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DOE OSTI2022

Progress on Pu-238 Production at Idaho National Laboratory From March 2021 to February 2022

Idaho National Laboratory has completed irradiation of Np-237 targets in the Advanced Test Reactor’s (ATR) South Flux Trap (SFT) and I-7 positions. INL also progressed qualification of new ATR Gen 1 Np-237 targets for the North East Flux Trap (NEFT), inner A, and H positions. This paper gives an overview of operational and technical activities from March 2021 to February 2022.

07 ISOTOPE AND RADIATION SOURCES↗

DOE OSTI2024

Development of Magnesium Oxysulfate Formulation for SRPPF Aqueous Recovery Liquid Solidification

The liquid effluent from the Savannah River Plutonium Processing Facility (SRPPF) Aqueous Recovery Processes will be solidified into a stable form that is acceptable by Waste Isolation Pilot Plant (WIPP) for disposal. The current Aqueous Recovery flow sheet proposes to solidify the liquid effluent using a grout formula that was developed and tested for the former Waste Solidification Building process. This Portland cement based mixture results in a high pH (~13) leachate from the solidified waste form which is not acceptable to WIPP in the large quantities expected from production at SRPPF. Various cementitious materials were previously evaluated as alternative grout formulations to Portland cement and a MgO-based mix was identified as a promising alternative. A magnesium oxysulfate (MOS) cement formulation comprised of reactive magnesium oxide (MgO), anhydrous magnesium sulfate (MgSO 4 ), and sand, as a non-reactive heat sink provided good mixability, similar density to the original Portland-cement based mix, and a leachate pH of 9.4, within the assumed WIPP brine pH range. However, the MOS formulation exhibited an appreciable amount of heat generation, which resulted in premature setting of a large-scale test.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

Automated Laboratory Kilogram-Scale Graphene Production from Coal

The flash Joule heating (FJH) method converts many carbon feedstocks into graphene in milliseconds to seconds using an electrical pulse. This opens an opportunity for processing low or negative value resources, such as coal and plastic waste, into high value graphene. Here, in this work, a lab-scale automation FJH system that allows the synthesis of 1.1 kg of turbostratic flash graphene from coal-based metallurgical coke (MC) in 1.5 h is demonstrated. The process is based on the automated conversion of 5.7 g of MC per batch using an electrical pulse width modulation system to conduct the bottom-up upcycle of MC into flash graphene. This study then compare this method to two other scalable graphene synthesis techniques by both a life cycle assessment and a technoeconomic assessment.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2020

Effects of He Ion Irradiation in Simple Borosilicate Glasses for HLW Immobilisation - 20324

High-level radioactive waste (HLW) consists of fission products and minor actinides. Borosilicate glass is the host material of choice in most countries to safely immobilize HLW, followed by eventual geological disposal. HLW glasses will experience both self-heating and self-irradiation effects due to the decay of fission products and minor actinides present therein. During the first 500 years of geological disposal, beta-gamma decay will be the main source of radiation due to short half-lives of fission products, as compared to very long-lived actinides which will be responsible for irradiation over much longer timescales. High-energy alpha particles and alpha recoil nuclei can potentially have significant impact (stored energy, volume change, accumulated dose, chemical durability) on the performance of the wasteform over longer timescales. Thus, to ensure safe and economic disposal over geological periods (10{sup 4} - 10{sup 6} years), the assessment of performance and properties in terms of radiation effects becomes indispensable. This work aims to simulate the effects of alpha decay in radioactive waste glasses. Two international glasses, namely UK 'MW' lithium-sodium borosilicate and Indian sodium-barium borosilicate, which are being used as HLW immobilization matrices by the UK and India respectively, were prepared by a melt-quench method and annealed below their glass transition temperatures. Both glasses were irradiated with 650 KeV He{sup 2+} ions with doses ranging from 10{sup 15} to 10{sup 17} ions/cm{sup 2}. Structural analysis was carried out using electron paramagnetic resonance (EPR) and Raman spectroscopies. First derivative continuous wave EPR spectra were recorded for all pristine and irradiated glass monoliths at room temperature using an X-band (frequency 9.6 GHz) EPR Bruker spectrometer. Results from EPR analyses showed the formation of irradiation induced paramagnetic centers at g ∼ 2.00 in all irradiated glasses. Raman spectra of pristine and irradiated samples were acquired, and showed notable changes in glass structure post-irradiation, with the emergence of a broad Raman band at 1560 cm{sup -1} upon irradiation with high fluences. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2021

Removable smart sequestration coatings for hazardous metals

Materials are disclosed for the safe sequestration and removal of hazardous contaminants from a surface. The materials can be sprayed, rolled, painted, brushed or dip coated onto any surface and allowed to dry and/or cure at room temperature or drying/curing can be accelerated by the application of heat to form a coating that entraps the contaminant therein. The coating and the entrapped contaminant can then peeled from the surface and safely disposed of to minimize hazardous waste. The coating includes a colorimetric additive that is specific to the contaminant, the coating and the contaminant producing a visual indication of contamination.

Sampathkumaran, Uma↗

DOE OSTI2023

Removable smart sequestration coatings for hazardous metals

Sampathkumaran, Uma↗

DOE OSTI2020

2020 LANL Contributions to the BATS Test in WIPP

The DOE Office of Nuclear Energy (DOE-NE) repository research and development program seeks to provide a sound technical basis for multiple viable disposal options, increase confidence in the robustness of generic disposal concepts, and develop science and engineering tools needed to support disposal concept implementation. Sandia, Los Alamos, and Lawrence Berkeley National labs are conducting research into salt, which includes the Brine Availability Test in Salt (BATS) field test at the Waste Isolation Pilot Plant (WIPP), a DOE Office of Environmental Management facility. BATS is leveraging the existing infrastructure associated with the WIPP to advance science informing generic disposal concepts. BATS is an ongoing heated borehole experiment being conducted in the WIPP underground. The goal of this experiment is to reduce the uncertainty associated with spent nuclear fuel disposition in geologic salt formations. The BATS experiments is designed to accomplish this by increasing our understanding of brine migration in salt, assessing damaged zones from mining and drilling, simulating a post-closure environment, confirming salt properties, and providing data for model validation. Phased testing for generic salt repository R&D was proposed in 2015. Subsequently, borehole thermal testing was developed as a first step in this process. This document summarizes the work conducted on the BATS experiment during fiscal year 2020 with an emphasis on the contributions by Los Alamos National Lab.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2023

Non-condensable gas in the refrigerant of air-source heat pumps: Interactions between detection features, charge level, and temperature

Not provided.

Engineering↗

DOE OSTI2022

Plastic waste upgrade to olefins via mild slurry microwave pyrolysis over solid acids

Chemical upcycling technologies are emerging as the most viable to combat plastic waste accumulation. Among them, catalytic pyrolysis is very promising as it is feedstock agnostic. However, the high energy demand associated with pyrolysis can lead to significant carbon dioxide production. In this work, we demonstrate that coupling microwave heating with suitable solid acid promoters in a slurry reactor coupled with a distillation unit can overcome the energy-related challenge of conventional pyrolysis, by operating at modest temperatures (350–375 °C), enhancing transport, and furnishing high yields of olefins (~88 %) in seconds, with medium-sized olefins (>75 %) composing a significant fraction. Reduced thermal gradients minimize coke formation, further improving the performance. Techno-economic analysis and life cycle assessment indicate the potential of the technology.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2021

Alternative Liquid DSA Containers for Sludge Slurry Storage in the SRNL Shielded Cells

A pending revision of the Documented Safety Analysis (DSA) for the Savannah River National Laboratory (SRNL) defines “DSA containers” for liquid sludge slurries as containers not susceptible to a flashing spray release in a fire and requires that a list of DSA containers be maintained. High Level Waste (HLW) samples are typically received from the Savannah River Site (SRS) tank farm after retrieval from the storage tanks. Glass bottles are preferred for long-term storage of radioactive liquid sludge slurry samples but are not on the DSA container list. An evaluation has been conducted to identify vessel lids for the glass bottles that would vent prior to pressurization and liquid superheating in a fire event. Low melting Field’s Metal eutectic alloy with a melting point of 62 °C has been identified as a preferred material of construction for vessel lids for this application because the material is resistant to puncture and is expected to have good chemical compatibility and radiation stability in the shielded cells environment. A test vessel was designed to evaluate the alloy and confirm that it would melt before the water in the vessel reaches the boiling point. The tests confirmed: 1) that the reported melting point of the alloy was accurate, 2) that a top fashioned from this material will melt creating an open atmosphere in the vessel headspace prior to sample boiling under moderate and fast heating rates, and 3) that nonuniform heating of the bottle from the bottom also results in melting of the alloy prior to boiling. Based on the results, neither an engulfing fire with standing or toppled bottles or a fire producing localized heat at the vessel bottom would result in flashing spray conditions.

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Hydrocoals from waste biomass via catalytic hydrothermal carbonization processing

This study investigates how operating conditions (temperature and residence time) and benzoyl chloride impact hydrochar production from almond shells through hydrothermal carbonization. Carbon content rises while volatile matter decreases with increasing temperature, yielding a hydrochar with an estimated heating value of 28 MJ/kg. Elevated temperatures lower the O/C and H/C atomic ratios of hydrochars. Even at the lowest temperature under scrutiny, catalytic experiments using benzoyl chloride enhance carbonization and fuel ratio across all temperatures. Hydrochars produced through catalytic runs demonstrate elevated fuel ratios relative to those generated through noncatalytic runs, despite operating under the same conditions. These insights reveal the capacity of benzoyl chloride as a catalyst to improve hydrochar properties, suggesting its utility for advancing both the efficiency and effectiveness of hydrothermal carbonization processes.

09 BIOMASS FUELS↗

DOE OSTI2020

Product consistency test results for the LAW Phase 4 gases

In this report, the Savannah River National Laboratory provides chemical analysis of Product Consistency Test (PCT) leachates from a series of simulated nuclear waste glasses fabricated at the Pacific Northwest National Laboratory (PNNL). The series included quenched and canister-centerline cooled (CCC) versions of the glasses. The resulting data will be used in the development of enhanced property/composition models for waste vitrification at Hanford. For some of the glass leachates, minor scatter among the triplicate values of some analytes were observed. For other leachates, there were more significant differences among the triplicate values. A review of the PCT data noted that there was little difference between the normalized values based on targeted or measured glass composition. Several of the study glasses have normalized concentration of element “i” (NCi) values that are greater than the Hanford Tank Waste Treatment and Immobilization Plant immobilized low-activity waste constraint of 4 g/L for boron (B), sodium (Na), and silicon (Si). The results of these glasses will help ensure the ability of advanced glass performance models to appropriately predict acceptable compositions. For the study glasses with NCi values exceeding 4 g/L, the CCC heat treatment samples had generally lower NCi values than quenched samples. The samples of the Environmental Assessment (EA) reference glass included with each PCT set had generally consistent NCi values. The release rates for boron (B), potassium (K), lithium (Li), sodium (Na), and silicon (Si) were highly correlated for the study glasses.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2020

Brine Availability Test in Salt: Thermal-Hydrological-Mechanical-Chemical Simulations of a Heated Borehole in Salt - 20239

The Brine Availability Test in Salt (BATS) is a collaboration between Los Alamos, Sandia, and Lawrence Berkeley National Laboratories that is being conducted to reduce the uncertainties associated with disposal of spent nuclear fuel (SNF) and high-level radioactive waste (HLW) in a hypothetical bedded salt repository. Bedded salt formations may be an acceptable host rock for disposal of nuclear waste due to salt's high thermal conductivity, extremely low permeability, and self-healing capability. In this paper, we report on the first round of the BATS project, a 'shakedown test' known as Phase 1s, with an emphasis on the supporting numerical modeling. The experiment was conducted at the Waste Isolation Pilot Plant (WIPP) using previously drilled horizontal boreholes. The test included a heater borehole in which temperature, pressure, and moisture was monitored, and two nearby temperature monitoring boreholes. Numerical simulations that reflect the 36-year-long history of activity at the WIPP site are necessary to develop the appropriate initial conditions. Testing with different heater designs reveals that a 750 W radiative heater within a borehole can achieve the 120 deg. C borehole wall temperature goal. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

toughio v1.2.2

TOUGH is a widely used general purpose numerical simulator designed for fluid and heat flows of multiphase, multicomponent fluid mixtures in porous and fractured media, which has been applied to many real-world problems such as underground geological storage, geothermal reservoir engineering or nuclear waste disposal, to name a few. `toughio` is a lightweight, object-oriented and vectorized Python library that aims to provide user-friendly routines to facilitate pre- and post-processing of a TOUGH simulation. Although its primary target is the latest version TOUGH3, `toughio` can also be used to read/write TOUGH2 input/output files. Currently, to the best of our knowledge, only PyTOUGH offers an exhaustive number of features to carry out a complete TOUGH simulation using a scripting language. `toughio` and PyTOUGH share the same objectives, yet with different approaches and philosophies. On the one hand, a PyTOUGH mesh is represented as a MULGRAPH geometry where elements can be unstructured horizontally but only layered vertically. It also checks that the model parameters are valid to ensure that a TOUGH simulation runs smoothly. On the other hand, although it provides basic meshing features, `toughio` mostly relies on common third-party softwares (e.g. Abaqus, FLAC3D, Gmsh, LaGriT) to generate the mesh by importing and converting it to a TOUGH mesh, which also conveniently facilitates the coupling of TOUGH with any other simulator that also supports the same mesh formats. Besides, `toughio` is designed to be just a TOUGH input and output file reader/writer. It assumes that the user knows what he is doing and does not verify the validity of the model parameters (`toughio` does verify the functional arguments).

Luu, Keurfon↗

DOE OSTI2022

South Texas Industrial Assessment Center (Final Report)

The South Texas Industrial Assessment Center (ST-IAC) provides small to mid-size manufacturing companies and water treatment plants in the Rio Grande Valley of Texas, free energy assessments to help them reduce costs and stay competitive for sustainable development. The ST-IAC operates within the University of Texas Rio Grande Valley (UTRGV), and is the largest Hispanic-serving IAC in the U.S. Created in 2016, the ST-IAC, situated in the most economically disadvantaged region in the country, has been successful in training students and assessing local industries served by a predominantly Hispanic population. UTRGV, now the second largest Hispanic Serving Institution (HSI) of higher education in the U.S., has a student population of 32,000, of which 90% is Hispanic. While Covid-19 had a negative impact to our program during Budget Periods (BP) 4 and 5, the center still managed to provide opportunities for individuals, manufacturing and water industries in the local region. The program developed an energy engineering program in the region and further advanced national priorities. Those include resilience and sustainability of operations by implementing energy efficiency processes, renewable energy sources, decarbonization, battery storage, and cybersecurity in south Texas.

14 SOLAR ENERGY↗

DOE OSTI2023

Management of Alkali and Alkaline Earth Fission Products in Used Pyroprocessing Salt

Pyroprocessing of spent nuclear fuel (SNF) involves dissolving metallic fuel into a molten salt electrolyte (typically eutectic LiCl-KCl) and then preferentially depositing actinides onto inert cathodes. Subsequent operations include drawdown of residual actinides and lanthanides from the electrolyte prior to re-using the salt. The recovered actinides are recycled and the recovered lanthanides are disposed as waste. Alkali and alkaline earth metal fission products in the fuel, such as Cs, Sr and Ba, dissolve into the salt during electrorefining. The concentrations of these elements buildup over time in the molten salt electrolyte, which may change the freezing point. The radioactive decay of 137 Cs and 90 Sr (half life 30 and 29 years) generates significant heat and produces strong ionizing radiation fields (β and γ). The increasing heat load and radioactivity as these elements build up in the molten salt requires frequent replacement and disposal of the electrolyte salt. Alternatively, the salt can be treated to remove these and other elements and then recycled to the electrorefiner. An effective strategy to manage these alkali and alkaline earth metal fission products in the molten salt electrolyte would increase the efficiency of pyroprocessing and decrease the volume of salt waste requiring disposal. Alkali and alkaline earth metal fission products are extremely stable in molten salt as chlorides--even more stable than the LiCl-KCl eutectic base salt--making them challenging to remove. They are not removed during drawdown operations to recover residual actinides and lanthanides and a separate operation is required to sufficiently purify the salt for reuse. This work is focused on selecting a method for separating Cs, Sr and Ba from the salt recovered from the lanthanide drawdown operation prior to recycling the cleaned salt back to the electrorefiner. Not addressed in this work is the management of the waste stream produced by the separation. This report summarizes the issues to be addressed when developing removal strategies for cesium, strontium, and barium and reviews existing methods to identify suitable methods and any technological gaps in their application.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2021

Human-in-the-loop Sensing and Control for Commercial Building Energy Efficiency and Occupant Comfort

Most of the existing heating, ventilation and air conditioning (HVAC) systems in commercial buildings operate in a conservative manner by assuming maximum occupancy in each room during pre-specified periods of the week, leading to significant energy being wasted as rooms are over-conditioned compared to the actual requirements of the occupants. Though critical, our understanding of occupancy patterns and thermal comfort needs of the occupants in commercial buildings is lacking and it is well known that both of these quantities are stochastic and time-varying, thus requiring sensing solutions to estimate them. This project had the goal of designing, implementing and evaluating a hardware and software solution to ameliorate this challenge. In particular, a depth camera (one whose pixels reveal distance from the camera as opposed to color values) placed on doorways is used to detect entrance and exit events from thermal zones in the building, and thereby estimate their occupancy levels. This information is then fed to a novel control algorithm that can, through interactions with the HVAC system, learn how to provide control inputs that maximize comfort and minimize energy waste. The resulting system represents a significant improvement over existing controllers for commercial HVAC systems and allowed us to improve our understanding of the design of future human-in-the-loop control solutions. For this solution to be feasible, the project had target metrics for its performance and cost. In particular, entrance and exit events for occupants moving about the building would need to be detected with an accuracy higher than 97%; and the resulting control inputs derived from this information would need to lead to approximately 10% energy savings compared to a schedule-based controller. Furthermore, regarding the final hardware design, the project had a target bill of materials (BOM) cost for the sensing solution of less than US$200 per unit while using less than 25W of power on average. All of these target metrics were met or exceeded by our final proposed solution. We performed evaluations by deploying the system in over 20 rooms of different types across 6 commercial buildings in Pittsburgh, PA over the course of three years, and performing targeted controlled experiments to test its performance along the different metrics. The human-in-the-loop control solutions (both hardware and software) developed through this project are expected to lead to significant improvements in the comfort and energy efficiency of HVAC systems used in commercial buildings. The insights we developed through the project pave the way to HVAC systems that can condition interior spaces according to their real-time utilization and the thermal comfort needs of the occupants, thereby reducing energy use. They also open up a new learning-based way of configuring HVAC controllers without having to manually fine-tune them for each building. These innovations can significantly increase the adoption of novel control solutions by the industry and thereby save resources and reduce costs of operation.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗

DOE OSTI2022

Using discrete Bayesian networks for diagnosing and isolating cross-level faults in HVAC systems

Fault detection and diagnosis (FDD) technologies are critical to ensure satisfactory building performance, such as reducing energy wastes and negative impacts on occupant comfort and productivity. Existing FDD technologies mainly focus on component-level FDD solutions, which could lead to mis-diagnosis of cross-level faults in heating, ventilating, and air-conditioning (HVAC) systems. Cross-level faults are those faults that occur in one component or subsystem, but cause operational abnormalities in other components or subsystems, and result in a building level performance degradation. How to effectively diagnose the root cause of a cross-level fault is the focus of this study. Here, this paper presents a novel discrete Bayesian Network (DisBN)-based method for diagnosing cross-level faults in an HVAC system commonly used in commercial buildings. A two-level DisBN structure model is developed in this study. The parameters used in the DisBN model are obtained either from expert knowledge or through machine-learning strategies from normal system operation data. Meanwhile, the probability parameters are discretized to incorporate the uncertainties associated with typical expert knowledge. Thus, the developed DisBN method addresses the challenges many other BN based FDD methods face, i.e., the lack of fault data for BN parameter training. The developed DisBN represents causal relationships between a fault and its cross-level system impacts (i.e., fault symptoms or fault indicators) by considering how fault impacts propagate across different levels in an HVAC system. A weather and schedule information-based Pattern Matching (WPM) method is employed to automatically create WPM baseline data sets for each incoming real time snapshot data from the building systems. Consequently, BN inference and real-time diagnostics are achieved by comparing incoming snapshot data and the WPM baseline data set. The proposed method is evaluated using experimental fault data collected in a campus building. Fault diagnosis results demonstrate that the WPM-DisBN method is effective at locating the root causes of cross-level faults in an HVAC system.

32 ENERGY CONSERVATION, CONSUMPTION, AND UTILIZATI↗