations of currently used well cements, aggressive environments, temperature and repeated shock conditions associated with them, and very weak formations that are not uncommon in these wells. During the last 70 years the most common systems for thermal-well construction have been Ordinary Portland Cement (OPC) (absolute majority of the wells), silica-lime system, and high aluminum cement-containing formulations. The major issues of calcium-silicate hydrates, that form during the hydration of OPC resulting in hardened material, are their poor chemical resistance to acids due to the calcium interactions with acid anions followed by its eventual dissolution, even in mild acids, such as carbonic acid from CO 2 dissolution, and inadequate bonding to the steel causing serious casing corrosion problems (Sugama & Pyatina, 2019). Performance of OPC-based cement may be significantly improved with organic additives; however, those are limited by their temperature stability. An alternative to calcium-silicate cement was developed by BNL and commercialized by Halliburton as ThermaLock TM cement. Calcium-aluminate-phosphate-based chemistry of the material allowed overcoming acid-resistance problems of OPC, especially in CO 2 -rich geothermal environments. In 2012-2015, building upon this experience, BNL developed Thermal Shock Resistant Cement (TSRC) with the support of Geothermal Technology Office (GTO) of DOE. TSRC has high-temperature stable chemistry, superior properties of cement-metal casing bond and corrosion protection (4-times better than currently used OPC-based formulation), significantly outperforms common well-cements in thermal-shock tests, has self-healing properties, and like ThermaLock TM is CO 2 resistant incorporating carbonate ions into stable hydrates (Gill et al., 2012).

15 GEOTHERMAL ENERGY↗
DOE OSTI2024

Effect of Anoxic Iron Corrosion on WIPP Brine Geochemistry FY23 Final Report (U)

A 280-day study was completed to evaluate the effect of zero-valent iron (Fe 0 ) on the Waste Isolation Pilot Plant (WIPP) brine geochemistry under anticipated reducing conditions. Hydrogen (H 2 ) gas is expected to be present in the repository after closure due to the anoxic corrosion of a vast quantity of iron contained in the waste forms disposed at WIPP; therefore, a background argon atmosphere containing H 2 was chosen for this study. WIPP groundwater brine pH and E h will impact the mobility and fate of plutonium within the repository. Modeling and laboratory results for Castile WIPP brine indicate that equilibrium fa values relative to the standard hydrogen electrode (SHE) are 40 mV more reducing (i.e., more negative) than those for Salado WIPP brine (-480 mV vs. -440 mV, respectively) because of the higher pH of the Castile brine (pH 9 .3 for Castile vs. pH 8.8 for Salado). The E h and pH data were corrected for the effects of high ionic strength. The experimental results for both brines are consistent with thermodynamic predictions using OLI Systems' Mixed Solvent Electrolyte chemical equilibrium model. The measured and corrected pH and E h data from this study are provided in Table ES-I and Table ES-2, respectively. The experimental study, with four test conditions in triplicate, was performed in a dual glovebox with a nominally 3 vol.% H 2 in argon atmosphere (target H 2 range: 3 ± I vol.%). Simulants containing MgO only ( experimental control) and MgO+Fe 0 (WIPP base case) were prepared for both the Salado and Castile brines. MgO was included in all simulants to account for the use of bulk magnesium oxide in the WIPP repository. Fe 0 was included in some simulants to incorporate the effects of the anoxic corrosion of iron and in-situ hydrogen generation in the study. The brine compositions were developed by Sandia National Laboratory (SNL; Xiong, 2008) and have been used in previous WIPP evaluations. The test method (agitation, etc.) is partially based on ASTM D3987-12. Twelve rounds of periodic measurements of pH and E h were performed over the course of the study. Chemical analysis results for liquids and solids (ICP-MS, ICP-ES, IC Anion, TIC, SEM-EDX) are consistent with the pH, E h , and thermodynamic modeling results. This study included the following conditions that deviate from anticipated post-closure conditions following brine intrusion, but were selected to facilitate bench-scale testing to validate modeling of pH and E h for the post-closure WIP P repository: an anoxic glove box atmosphere containing ≤ 4 vol. % H 2 vs. substantially higher H 2 gas concentrations assumed in the WIPP Performance Assessment (PA); a significantly higher liquid-to-solid test ratio compared to the much lower phase ratio anticipated in the WIP P repository; agitation of the simulant bottles to maximize mass transfer; and finally the use of Fe 0 reagents having a much greater surface area than expected in the WIP P repository. Non-representative conditions were chosen for various reasons such as: to provide bounding conservative results, to provide a margin of safety for testing, or to facilitate simulant sub-sampling and analysis. In a parallel effort, aqueous electrolyte thermodynamic models were developed for the synthetic Salado and Castile brines to inform the experimental design, facilitate laboratory data interpretation, and allow extension of evaluations beyond the parameters tested. Thermodynamic modeling simulations including the MgO and Fe 0 additives that are directly relevant to the experimental measurements (e.g., pH calibration curve, ORP corrections) are included in this report. The measured fa of the simulants was close to the OLI model predictions for both brines and was largely controlled by the background H 2 partial pressure in the vapor phase as well as H 2 generated in situ in the aqueous phase by the Fe 0 corrosion. The H 2 gas-phase concentration tested and thermodynamically evaluated was much lower than is assumed in the WIPP PA; however, H 2 (g) concentrations significantly below this level are still predicted to result in very reducing conditions. In conclusion: • The experimental results are consistent with thermodynamic model predictions for fa, pH, and the effects of high ionic strength. • Evidence to date suggests that the H2 concentration in the glovebox atmosphere ultimately determined the final E h values of the simulants and resulted in highly reducing conditions. As a result, little difference was observed between the control simulants containing only MgO and the WIPP base-case simulants that contained MgO and Fe 0 . • This test methodology is recommended for future studies evaluating WIPP repository conditions. The methodology includes: (1) background H 2 in argon with agitation ( or could alternatively include in-situ-generated H 2 in sealed bottles); (2) carefully measured and corrected ORP data ( with much effort focused on allowing the probes to fully stabilize); and (3) ionic-strength-corrected pH data. Other best practices, such as simulant sparging/handling, ORP probe replacement, etc., should also be considered. • The coupling of experimental studies and thermodynamic modeling is also highly recommended because these methods inform and direct one another leading to greater confidence in and understanding of the results.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗
DOE OSTI2025

Microscopic Measurement: Need for Nuclear Material Sample Specimen Characterization Capability

The Surveillance, Fabrication, and Off-Site Operations team at Lawrence Livermore National Laboratory is beginning an update to the nuclear material machining lab in Superblock. Plutonium and other nuclear materials tend to accelerate the aging process for equipment and machines that would otherwise be maintainable for long lives. They have their lifespans shortened from deteriorated seals, embrittled polymer components, accelerated corrosion, and damage to electronics from exposure to radioactive materials. The cost of installation of equipment into a glove box (GB) tends to outstrip the cost of the equipment itself. Due to the magnification of cost, the historical approach to equipment installs has been to purchase and install the highest-quality and most robust equipment available to maximize time between failures and updates. To make room for the installation of a new lathe, the inspection GB is being moved to a different location within the machining lab. As part of the overall effort, the equipment within the inspection GB is being revisited. Current measurement capabilities are antiquated and starting to become problematic due to age. Advances in metrology are sought for more comprehensive characterization of scientific samples. This document aims to identify several options for the replacement of current measurement equipment and identify a system for purchase and eventual installation. The intention is not to select the cheapest system, but rather to identify a system that best meets the needs of both the operators and principal investigators (PI). Following the convention of the SYSM-5620 Design Thinking and System Engineering, it was determined that a laser confocal measurement system from Keyence is the most suitable option for our programmatic need. Form factor, capability, and maintainability were considered. Along with stakeholder input, to ensure the best decision for the Nuclear Material Technology Program.

36 MATERIALS SCIENCE↗
DOE OSTI2024

Cements and a Modeling Tool to Calculate their Viability under Various Exploitation Conditions of HT RTES Systems

Primary cementing is the most important operation performed on a subterranean reservoir. Cement, placed in the annulus between the casing and the formations serves as a hydraulic seal preventing fluids and gas migrations, protecting steel casing from corrosion and supporting the well structure. Poor cementing jobs can be directly responsible for wells not reaching their full capacity, casing corrosion, compromised well integrity and, in the worst-case scenarios, well collapse.

15 GEOTHERMAL ENERGY↗
DOE OSTI2021

Management of the Three Mile Island, Unit 2, Accident Corium and Severely Damaged Fuel Debris

The Three Mile Island, Unit Two (TMI-2) pressurized water reactor core melted down in 1979 due to an untimely combination of maintenance problems that led to a loss of feedwater, followed by a series of operational misunderstandings and errors. The melted core recovery process required development of a wide array of tools. After approximately three years of water management and other cleanup actions, the first views of the core revealed a much higher degree of damage than previously expected. Approximately 62 metric tons of the core had melted, leaving only 42 of the 177 fuel assemblies standing with a majority of rods intact. The core to be recovered was composed of loose debris and a solidified mass of formerly molten fuel. Robotic tools that had been designed for the task were of limited effectiveness due to the range of material types and phases. Over a period of several years, the central melt was broken up, primarily by use of a core-boring drill originally designed to acquire samples through the depth of the debris field. The broken pieces were loaded into specially designed debris canisters by use of long-handled pick-and-place tools and suctioned into baffled knockout canisters using an airlift vacuum system. A remotely operable underwater plasma arc torch was developed for removal of the lower core support structure to be able to retrieve the fuel pieces and secondary melt that had accumulated on the bottom reactor vessel head. Canister design played a central role in defining the initial retrieval process and later affected transportation, interim wet and its current interim dry storage. Due to concerns about the potential for radiolysis of residual water in the debris and other canister material, the canisters were fitted with hydrogen recombiner catalyst units to prevent a buildup of flammable gas and potential pressurization. To confirm the effectiveness of the recombiners during shipping, eight dewatered canisters were kept sealed for up to 205 days with periodic sampling of the headspace gas. The highest hydrogen value (9 vol%) was observed in a canister held for 147 days while the longest stored canister resulted in a 5% hydrogen concentration. The oxygen concentration never exceeded 0.5 %, and the primary backfill was >80% argon, meaning there was no flammability risk. Radiolytic hydrogen was also observed in wet pool storage, where the vented canisters discharged a portion of the water backfill as a result of gas production. The 344 canisters (268 fuel debris, 62 filter, and 12 knockout type) were dewatered, loaded in groups of seven into a double barrier shipping cask, and transported to the U.S. Department of Energy site in Idaho for 10 years of pool storage.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗
DOE OSTI2025

High-Resolution Computed Tomography Dataset of Mount Simon Sandstone

The Illinois Basin is a critical structure for subsurface energy related activities and their implementation in the United States. The Mount Simon Sandstone has been identified as a storage target for permanent and transient storage of fluids in the basin. Known for its exceptional thickness, depth, porosity, and sealing properties of overlying formations, this saline reservoir is crucial for long-term subsurface energy efforts. We present an extensive Computed Tomography (CT) dataset on a high porosity and permeability zone in the lower Mount Simon Sandstone available on the Energy Data eXchange® (EDX). This publicly accessible database comprises over 500 GB of high-resolution CT scans of six core samples, with resolutions ranging from 14.8 µm to 0.7 µm per pixel. The scans include both dry sandstone samples and those saturated with multiple fluids, allowing for comparative analyses across different conditions and resolutions. Coarser scans capture the bedding structure of the sandstone, while finer resolutions reveal detailed pore infill and throat characteristics. Metadata on location, depth, and saturation state enhance usability, enabling quick identification and cross-sample comparisons. By providing a robust resource for research and collaboration, the database contributes to domestic energy advancement by supporting continued progress in the use of the subsurface for energy solutions.

characterization↗
DOE OSTI2024

Novel Full-Ceramic Multi-Tubular Membrane Systems for Pre-Combustion CO2 Capture with Simultaneous H2 Production: Fabrication, Performance Testing, and 3D CFD Modeling

Inorganic membranes show promise for application in pre-combustion CO2 capture with simultaneous H2 production. State-of-the-art systems for use under high temperature and pressure conditions consist of multiple membrane tube bundles prepared in a "candle-filter" configuration, in which the membrane tubes are open at one end and sealed at the other. This configuration is used for practical reasons, specifically the need to minimize potential problems due to thermal expansion mismatch, at high temperatures, between the ceramic tube bundle and the steel housing. The primary technical problem with the candle-filter configuration for use in commercial-scale installations is the inability to purge the permeate side (typically the tube side), a feature that is crucial for high H2 recovery. In this study, we fabricated dual-end open, commercial-size ceramic multiple-tube bundles made of zeolite, palladium (Pd), and carbon molecular sieve (CMS) membranes that enable permeate-side (tube-side) purge for gas separation applications. Experimental gas separation data with these membrane bundles under harsh operating conditions (temperatures up to 350 and pressures up to 800 psig), to be presented at the meeting, manifest excellent performance. Parallel to the membrane bundle construction and testing efforts, we have also developed a detailed 3D CFD modeling package using COMSOL Multiphysics software to gain more insight into the effect on the H2 purity and recovery of the detailed geometry of the multi-tubular membrane system, including the number of tubes used, their dimensions, and placement in the bundle, as well as the number, type, and positioning of internal baffles and other flow-enhancement accessories. The CFD package is validated with experimental data from different systems (1-tube, 3-tube, and 19-tube bundles), and shows high accuracy in predicting the experimental results (<5 % error in all cases). The results of our study show that the detailed internal geometry of these multi-tubular membrane systems has a considerable impact on the performance of the system as the flow maldistribution within the shell-side can substantially decrease (>40%) the H2 recovery.

20 FOSSIL-FUELED POWER PLANTS↗
DOE OSTI2022

Salt Sampling FY21 Technical Report

The goal of the salt sampling program at Argonne is to develop and deploy automated molten salt sampling approaches to enable high-precision in-process salt sample analysis to improve the timeliness of sampling-based accountancy measurements. Tools currently under development in support of this goal include (1) a modular vacuum sampler with an accompanying sample handling method for coupling vacuum sampling with high-precision at-line sample analysis, (2) a pneumatic sample generator that enables high-throughput sample analysis to improve the precision of existing analytical techniques, and (3) a windowless flow cell to enable on-line optical analysis of molten salt in a sampling loop. Compared to point sampling approaches (i.e., dip probes), vacuum sampling systems and on-line sampling loops facilitate access to a larger cross-section of a process fluid. This is known to improve the characterization of the process fluid by producing more representative samples and by enabling the analysis of a larger cross section of the fluid. A vacuum sampling approach for molten salts eliminates the risk of dross contamination of samples and avoids the use of moving parts in the salt. In FY21, two methods for integrating a vacuum sampler with a pneumatic sample generator were tested. These included direct fluidic coupling and coupling using a solid salt transfer mechanism. Solid salt transfer was ultimately selected over fluidic coupling, primarily to enable the transport of samples over longer distances to support automated at-line integration with high-precision techniques (such as microcalorimetry) that cannot withstand the extreme conditions near an electrorefining process. To facilitate rapid solid salt coupling, new mechanisms were developed for rapidly charging and discharging salt sample tubes at the vacuum sampler and pneumatic sample generator, respectively. While the charging mechanism will be deployed in FY22, the tube transfer method and discharge mechanism were tested in FY21. These were deployed at one of Argonne’s engineering-scale electrorefiners to implement at-line high-throughput pneumatic micro-sample generation capabilities. The method was used to generate precise uranium- and lanthanide-bearing electrorefiner micro-samples with the specific dimensions requested by researchers at Los Alamos National Laboratory for use in testing their novel microcalorimeter x-ray techniques. The solid salt transfer mechanism proved not only to be an effective means of integrating the precision sample generator with vacuum sampling, but also improved the performance of the sampler generator. Because the modular sampling approach described here eliminates the need for new high-radiation sample handling capabilities, salt-wetted seals, salt-wetted moving parts, and heated transfer lines outside the electrorefiner, it will address most of the remaining technical challenges for the at-line deployment of high-precision analytical techniques. This will enable significant reductions in the time delay for sampling-based accountancy measurements by eliminating the need for manual off-line sample processing and analysis. On-line optical analysis of molten salt in a sampling loop would provide complementary information to at-line and in-situ techniques. In FY21, an open-aperture molten salt gravity flow cell with windowless optical access to flowing salt was successfully demonstrated. Future work should include the refinement and performance testing of the on-line and at-line sampling tools, integration of additional analysis techniques, stakeholder outreach and collaboration, evaluation of the integrated methods, and analyses to determine how the various tools might fit into an integrated safeguards monitoring system of unattended near real time monitoring tools.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗