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DOE OSTI2022

Pilot Testing of a Highly Efficient Pre-combustion Sorbent-based Carbon Capture System

TDA developed and demonstrated a highly efficient pre-combustion carbon capture system. The overall objective of this work was to develop a new sorbent-based pre-combustion carbon capture technology for Integrated Gasification Combined Cycle (IGCC) power plants. In this project our goal was to demonstrate the techno-economic viability of the new technology by 1) demonstrating it in large-scale slipstream tests, and 2) carrying out a high fidelity engineering and cost analysis. TDA’s process used an advanced physical adsorbent that selectively removes CO 2 from coal-derived synthesis gas above the dew point of the gas at temperatures as high as 300°C. The sorbent consists of a mesoporous carbon whose surface was grafted with functional groups that remove CO 2 via a well-known acid-base interaction. As documented in bench-scale experiments and field tests with actual coal gas, the sorbent achieved a very high capacity for CO 2 at temperatures as high as 300°C. The sorbent bound CO 2 more strongly than common physical adsorbents, providing the chemical potential needed for the high temperature operation. However, because CO 2 does not form a true covalent bond with the surface sites (as is the case with chemical absorbents), the sorbent regeneration could be carried out with only a very small energy input. The heat input to regenerate our sorbent was only 4.9 kcal per mol of CO 2 , which is much lower than that for chemical absorbents (e.g., 29.9 kcal/mol CO 2 for sodium carbonate) and was similar to the requirements of physical solvents (e.g., 4 kcal/mol CO 2 for Selexol TM ). Because the sorbent operates above the dew point of the synthesis gas (unlike the Selexol TM process), a higher power cycle efficiency can be achieved. With previous DOE/NETL funding (Contract No. DE-FE-0000469), we demonstrated the techno-economic viability of the technology in bench-scale tests and slipstream demonstrations at the National Carbon Capture Center (NCCC), Wilsonville, Alabama and Wabash River IGCC plant in Terra Haute, Indiana. We demonstrated a stable working CO 2 capacity for over 11,650 cycles with simulated synthesis gas. We also evaluated its performance with actual synthesis gas in two test campaigns at the Wabash River IGCC Plant, Terre Haute, IN and the National Carbon Capture Center (NCCC), Wilsonville, AL. The slipstream tests clearly showed that the actual coal gas constituents and potential contaminants (e.g. trace metals, halides, tars) had no effect on the sorbent’s ability to remove CO 2 (the same sorbent beds were used in both field tests with no sign of deactivation for 2,000 cycles with over 26,750 SCF of gas treated). As expected, due to the high temperature CO 2 removal capability and low energy needed to regenerate the sorbent, the power cycle efficiency with our process was greater than 34% on a higher heating value (HHV) basis; in comparison, the same IGCC plant equipped with the Selexol TM solvent for carbon capture can only achieve 31.4% HHV efficiency. The capital cost for an IGCC system with TDA’s process is estimated as $2,417/kW e , which is 12% lower than that of the IGCC/ Selexol TM process. The levelized cost for electricity including the transport, storage and monitoring (TS&M) cost for CO 2 was calculated as $\$ $92.9/MWh (lowest reported to our knowledge), which is much better than the $105.2/MWh estimated for the IGCC/ Selexol TM process. In this project (DE-FE0013105), TDA Research, in collaboration with our partners Gas Technology Institute (GTI), Illinois Clean Coal Institute (ICCI), University of California, Irvine (UCI), University of Alberta (UOA), Siemens, NCCC and Sinopec advanced the technical maturity of the technology; scaling it up by a factor of 100. We optimized the reactor design using computational fluid dynamics (CFD); using adsorption modeling we improved the pressure swing adsorption (PSA) cycle sequence. We carried out two field test campaigns with a fully-equipped 0.1 MW e prototype unit (for a total of 844 hours) using actual synthesis gas to prove the viability of the new technology. A successful 30 day (707 hrs) evaluation was completed at NCCC under air blown gasification conditions. We demonstrated 97.3% carbon capture at 1,500 SLPM, 93% carbon capture at 1,800 SLPM, and 90% carbon capture at 2,100 SLPM in the NCCC tests. We also demonstrated the system for 137 hours at a Sinopec petrochemical plant under oxygen blown gasification, demonstrating 86% carbon capture at 2,660 SLPM. In collaboration with University of California, Irvine (UCI), we completed a techno-economic analysis (TEA) for TDA’s warm gas cleanup technology integrated to IGCC power plant. The net plant efficiencies (on a coal HHV basis) for the warm gas cleanup cases were estimated to be 34.0% for E-GasTM gasifier, 34.4% for GE gasifier, 33.4 for the Shell gasifier and 34.2 for the TRIG TM gasifier (Cases 2, 4, 6 and 8 in this study) with a catalytic combustor for CO 2 purification, which are significantly higher than those for the Cold Gas Case, or an increase of as much as 12% in the heat rate for Case 2, 6% for Case 4, 9% for Case 6, and 9% for Case 8. The 1st year cost of electricity with the transport, storage and monitoring (TS&M) costs for the CO 2 included was $\$ $129.2/MWh for the E-GasTM gasifier Warm Gas Cleanup Case, $\$ $131.9/MWh for the GE gasifier Warm Gas Cleanup Case, $\$ $146.8/MWh for the Shell Gasifier Warm Gas Cleanup Case, and $\$ $129.9/MWh for the TRIG TM gasifier Warm Gas Cleanup Case. For comparison, the costs for the baseline Cold Gas CO 2 removal with Selexol for the different gasifiers were: $\$ $146.6/MWh for the E-Gas TM gasifier, $\$ $142.2/MWh for the GE gasifier, $\$ $159.0/MWh for the Shell gasifier and $\$ $144.3/MWh for the TRIG TM gasifier. In summary, the costs for our system were 7 to 12% lower than the corresponding Cold Gas Cleanup cases. The results of this techno-economic analysis suggested that TDA’s high temperature PSA-based Warm Gas Clean-up Technology can make a substantial improvement in the IGCC plant thermal performance for achieving near zero CO 2 emissions for E-Gas TM , GE, Shell and TRIG TM gasifier based IGCC power plants. The capital expenses were estimated to be lower than that of Selexol’s™. Taken together, the higher net plant efficiency and lower capital and operating costs resulted in substantial reduction in the cost of carbon capture for the IGCC plant equipped with TDA’s high temperature PSA-based carbon capture system. Finally, in collaboration with Gas Technology Institute (GTI) we completed the environmental health and safety assessment for TDA’s warm gas carbon capture technology.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2021

A review of rare earth elements and yttrium in coal ash: Content, modes of occurrences, combustion behavior, and extraction methods

Rare earth elements and yttrium (REY) have attracted considerable attention over the last decade because of their vital roles in clean energy, consumer product, national defense and security applications, among other uses. Due to the retention of REY during coal burning, coal combustion ash is considered as potential alternative sources for REY. Understanding the content, speciation, retention and/or transformation behavior of REY during coal combustion not only expands our knowledge of the combustion behavior of the trace elements in coal, but also provides basis for modeling REY partitioning during coal combustion and for developing economically viable REY recovery technologies. This review makes a critical summary of recent progress in the study of REY in coal ash. The contents and the extraction potentials of REY in coal ash derived from 15 major coal-producing countries worldwide were summarized and evaluated. Various analytical methods for determining REY bulk contents and speciation, together with the solid sample pretreatment, analytical accuracy and precision, advantages and disadvantages were summarized and compared. Modern analytical approaches combined indirect methods (e.g., sequential extraction) shed light on the physical distribution, mineralogy, and the chemical state of REY in coal ash. Three types of REY occurrences in coal ash, including Si-Al glassy association, discrete minerals or compounds, and organic association (bound with unburned carbon) were defined in the review. The glassy association can be further divided into REY minerals closely bound to glass phases and dispersed throughout the glassy structure. REY partitioning in various emission streams, the size distribution, and their enrichment behavior in coal ash were discussed. Additionally, thermal behavior and transformation of various REY forms in coal during combustion process, including organic-associated REY, REY phosphates, REY carbonates, clay-bound REY and among others were summarized. Two possible retention mechanisms of REY by aluminosilicate glass at boiler temperature were proposed: the incorporation of the individual REY phases into the glass as inclusions and the diffusion of REY phases throughout Si-Al glass structures in the melting process. Feed coal mineral types, mineral-mineral associations, boiler conditions, and other factors control the retention process. After coal combustion, the speciation of REY in fly ash may be modified by the reactions of REY phases with flue gas components. Further, an overview of REY transformation mechanisms during coal combustion was deeply discussed. Finally, current extraction techniques for REY recovery from coal combustion ash were introduced. Future outlooks and research problems were also identified.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Description of FY25 Theory and Simulation Performance Target: Development of an integrated modeling framework for fusion reactor design and assessment

The urgency to deliver fusion power is growing now more than ever, with increasing pressure for both public programs and private companies to meet milestones timelines and overcome significant remaining technical challenges to ensure growth of a nascent fusion industry in time to meet rapidly growing clean energy demands. With incredible advancements in computation and years of investment in fusion model development and validation, integrated modeling is poised to fill a key role in accelerating the timeline to a fusion pilot plant (FPP). Future fusion pilot plants will operate in regimes far beyond current experience, and device design will rely on physics-based prediction and extrapolation. Many concepts will also rely on simulation to assess safety (shielding, tritium management, materials activation and lifetimes), economics and scalability before the decision to build. Importantly, integrated simulation can be used to reveal and solve the complexities of system integration that may otherwise not be apparent in physical components or models developed in isolation. New experimental test facilities that produce relevant conditions to validate and resolve key technical challenges for various subsystems (materials, blankets, fuel cycle, etc.) have been repeatedly called for by the fusion community but are not yet realized. Integrated modeling has an important role in identifying realistic load conditions (thermal, electromagnetic, plasma, neutron and photon loads, etc.) and defining the components and experiments for these test facilities in order to ensure meaningful validation that sufficiently reduces modeling uncertainties and technical risk for the full integrated reactor. The Fusion REactor Design and Assessment (FREDA) SciDAC project is building a component-based integrated modeling framework & data structure to enable self-consistent, multi-fidelity, iterative optimization workflows for the fusion reactor design process. FREDA aims to shorten the time to viable designs by providing a set of flexible workflows to support the various stages of the design process using an integrated model hierarchy, ranging from the simple analytic descriptions to the highest fidelity, theory-based plasma and engineering modeling developed by the fusion and fission communities. These tools are expected to be needed for timely support of FPP design in the milestone program and in the FIRE collaboratives. The plasma simulation backbone of FREDA is IPS-FASTRAN with newly developed coupled Core-Edge Pedestal-SOL (CESOL) workflows, which is being extended to the far-SOL region up to the plasma facing components. FREDA incorporates the FERMI engineering modeling suite and will enable self-consistent evaluation of the thermal shields, limiters, blanket, magnets, and other surrounding structures with predictions of temperatures, erosion, dpa, activation, tritium generation and transport, creep, corrosion, material degradation, etc. Parametric generation of 3D CAD enables rapid iteration of component geometry in response to plasma and loading specifications.

70 PLASMA PHYSICS AND FUSION TECHNOLOGY↗

DOE OSTI2024

Calcium-organic matter fouling in nanofiltration: Synchrotron-based X-ray fluorescence and absorption near-edge structure spectroscopy for speciation

Calcium (Ca)-enhanced organic matter (OM) fouling of nanofiltration (NF) membranes leads to reduced flux during desalination and requires frequent cleaning. Fouling mechanisms are not fully understood, which limits the development of targeted fouling control methods. This study employed synchrotron-based X-ray fluorescence (XRF) and X-ray absorption near-edge structure (XANES) spectroscopy to quantify the spatial distribution and mass of Ca deposition as well as changes in the Ca coordination environment characteristic of specific fouling mechanisms, respectively. Bench-scale filtration experiments were performed using feed solutions containing Ca and ten different types of organic matter (OM), as well as the common scalants, calcium carbonate (CaCO 3 ) and calcium sulfate (CaSO 4 ). Osmotic backwash (OB) was performed at regular intervals for fouling control. Ca-OM aggregation resulted in greater flux decline and lower flux recovery during OB than Ca conditioning of membranes followed by filtration of feed solution with OM. Linear combination fitting (LCF) of XANES absorption spectra from fouled membranes indicated that Ca-OM aggregation preferentially occurred for OM types that exhibited both high carboxylic group and negative charge density. Consequently, these OM types exhibited greater deposition of Ca and TOC on the membrane surface when compared to other OM types. For the coexistence of scalants and OM, Ca speciation within the fouling layer was characteristic of both Ca bound to the membrane (i.e. potential bridging, charge screening) as well as Ca-OM aggregation and deposition mechanisms, while a range of crystal polymorphs were observed to occur simultaneously. XRF and XANES represent powerful tools for the elucidation of NF fouling mechanisms by quantification of Ca deposition as well as Ca speciation. Fouling control methods should target OM types with high carboxyl group density and negative charge to neutralize or eliminate interactions with Ca.

42 ENGINEERING↗

DOE OSTI2021

Development and Field Testing Novel Natural Gas Surface Process Equipment for Replacement of Water as Primary Hydraulic Fracturing Fluid (Final Report)

Southwest Research Institute® (SwRI ® ), Schlumberger Technology Corporation (SLB), and Chevron Corporation ® (Chevron) developed a novel, optimized, and lightweight process for natural gas (NG) to replace water as a low-cost fracturing medium with a low environmental impact. Hydraulic fracturing is used to increase oil and NG production by injecting high-pressure fluid, primarily water, into a rock formation, which fractures the rock and releases trapped oil and NG. This method was developed to increase yield and make feasible production areas that would not otherwise be viable for large-scale oil and NG extraction using traditional drilling technologies. Since the fracturing fluid is composed of approximately 90% water, one of the principal drawbacks to hydraulic fracturing is its excessive water use and associated large environmental footprint. According to recent data collected at fracture sites within the United States, fracturing applications in North America can consume as much as 9 million gallons of water per well. During the fracturing process, some of the fracturing fluid is permanently lost and the portion that is recovered is contaminated by both fracturing chemicals and dissolved solids from the formation. The recovered water or flow-back represents a significant environmental challenge, as it must be treated before it can be reintroduced into the natural water system. Although there is some recycling for future fracturing, the majority of the flow-back water is hauled from the well site to a treatment facility or to an injection well for permanent underground disposal. To mitigate these issues, an optimized, lightweight and modular surface process using NG to replace a majority of the water was developed as a cost-effective and environmentally clean fracturing fluid. Using NG will result in significantly less consumption since the gas that is injected as a fracturing fluid will be mixed with the formation gas and extracted as if it were from the formation itself. This process will minimize the collection, waste, and treatment of large amounts of water and will reduce the environmental impact of transporting and storing the fracturing fluid. There are two major steps involved in utilizing NG as the primary fracturing medium: (1) increasing the supply pressure of NG to wellhead pressures suitable for fracturing and (2) mixing the required chemicals and proppant needed for the fracturing process at these elevated pressures. The second step (NG-proppant mixing at elevated pressures) still requires demonstration; but very similar processes have been demonstrated in the field with other gases such as nitrogen (N 2 ) and carbon dioxide (CO 2 ). However, the first step (a compact, on-site unit for generating high-pressure NG at costs feasible for fracturing) has not been developed and is currently not commercially available. Due to the inherent compressibility of NG, more energy is required to compress the gas than what is required to pump water (or other incompressible liquids) to the very high pressure required for downhole injection. This project aimed to develop a novel, hybrid method to overcome this challenge. The project accomplishments and findings are discussed in this report. Ultimately, the research and development efforts described herein demonstrate that fracturing with NG foam is a feasible alternative to using water.

02 PETROLEUM↗

DOE OSTI2023

Conclusions from 3 years of continuous capture plant operation without exchange of the AMP/PZ-based solvent at Niederaussem – insights into solvent degradation management

A many times heard mantra of solvent degradation management in amine-based post combustion capture is “keep the solvent clean” to minimize solvent consumption. It is assumed that the amine losses would decrease by the removal of metals, degradation products, and reactive trace components which are captured from the flue gas, like NO 2 (as potentially driving components of the amine degradation besides dissolved O 2 ). However, this theoretical hypothesis – based on results from laboratory experiments typically generated with fresh amines – disregards the complexity of the solvent matrix, interaction of potential metal catalysts with degradation products and oxidizing agents, and specific chemical requirements which must be fulfilled before a degradation mechanism can proceed. Degradation of the solvent CESAR1 (aqueous solution of 3.0 molar 2-amino-2-methylpropan-1-ol (AMP) and 1.5 molar piperazine (PZ)) is investigated in a unique long-time test campaign (testing time up to now 40 months; 24/7 operation) without replacement of the solvent inventory at the capture pilot plant at the lignite-fired power plant in Niederaussem. Three solvent management strategies with different effect mechanisms are investigated and evaluated: (a) removal of only anionic compounds and trace elements (within 75 days solvent inventory treated two times) and anionic as well as cationic compounds and trace elements (114 days, inventory treated four times) from the solvent by ion exchange, (b) adsorptive removal of trace elements from the solvent by active carbon in 35% of the operating time, and (c) removal of >80% NO 2 by flue gas pretreatment with thiosulfate/sulfite solution (dosing for 2,000 h). The results of the testing program clearly show that “solvent cleanliness” is not a well-defined parameter and that results from laboratory tests, tests without fully representative industrial flue gasses, and short-term testing of monoethanolamine cannot be generalized for other solvents and industrial application. Furthermore, these results showcase that specific degradation management considering solvent, capture plant and flue gas quality is reasonable. Overshooting efforts for solvent management are contra-productive and produce unnecessary waste streams, efficiency losses and costs.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

DOE OSTI2024

Electromagnetic Energy-Assisted Thermal Conversion of Fossil-Based Hydrocarbons to Low-Cost Hydrogen

The goal of this project was to develop and optimize catalysts for methane decomposition, particularly focusing on regeneration via an electromagnetic energy-assisted mechanism, to produce hydrogen more cost-effectively compared to electrolysis routes. To achieve this goal, the project pursued several key objectives. The project began with the preparation and testing of various catalysts. A nickel-silica based catalyst was identified as the most promising material for the pyrolysis of methane into carbon and hydrogen. Kinetic parameters for methane decomposition were determined, aiding in computational modeling efforts. Structured catalysts were investigated, highlighting the need for frequent cleaning or regeneration to maintain performance, with methane conversion rates exceeding 70% in tube furnace tests. Computational fluid dynamics modeling was employed to optimize reactor designs and electrode angles, leading the project team to propose a multi-compartment thermal conversion system for larger setups. This modeling work was important in understanding reaction characteristics, carbon deposition rates, and temperature profiles under various conditions. A bench-scale reactor system was assembled to evaluate catalyst regeneration using electromagnetic energy-assisted mechanisms. Experiments demonstrated the potential for carbon removal, though further optimization is needed. The carbon produced from the methane conversion process was evaluated for potential use in lithium-ion battery electrodes. The carbon exhibited properties similar to commercially available high-purity multi-walled carbon nanotubes and nanofibers, with a carbon content greater than 95%. Coin cell batteries assembled with this carbon showed that lower replacement levels (10% to 33%) outperformed the control group, improving specific capacity density and stability. However, higher replacement levels (100%) demonstrated poorer performance, suggesting that excessive carbon substitution negatively impacts battery performance. These findings indicate the potential marketability of the produced carbon as a component in lithium-ion batteries, though further testing is necessary to confirm long-term advantages and disadvantages associated with the use of the carbon product. These results however justified further technoeconomic assessments to determine if the process can provide low-cost hydrogen. The economic feasibility and technical performance of methane decomposition for hydrogen production were assessed, focusing on three plant configurations: 100E (electrically heated), 100C (combustion heated using produced hydrogen), and PE-Hybrid (a combination of pyrolysis (indicating decomposition) and electrolysis). The Levelized Cost of Hydrogen (LCOH) for the pyrolysis configurations was found to be approximately 25% lower than that of electrolysis. The 100E configuration had the lowest LCOH at $\$$3.12/kg. Including carbon product sales significantly improved the economics, with the 100C configuration achieving a negative LCOH of -$\$$0.35/kg. The PE-Hybrid configuration was not economically advantageous compared to pure pyrolysis plants due to its complexity and additional equipment requirements. Ultimately, methane pyrolysis presents a viable method for near carbon dioxide-free hydrogen production, with significant economic advantages over electrolysis, especially when considering the sale of carbon byproducts. The 100E and 100C configurations showed the most promise, with the choice between them ultimately depending on the prices of power and natural gas. In conclusion, this technology has the potential to lower hydrogen production costs by leveraging the methane decomposition process with the sale of valuable carbon byproducts. By optimizing catalyst performance and integrating electromagnetic energy-assisted regeneration, the process can achieve higher efficiency and economic viability, making it a competitive alternative to traditional hydrogen production methods.

08 HYDROGEN↗

NASA NTRS2016

CryoCart Restoration and Vacuum Pipe Construction

Propulsion systems that utilize hypergolic propellants have been used to power space vehicles since the beginning of the space program. Liquid methane and oxygen propulsion systems have emerged as an alternative and have proven to be more environmentally friendly. The incorporation of liquid methane/liquid oxygen (LOX) into the propulsion system has demonstrated an increase in engine performance, as well as a reduction in the volume, size and complexity of the system. Consequently, reducing the total mass of the vehicle which is a crucial aspect that is considered when planning space missions to both the Moon and Mars [1]. Project Morpheus has made significant advancements in liquid oxygen/liquid methane propulsion system technologies by incorporating a LOX/methane propulsion system to a vertical test bed. The vehicle consisted of a 5,000 lb main engine and four 20 lb remote control system (RCS) engines that utilize liquid methane/LOX as its propellant [1]. The vehicle completed successful flight testing at Kennedy Space Center in 2014 which marked the completion of the Morpheus project. Subsequent projects utilizing Morpheus' vertical test bed have been developed to make further advancements. One of the subsequent projects consisted of the addition of a smaller 2,000 lb main engine and a cold helium heat exchanger which would make it possible for a pressurant tank systems to be send to Mars or the Moon by significantly decreasing the overall mass and volume of the pressurant tank. The hot fire tests of the integrated system with the smaller main engine and cold helium heat exchanger were successful at sea level, but further studies are being conducted to better understand how the vertical test bed will behave under thermal-vacuum conditions. For this reason, the integrated vehicle will be taken to Plum Brook to be tested in a chamber capable of simulating these conditions. To ensure that the vehicle will function properly under vacuum conditions, testing will be first completed at the component level. During this process, the igniter of the main engine and the RCS thrusters will be tested under a vacuum. To complete the testing of the components, the test setup first needed to be finalized. The CryoCart is being used to feed the propellants to the test article. The CryoCart is a movable test set-up that was developed in 2009 to provide a mobile platform for testing oxygen/methane systems with hot-fire capability up to 100 lbf. The CryoCart consists of three different systems: Oxygen, Methane, and liquid Nitrogen. The Oxygen and Methane systems are placed into two different carts while the liquid nitrogen system is mainly located in the methane cart. Over the years, the CryoCart has been utilized for different projects and has undergone deterioration. For this reason, a new phase has been developed to rebuild it to working conditions once again. During my internship, I was aiding in the construction and restoration of the CryoCart. In the initial stages of the process, I updated the fluid and electrical schematics for the oxygen, methane, and test article systems. The original CryoCart consisted of an electrical panel that utilized electromechanical relays and a terminal to drive the igniter power and signal, as well as the main fuel and oxygen valves. This electrical panel connected to the CryoCart through various wire harnesses that could be found exiting from the CryoCart. First, it was determined how these harnesses connected to the electromechanical relays so that they worked correctly. Once the electrical system was understood, an alternative for the electromechanical relays and the Molex connectors used throughout the system was sought since these components can often prove to be unreliable. Solid State relays and MIL connectors were purchased to serve as replacements. Upon arrival of the parts, crimping and wiring was completed to install the new solid state relays and MIL connectors. During the replacement of the relays and connectors, system checks of the electrical system were ran to ensure that the system was working correctly. While completing system checks, the pressure transducers that were not functioning properly were also replaced and any issue with the wiring or signal was addressed. Once the electrical components were replaced, the restoration of the fluid system began. Parts of the tubing in the CryoCart had to be rebuild and often consisted of sizing, cutting, bending, filing, and sanding the tubing to prepare it to be flared. Many components had to be proof-tested to bring their certifications up to date, and several components had to be replaced. Various flex hoses, valves, and fittings were send to the Clean Lab because they were new, dirty, or had gone through proof-testing. Once they arrived from the cleaning lab they had to be put back to the system and leak checks and functional tests were conducted. In the Nitrogen system, the copper tubing located in the Oxygen cart was rebuild and Aerogel insulation was added to this section. A new gaseous nitrogen system was added to the CryoCart to purge the vacuum tube which will serve as the test chamber. Once the CryoCart was completed, construction of parts of the vacuum tube began. A flange was manufactured with welded fittings to hold the line of the vacuum pump as well as some extra fittings which will serve as extra inlets used to introduce fluid lines to the vacuum tube. Stress analysis was ran in this flange to ensure that it would not fail under vacuum conditions. The fluid lines leading from the air side of the vacuum to the test article were also constructed and added to the mount that had already been manufactured. Three different sets of tubing were constructed to accommodate the seven different RCS thruster and the main engine igniter that are going to be tested. Full electrical system checks were completed to ensure that all the wire harnesses and valves were functioning. Upon the completion of the CryoCart and the vacuum tube, hot fire testing for the RCS thrusters and the main engine igniter are going to begin. During this time any issues encountered with the engines or igniter will be addressed to ensure that the components function under vacuum conditions. After successful completion of testing, the vertical test bed, Morpheus, will be rebuilt and prepared to be sent to Plum Brook. In Plum Brook, the vehicle will be tested in the thermal-vacuum chamber to demonstrate that integrated lox-methane propulsion system operation in space-like conditions. This internship has allowed me the opportunity to gain valuable hands on experience and to develop skills that will aid in my education as well as in the workforce, while at the same time helping me determine that I would like to further pursue a career in propulsion engineering.

Chaidez, Mariana↗

NASA NTRSDate not supplied

EVA Swab Kit: Tools and Techniques for Collecting Aseptic Samples from Crewed Space Missions

Introduction: When we send humans to search for life on other planets, we'll need to know what we brought with us versus what may already be there. To ensure our crewed spacecraft meet planetary protection requirements—and to protect our science from human contamination—we'll need to assess and verify whether micro-organisms may be leaking/venting from our spacesuits. This requires collecting samples under Extravehicular Activity (EVA) conditions. Detailed, systematic research on forward contamination from robotic spacecraft has been steadily progressing since the Viking missions, but systematic studies of contamination from space suits has not been conducted in many years. The modern EMU (Extravehicular Mobility Unit) suit used by NASA is designed to leak at rates as high as 100 cc/min. Before humans land on Mars there is a critical need to understand the types and quantities of microbes that could be introduced via space suits. The Human Forward Contamination Assessment team at NASA’s Johnson Space Center (JSC) has developed a prototype EVA swab tool [1,2,3,4] designed for use in space to sample cleaned and uncleaned space suits to determine the present day microbial load and eventually the rate of leakage. The ability to assess microbial leakage early in advanced space suit and life support system design cycles will help avoid costly hardware redesign later. Test Objectives: The primary objective of EMU testing was to characterize the type of micro-organisms typically found on or near selected suit pressure joints under suit differential pressure conditions. Most human-borne microbes can fit through a 0.5 to 1.0 µm gap. Knowing which joints are more likely to leak will inform hardware design decisions. Knowing which types of micro-organisms may leak from EVA suits provides a basis for subsequent studies to characterize the viability of those organisms under destination conditions, as well as how far they might spread through natural or human-influenced processes. That data, in turn, will inform exploration mission operations and hardware design. The secondary objective of testing was to evaluate the interface between a fully suited test subject and the EVA swab tool at vacuum. Bulky EVA suits can restrict movement and limit visibility through the helmet visor. Fully suited testing is important for identifying tool design issues prior to flight. At exploration destinations, such as Mars, suited crew may be required to periodically sample their suits as part of an environmental monitoring protocol. Suit Microbial Sampling Results: This report details results of microbial swabs collected from current flight suit configurations worn by crew members assigned to upcoming ISS expedition missions as well as swabs collected from prototype suits intended for use on the Orion spacecraft. These tests were intended to characterize the types of contaminants found on flight suits under current, typical handling conditions. No attempt was made to change suit handling procedures, provide additional sterilization, or to limit typical potential contaminant sources. Using culture based techniques, we cultivated 235 CFU (colony forming units) comprised of 26 bacterial species and one fungal species on the outside of the suits. The fungal species and 14 of the bacterial species were unique to the suit surfaces and were not detected in any of the background samples collected within the chambers. We sequenced 755,434 ribosomal fragments on all of the suit surfaces from swab samples. 557,016 of these sequences represent DNA that survived at least 4 hours at vacuum. These sequences formed 2,464 OTU's (Operational Taxonomic Units, 97% similarity) showing low diversity in the samples. The most abundant sequences that survived vacuum belong to the genera Staphyloccocus, Ralstona, Bacillus and Rhodobacter all of which are common to the human microbiome. [5] See Danko et al., (2021) for more complete details of these first analyses. Further analysis of EVA suit materials with respect to the efficacy of various cleaning protocols and engineered containment solutions is planned to inform suit design for NASA’s Artemis Moon to Mars program crew testing. Swab Tool Function Results: The kit was demonstrated for fit and function in suited subject vacuum tests to determine how well the tool worked as an aseptic microbial sampling device as well as to identify any design elements that could be upgraded for EVA task specific improvement. It was found that sample acquisition efficacy could be enhanced by redesign of the sample canister to end-effector interface. Several modifications of the sample caddy assemblies to optimize EVA safety and functionality were also identified. Consequently, fabrication of the redesigned sample canister to end-effector assembly interfaces and and the sample caddy assemblies are required. Fabrication of sixteen flight sample canister assemblies (8 per each of two EVA Swab Kits) and two sample caddy assemblies are in process to be followed by hardware testing and certification to produce two flight-certified EVA Swab Kits for transport to ISS no earlier than summer of 2022. Sampling Strategy: The International Space Station is an ideal testbed for systematic studies of contamination from crewed vehicles since it has been continuously occupied for 20 years and exposed to non-terrestrial conditions. We will sample the exterior of the ISS during EVA using a purpose-built swab tool capable of maintaining sterility while undergoing temperature changes from -151 to +121°C under hard vacuum. Prior to each EVA, the project team will work with ISS mission managers to identify precise sampling locations, which will vary by EVA based on the translation paths and worksites scheduled for that particular EVA. Ideally, translation path handrails and areas near ECLSS (Environmental Control and Life Support System) external vent openings on a spacecraft would be assessed. There are currently more than a dozen ECLSS external vents on the ISS. Some are connected to systems that vent waste products, while others are intended to equalize cabin pressure. As EVA opportunity allows, microbial samples from any of these external vents would provide a valuable data point, though some will be more useful than others. Four criteria have been identified to help prioritize sampling sites near vents: • EVA Accessibility: To minimize cost, it is desired to piggy-back onto a planned EVA. Therefore, the sampling location must be readily accessible by an EVA crew • Type of Vented Products: Vent products that have been in direct contact with crew, such as cabin air, are more likely to contain microorganisms than vent products associated with isolated systems, such as experiment module combustion products. • Mass of Vented Products: Higher-flow vents are more likely to contain detectible levels of microbial contaminants than lower-flow vents. • Local Environment: Sample locations with relatively benign local conditions, such as warm surfaces shielded from direct ultraviolet (UV) radiation exposure, may be more likely to support microbial growth than locations with harsher local environmental conditions. Because EVA accessibility is the most important criteria, the proposal team worked with an astronaut and flight controllers using the Dynamic Onboard Ubiquitous Graphics (DOUG) tool. The DOUG virtual environment allows an operator to “fly” around the current ISS vehicle configuration to assess EVA translation paths, attach points, and keep-out zones. While analysis on station or rapid return to Earth would be preferable, samples collected from the exterior of the ISS have already been exposed to temperature variations between -157 and +121 °C as well as hard vacuum. Therefore, they should be fairly stable and robust. We hypothesize that samples collected from the ISS exterior could be stored for up to 6 months at -80°C without degradation. Sample canisters will be returned to Earth while frozen at -80°C for analysis, and sterilized canisters can be re-flown back to ISS to support additional sampling opportunities Relevance to NASA Exploration Objectives: These data will allow us to identify new or improved methods, technologies, and procedures for spacecraft sterilization and leakage mitigation to minimize the amount of contamination introduced to the environment by human explorers. This work is funded by NASA research grant: NNH18ZDA001N-PPR References: [1] Bell, M.S. et al. (2015) LPS XLVI, Abst. #1832 [2] Rucker et al. (2018) 42nd COSPAR (PPP.3) [3] Bell, M.S. et al. (2019) Mars Extant Life Conference, Abst. #5096.[4] Bell, M.S. et al., (2020) 43rd COSPAR (BO.2).[5] Danko D, et.al.,(2021)Front.Microbiol.12:608478.

Mary Suzanne Bell↗

NASA NTRS2013

Planetary Protection Bioburden Analysis Program

This program is a Microsoft Access program that performed statistical analysis of the colony counts from assays performed on the Mars Science Laboratory (MSL) spacecraft to determine the bioburden density, 3-sigma biodensity, and the total bioburdens required for the MSL prelaunch reports. It also contains numerous tools that report the data in various ways to simplify the reports required. The program performs all the calculations directly in the MS Access program. Prior to this development, the data was exported to large Excel files that had to be cut and pasted to provide the desired results. The program contains a main menu and a number of submenus. Analyses can be performed by using either all the assays, or only the accountable assays that will be used in the final analysis. There are three options on the first menu: either calculate using (1) the old MER (Mars Exploration Rover) statistics, (2) the MSL statistics for all the assays, or This software implements penetration limit equations for common micrometeoroid and orbital debris (MMOD) shield configurations, windows, and thermal protection systems. Allowable MMOD risk is formulated in terms of the probability of penetration (PNP) of the spacecraft pressure hull. For calculating the risk, spacecraft geometry models, mission profiles, debris environment models, and penetration limit equations for installed shielding configurations are required. Risk assessment software such as NASA's BUMPERII is used to calculate mission PNP; however, they are unsuitable for use in shield design and preliminary analysis studies. The software defines a single equation for the design and performance evaluation of common MMOD shielding configurations, windows, and thermal protection systems, along with a description of their validity range and guidelines for their application. Recommendations are based on preliminary reviews of fundamental assumptions, and accuracy in predicting experimental impact test results. The software is programmed in Visual Basic for Applications for installation as a simple add-in for Microsoft Excel. The user is directed to a graphical user interface (GUI) that requires user inputs and provides solutions directly in Microsoft Excel workbooks. This work was done by Shannon Ryan of the USRA Lunar and Planetary Institute for Johnson Space Center. Further information is contained in a TSP (see page 1). MSC- 24582-1 Micrometeoroid and Orbital Debris (MMOD) Shield Ballistic Limit Analysis Program Lyndon B. Johnson Space Center, Houston, Texas Commercially, because it is so generic, Enigma can be used for almost any project that requires engineering visualization, model building, or animation. Models in Enigma can be exported to many other formats for use in other applications as well. Educationally, Enigma is being used to allow university students to visualize robotic algorithms in a simulation mode before using them with actual hardware. This work was done by David Shores and Sharon P. Goza of Johnson Space Center; Cheyenne McKeegan, Rick Easley, Janet Way, and Shonn Everett of MEI Technologies; Mark Manning of PTI; and Mark Guerra, Ray Kraesig, and William Leu of Tietronix Software, Inc. For further information, contact the JSC Innovation Partnerships Office at (281) 483-3809. MSC-24211-1 Spitzer Telemetry Processing System NASA's Jet Propulsion Laboratory, Pasadena, California The Spitzer Telemetry Processing System (SirtfTlmProc) was designed to address objectives of JPL's Multi-mission Image Processing Lab (MIPL) in processing spacecraft telemetry and distributing the resulting data to the science community. To minimize costs and maximize operability, the software design focused on automated error recovery, performance, and information management. The system processes telemetry from the Spitzer spacecraft and delivers Level 0 products to the Spitzer Science Center. SirtfTlmProc is a unique system with automated error notification and recovery, with a real-time continuous service that can go quiescent after periods of inactivity. The software can process 2 GB of telemetry and deliver Level 0 science products to the end user in four hours. It provides analysis tools so the operator can manage the system and troubleshoot problems. It automates telemetry processing in order to reduce staffing costs. This work was done by Alice Stanboli, Elmain M. Martinez, and James M. McAuley of Caltech for NASA's Jet Propulsion Laboratory. For more information, contact iaoffice @jpl.nasa.gov. This software is available for commercial licensing. Please contact Dan Broderick at Daniel.F. Broderick@jpl.nasa.gov. Refer to NPO-47803. NASA Tech Briefs, September 2013 29 This rapid response computer program predicts Orbiter Wing Leading Edge (WLE) damage caused by ice or foam impact during a Space Shuttle launch (Program "IMPACT2"). The program was developed after the Columbia accident in order to assess quickly WLE damage due to ice, foam, or metal impact (if any) during a Shuttle launch. IMPACT2 simulates an impact event in a few minutes for foam impactors, and in seconds for ice and metal impactors. The damage criterion is derived from results obtained from one sophisticated commercial program, which requires hours to carry out simulations of the same impact events. The program was designed to run much faster than the commercial program with prediction of projectile threshold velocities within 10 to 15% of commercial-program values. The mathematical model involves coupling of Orbiter wing normal modes of vibration to nonlinear or linear springmass models. IMPACT2 solves nonlinear or linear impact problems using classical normal modes of vibration of a target, and nonlinear/ linear time-domain equations for the projectile. Impact loads and stresses developed in the target are computed as functions of time. This model is novel because of its speed of execution. A typical model of foam, or other projectile characterized by material nonlinearities, impacting an RCC panel is executed in minutes instead of hours needed by the commercial programs. Target damage due to impact can be assessed quickly, provided that target vibration modes and allowable stress are known. This work was done by Robert Clark, Jr., Paul Cotter, and Constantine Michalopoulos of The Boeing Company for Johnson Space Center. For further information, contact the JSC Innovation Partnerships Office at (281) 483-3809. MSC-24988-1 Wing Leading Edge RCC Rapid Response Damage Prediction Tool (IMPACT2) Lyndon B. Johnson Space Center, Houston, Texas (3) the MSL statistics for only the accountable assays. Other options on the main menu include a data editing form and utility programs that produce various reports requested by the microbiologists and the project, and tools to generate the groupings for the final analyses. The analyses can be carried out in three ways: Each assay can be treated separately, the assays can be collectively treated for the whole zone as a group, or the assays can be collected in groups designated by the JPL Planetary Protection Manager. The latter approach was used to generate the final report because assays on the same equipment or similar equipment can be assumed to have been exposed to the same environment and cleaning. Thus, the statistics are improved by having a larger population, thereby reducing the standard deviation by the square root of N. For each method mentioned above, three reports are available. The first is a detailed report including all the data. This version was very useful in verifying the calculations. The second is a brief report that is similar to the full detailed report, but does not print out the data. The third is a grand total and summary report in which each assay requires only one line. For the first and second reports, most of the calculations are performed in the report section itself. For the third, all the calculations are performed directly in the query bound to the report. All the numerical results were verified by comparing them with Excel templates, then exporting the data from the Planetary Protection Analysis program to Excel.

Beaudet, Robert A.↗

DOE OSTI2022

Corrosion evaluation of metal foams in eutectic molten salts for high temperature latent heat energy storage application

High-temperature Thermal Energy Storage (TES) has drawn great attention as a technology that can increase the role and profitability of micro nuclear reactors in the decentralized clean energy market. Various research needs have been proposed by Idaho National Laboratory (INL) in "the Integrated Energy Systems: 2020 Roadmap" with the goal of utilizing the high temperature of 550 degrees or more generated in the 4th generation reactor to industrial purposes from the standpoint of integrated energy systems [1]. With the recent development of the 4th generation nuclear power plant, including micro nuclear reactor, there is a great deal of interest in researching how to efficiently couple a heat source to an industrial process through thermal processing. Texas A&M University (TAMU) and INL are currently collaborating to develop a novel latent heat storage design called HITB (Heat pipe-Integrated Thermal Battery). As part of the small-scale experimental demonstration research for HITB, a study for storage medium selection was conducted at TAMU. Eutectic salts have attracted interest as high-temperature heat storage medium for HITB. Especially, chloride molten salts and fluoride molten salts are considered promising candidates due to their high melting temperature, thermal stability, and high latent heat of fusion. Since eutectic salts have poor thermal conductivity in general, it is critical to distribute materials with high thermal conductivity evenly to facilitate the charging and discharging of heat. In this study, metal foam was considered in the HITB system to overcome the poor heat transfer characteristics of eutectic salts. In order to improve heat transfer, it is necessary to study materials with high thermal conductivity, corrosion resistant to molten salts, such as fins, extended surfaces, particles, microcapsulation, or foam structure. Porous structure of copper or aluminum can increase heat transfer area, form a thermal transfer network, and increase the effective thermal conductivity of thermal storage medium [2]. Since the melting temperature is required to be at least 450? in the current HITB design, various eutectic salts are being considered. FLiNaK and FLiBe, which are famous for fluoride salts, are good candidates, but due to the sharp rise in the price of LiF recently, they are excluded for economic reasons to be applied to large-capacity thermal energy storage. On the other hand, chloride salts are very cheap and easy to obtain, have a high melting temperature, and have a high latent heat of fusion, so they are recently in the spotlight as a phase change material. However, because of the hygroscopic nature of chloride salts, HCl gas due to impurity is easy to be released and is particularly vulnerable to corrosion. Chloride eutectic salts have been tested and suggested for metal alloys that are particularly resistant to corrosion, such as SS304, SS316, Hastelloy, Inconel 625, Incoloy 800H, which has low thermal conductivity, and is very expensive [3-6]. Porous materials with high thermal conductivity such as copper and aluminum have been tested for stability in fluids such as paraffin or water as metal foam or metal fin structures, but high temperature corrosion tests were not performed on various eutectic salts yet. Therefore, this study investigated the high temperature corrosion characteristics of metal alloys, such as C10100 foam, C10100 plate, 6101 alloy foam, and SS316 plate, while immersed in the candidate eutectic salts. A total of 20 tests for SS316 coupons and 10 tests for C10100 coupons were performed to ensure the repeatability of the present measurements. Since it is difficult to completely remove the salt inside metal foam due to the complex inner structure of the metal foam, only the surface condition was observed with a microscopy and scanning electron microscopy (SEM) image, except for measuring the corrosion rate and average mass loss.

25 ENERGY STORAGE↗

DOE OSTI2025

Demonstration of Super-X divertor exhaust control for transient heat load management in compact fusion reactors

Nuclear fusion could offer clean, abundant energy. However, managing the power exhausted from the core fusion plasma towards the reactor wall remains a major challenge. This is compounded in emerging compact reactor designs promising more cost-effective pathways towards commercial fusion energy. Alternative Divertor Configurations (ADCs) are a potential solution. In this work, we demonstrate exhaust control in ADCs, employing a novel method to diagnose the neutral gas buffer, which shields the target. Our work on the Mega Ampere Spherical Tokamak Upgrade shows that ADCs tackle key risks and uncertainties for fusion energy. Their highly reduced sensitivity to perturbations enables active exhaust control in otherwise unfeasible situations and facilitates an increased passive absorption of transients, which would otherwise damage the divertor. We observe a strong decoupling of each divertor from other reactor regions, enabling near-independent control of the divertors and core plasma. Our work showcases the real-world benefits of ADCs for effective heat load management in fusion power reactors.

Imaging techniques↗

DOE OSTI2022

Report on Year-4 of Water NSTF Matrix Testing: Facility Maintenance and Accident Testing

Under support from the Department of Energy (DOE) and the Office of Advanced Reactor Technologies (ART), a large-scale test facility has been constructed at Argonne National Laboratory to generate NQA-1 qualified validation data for passive decay heat removal systems in advanced reactors. The Natural convection Shutdown heat removal Test Facility (NSTF) reflects key features of a ½ scale, water-based, Reactor Cavity Cooling System (RCCS) and is intended to study the behavior, bound performance, and ultimately guide design decisions for passive decay heat removal systems for advanced reactors. In addition to the experimental activities detailed in this report, a supportive computational modeling effort is on-going which has been demonstrated to significantly strengthen the experimental program while also improving accuracy of the computer models. Together these create a mutually beneficial relationship integral to meeting the overall program objective of examining the heat removal performance of the RCCS concept. This report serves as a summary of maintenance and experimental activities during the program’s fourth year of water-based operation. A planned six-month maintenance period began in August 2021, during which major inspections, repairs, cleaning, and installation of new instrumentation and data acquisition hardware were conducted. Most significantly, two heaters that faulted during Year-3 were repaired, allowing the facility to resume use of the full heated section area and full range of available electric power. The remainder of the year consisted of eight months of test operations, during which the facility logged 211 hours of active heating across one bake-out (following the maintenance period) and seven matrix tests; five classifieds as Accepted per NQA-1, one as Trending, and one as Failed. Testing began by performing two repeat cases to confirm expected facility response and behavior during both single- and two-phase flow conditions, ensuring no changes were introduced during the maintenance period that might have altered the thermal-hydraulic characteristics of the facility. In continuation of the power parametric series initiated in previous years, a high-power test case was then performed examining heat removal performance at a decay heat load equivalent to 2.4 MWt, full-scale, a level exceeding maximum design targets. Additional testing then introduced various blockage scenarios along the network piping, examining the effects of partial and complete blockages of the flow paths on the system behavior and heat removal performance. A study of static boiling tests directed at understanding the geysering two-phase instability was also conducted. The loop was filled only to the bottom of the tank outlet, creating an open loop configuration that prevents any natural circulation flow from occurring, and the heaters were powered on until the facility reached saturation conditions. Following, a series of quasi-steady-state conditions were introduced by adjusting the inventory level in the adiabatic chimney piping at decreasingly lower elevations above the heated region. A strong correlation of geysering characteristics and loop level was observed, with flow and temperature excursions decreasing in intensity, but increasing in frequency, as the fill were reduced to lower elevations along the chimney piping. Once the level fell very low in the chimney, at points near the top of the heated section, the system reached a stable state of continuous boiling without any occurrence of geysering eruptions. A final significant testing accomplishment this year was successful completion of an “accident scenario” test, whose operating conditions were based on a prototypic decay heat curve provided by Framatome and scaled for the NSTF. This test began by establishing steady-state, single-phase “normal operation” conditions, before simulating an accident trip where the availability of active cooling systems was lost. Loop temperatures gradually increased until reaching saturation and subsequent two-phase boiling flow. Over the course of an extended operational period along the defined decay heat curve, steam boil-off caused gradual but continued depletion of liquid inventory until reaching a critically low level causing flow stagnation and cessation of natural circulation heat removal. At this point, after nearly 72 hours of continuous operation, a cold refill was performed to replenish the system inventory and allow the facility to re-establish closed loop natural circulation flow and return to a safe operational state.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗

DOE OSTI2021

Pilot-Scale Testing of an Integrated Circuit for the Extraction of Rare Earth Minerals and Elements from Coal and Coal Byproducts Using Advanced Separation Technologies

The primary objective of this project was to develop and demonstrate an integrated pilot-scale circuitry for recovering high-value rare earth elements (REEs) from coal and coal byproducts. The target performance was to produce a mixed REE product with content of at least two percent by weight on a dry mass basis in a cost-effective and environmentally benign manner. During the first nine months of the project period (Phase 2 Budget Period 2), pilot plant construction was completed including all field site startup activities such as permitting, engineering design, procurement/bidding, unit fabrication, site construction, equipment installation, module assembly, safety training, and circuit shakedown. During the remaining 21 months of project period (Phase 2 Budget Period 3), detailed field-testing activities were performed including feedstock sample collection and preparation, exploratory testing, circuit modification, detailed parametric study, and performance optimization. A detailed techno-economic analysis was performed based on the pilot plant testing findings which provided various scenarios for REE production. The project successfully accomplished the proposed target performance by producing mixed rare earth oxide (REO) with greater than 90% purity by weight in a continuous pilot scale operation from two distinctly different coarse refuse materials (i.e., West Kentucky No. 13 and Fire Clay coal seams), and at least three secondary sources (i.e., heap leach process and naturally formed acid mine drainage system). Project partners included the University of Kentucky, Virginia Tech, West Virginia University, Alliance Coal, Blackhawk Mining, Mineral Refining Company, and Mineral Separation Technologies. The pilot scale test facility was constructed at a former mining complex owned by Alliance Natural Resource Partners (Alliance Coal). The site was rehabilitated to accommodate the equipment installation, construction and fabrication, electrical power requirement, water line management and containment. The process units constructed and installed included X-ray sorting unit, crushing and grinding unit, physical separation unit, acid leaching unit, solvent extraction unit, and wastewater management unit. A rare earth mineral concentration unit was constructed as a standalone unit for flexible operation. A detailed environmental assessment and control plan was carried out to identify and quantify any potential impacts of the pilot-scale processing circuitry on the human and eco-system health and well-being. Corresponding mitigation strategies and control measures were provided. A conceptual flowsheet was developed to effectively remove thorium and uranium from high purity rare earth oxide mix or any potential radionuclide enriched stream. The two distinct feedstock materials were secured from the Blackhawk Mining Complex in eastern Kentucky where the Fire Clay (Hazard No. 4) seam is processed. The West Kentucky No. 13 (Baker) coarse refuse material was collected from an active process stream at an Alliance coal preparation plant located in western Kentucky. Characterization analysis indicated that both of feed materials generated from the two sources contained >300 ppm of TREEs on a dry whole mass basis which met the requirements for a qualified feed stock. The two feedstocks were further upgraded using a dual x-ray sorter to prepare the feed material for hydrometallurgical circuit. Thermal treatment on feed material prior to leaching was found to: 1) improve the leaching recovery of REEs, 2) increase the leaching kinetics, and 3) allow the leaching reaction to occur at lower acidity. Roasting at 600°C was selected as the pre-treatment condition for both West Kentucky No. 13 and Fire Clay coarse refuse material. Over 40% of leaching recovery was achieved by roasting West Kentucky No. 13 material having a top particle size of 3 mm in the pilot scale operation using 1.2M sulfuric acid leaching at 75OC. Initial pilot scale testing involved continuous operation of the pilot plant for 94 hours. The leaching unit was operated at solid-to-liquid ratio of 1 to 10 (w/v) using 0.5M sulfuric acid solution at a temperature of 75°C. The continuous solvent extraction circuit utilized rougher and cleaner units with DEHPA and TBP as the extractants. An innovative stripping circuit was developed to accumulate the REE concentration in the stripping solution to a level above 600 ppm. A bleed stream from the recycled strip solution was treated using oxalic acid precipitation which produced a high grade rare earth oxalate. The oxalate product was roasted to remove the oxalate which produced a rare earth oxide product having a purity greater 90%. Due to high concentrations of contaminant ions in the pregnant leach solution (PLS), a modified flowsheet was developed that involved pre-concentration of the REEs using multiple stages of precipitation and redissolution. The advantage of this process was improved removal of contamination before the downstream purification process and a significant cost reduction relative to the circuit that utilized the solvent extraction process. The modified circuitry included processes involving leaching, multistage precipitation, redissolution, and oxalate precipitation followed by roasting of the oxalate product. The circuit produced a mixed REO that was 92.96% pure from the initial test. A detailed parametric test plan was carried out which involved varying key parameters including solids feed rate, acid flowrate, acid concentration, multistage precipitation pH, redissolution pH, oxalate precipitation dosage and pH. The response variables included REE recovery, contaminant recovery, REO product grade and overall chemical consumption. Test results indicated that the acid-to-solid ratio is the key parameter to leaching efficiency as performance deteriorated with an increase in solids concentration. The optimal pH determined for REE precipitation and redissolution was 6.5 and 2.5, respectively. Additional tests were conducted to further improve the flowsheet. Recirculating a portion of the PLS to the feed of the leach tanks improved the leaching performance by lowering the pH of the leaching system and reducing the contamination recovery by shortening the residence time. Moreover, the removal of Al prior to REE precipitation significantly reduced the oxalic acid consumption in the oxalate precipitation circuit. The modified circuit produced over 90% grade REO by weight from both West Kentucky No. 13 and Fire Clay coarse refuse material in pilot scale continuous test programs. A case analysis model was developed to project the REE and major contaminants concentration in each PLS stream based on the leaching condition, pH cut point, and oxalic acid dosage. A correlation was established using empirical and semi-empirical models. Using the models, chemical consumption required for each stage was predicted based on the projected performance of the hydrometallurgy circuit. After identifying the optimum conditions, validation tests were carried out for the treatment of both West Kentucky No. 13 and Fire Clay coarse refuse materials in the pilot plant. The actual circuit performance and chemical consumptions were very close to the model predictions. Other than the two coarse refuse sources, several secondary feedstocks were also tested in the pilot plant facility. A “heap leach” system was constructed using the coarse refuse material generated from cleaning the West Kentucky No. 13 seam coal. Using the two stage SX rougher and cleaner circuit, a concentrate with a grade >90% REO was produced while recovering >97% of the REEs from the heap leach PLS. Naturally generated acid mine drainage (AMD) from West Kentucky No.13 mine was processed using the multistage precipitation circuit in the pilot plant in a test conducted for a period of 32 hours. The final grade of the mix RE oxide produced from the AMD was 90.84% with an overall circuit recovery of 64%. The primary source of REE was the selective precipitation steps involving iron and aluminum rejection. The hydrophobic-hydrophilic separation (HHS) process was proven to effectively recover coal from fine waste materials. For REM recovery, the HHS process was able to produce concentrates at grades of approximately 1.8% REE on an ash basis; however, recovery values were typically low, <10%, under the optimal conditions determined in the laboratory-scale testing. Staged testing of the pilot-scale HHS process for coal recovery and semi-continuous laboratory testing for REM testing showed that a total concentration ratio of more than 15x was observed for the REM recovery process. A circuit simulation package was developed for REE extraction and purification using a spreadsheet-based platform (Microsoft Excel). The REESim circuit simulation package is configured to track the mass and volume flows of components passing through a series of unit operations specified and configured by the user. The mass rates can then be utilized by the user to determine important performance indicators such as product mass yields, concentrate purity levels, element-by-element recoveries, and so forth. The techno-economic analysis showed that the roasting and leaching operations were the most expensive capital items, each contributing approximately 30% to the total capital cost. One notable contributor to the high production costs was the low REE recovery observed in the pilot scale trials. The product basket price was shown to have a strong influence on the economic viability of the scenarios, with the scandium price being the most significant influencer. Operating cost was shown to be extremely sensitive to REE recovery, REE feed grade, and leaching acid consumption. An analysis of ten different scenarios for a 500 t/h commercial operation revealed that three were economically favorable, producing internal rates of return varying from 27.7% to 33.1% and payback periods of 4 to 5 years. The project successfully developed and demonstrated a process to recover REEs from coal and coal byproducts in a pilot-plant operation which consistently produced over 90% grade REO mix from varies types of feedstocks. Commercialization analysis showed that the technology readiness level successfully achieved TRL 6 at the end of the project and demonstrated the need and the potential for scaling the process to further advance the technologies toward the goal of providing a domestic supply of REEs at a commercial scale.

01 COAL, LIGNITE, AND PEAT↗

DOE OSTI2023

Onshore U.S. Carbon Pipeline Deployment: Siting, Safety, and Regulation

Carbon capture, utilization, and storage (CCUS) technology has significant potential to reduce greenhouse gas (GHG) emissions and mitigate the impact of climate change, particularly in hard to decarbonize industrial and commercial sectors. CCUS involves capturing carbon dioxide (CO 2 ) from industrial processes or power generation and utilizing it for other purposes, such as enhanced oil recovery (EOR), or storing the captured CO 2 underground. CCUS technology can reduce the environmental impact of continued fossil fuel use while smoothing the transition to a low-carbon economy. CCUS can create new economic opportunities, such as the development of new industries and job creation, and can enhance energy security by diversifying energy sources. For these reasons, enabling CCUS has become a key objective of the Biden-Harris administration’s clean energy policy and has received bipartisan support. Despite its environmental and economic potential, CCUS faces multiple barriers to widespread deployment. One of the main challenges is the high cost and technical difficulty of implementing and operating large-scale CCUS infrastructure. CCUS remains a relatively expensive way to reduce carbon emissions (e.g., compared to solar photovoltaic technology’s displacement of coal generation). Additionally, financial incentives and supportive policies like those enacted to support solar photovoltaic development, especially at the state level, are inconsistent or nonexistent, which can discourage investment in CCUS projects. There are also technical challenges associated with safe and secure underground CO 2 storage and the development of new carbon utilization technologies. Public opposition to various aspects of CCUS technologies, ranging from concerns that CCUS will extend reliance on fossil fuels to CCUS infrastructure being sited in disadvantaged communities, is a growing challenge. This paper focuses on another significant barrier to broad CCUS deployment: the need for considerable expansion of the dedicated land-based CO 2 pipeline network in the United States to meet CCUS goals and the unique regulatory challenges to its development. To reach carbon emissions targets in the United States by 2050, CCUS technology will need to be supported by tens of thousands of miles of CO 2 pipelines. Estimates range from a minimum of roughly 29,000 pipeline miles (according to a 2020 Great Plains Institute study) to 66,000 pipeline miles (as per a 2021 Princeton University–led study). As of October 2022, however, the U.S. Department of Transportation (U.S. DOT) reports fewer than 5,400 miles of U.S. pipelines carrying CO 2 . This deficit—and what it means for the prospect of moving substantially larger quantities of CO 2 from source to use or storage—threatens to stifle the development of CCUS projects and technologies identified as an important tool to meet emissions targets. The current regulatory landscape facing CO 2 pipeline development can best be described as uncertain. At the federal level, the U.S. DOT Pipeline and Hazardous Materials Safety Administration (PHMSA) oversees safety regulation of pipelines transporting hazardous materials, including CO 2 upon commencement of operation. However, PHMSA’s definition of CO 2 as “a fluid consisting of more than 90 percent CO 2 molecules compressed to a supercritical state” has not been updated since its 1991 addition to the Federal Register. Because CO 2 can be transported in a gaseous, liquid, or supercritical state (indeed, the physical state of CO 2 can fluctuate within a single pipeline due to environmental changes), doubts persist about the extent of PHMSA’s purview—and raise questions about what, if anything, states should do to address this apparent gap. PHMSA has begun a major revision of its existing rules, but the agency does not expect a first draft before 2024. Economic oversight of CO 2 pipelines is even less clear. The Federal Energy Regulatory Commission (FERC) and Surface Transportation Board (STB)—which regulate the rates of interstate oil/natural gas and non-energy pipelines, respectively—have both declined jurisdiction over interstate CO 2 pipelines. This presumably leaves economic regulation to state and/or local governments, but few if any states have the laws or resources in place to oversee just and reasonable rates. Further, the interstate nature of CO 2 pipeline development creates questions around how different states should align their rate-making decisions. Onshore U.S. Carbon Pipeline Deployment: Siting, Safety, and Regulation Currently, regulatory responsibilities regarding CO 2 pipeline siting and permitting fall to state and local governments. The variety of laws and regulations across the country, however, creates a maze of requirements for pipeline developers to navigate. To secure necessary permits, most states require pipeline companies to be “common carriers” that provide transport service to the public at uniform rates. However, the specific definition of that term varies. Some states require clear evidence that a pipeline services the public, while others automatically deem any pipeline company transporting energy products or hazardous materials to be a “common carrier”—with little consideration for accessibility to third parties. Other states have eschewed common-carrier terminology entirely, placing private and publicly accessible pipelines on equal footing. Much like the variation in common-carrier requirements, laws governing eminent domain authority to secure rights-of-way (ROW) to commence construction on a planned pipeline route differ by state. Several states have no laws or rules governing CO 2 pipelines. In addition to creating questions about whether long-standing rules for other pipelines (e.g., natural gas or petroleum products) apply to CO 2 , this policy vacuum leaves local governments as the sole authority over sections of pipe within their boundaries. With dozens of counties along a given route, the probability of inconsistent regulation of the same pipeline is significant. Even in states with CO 2 pipeline laws in place, local regulatory attempts to address rising concerns over pipeline routing and safety have triggered lawsuits by pipeline companies seeking to delimit areas of federal, state, and local government responsibility. Meanwhile, legislators across the country have introduced bills to restrict the application of eminent domain to CO 2 pipeline projects, which could threaten a key means of securing ROW that companies cannot secure through negotiation with landowners. Taken separately, any of these regulatory issues—the narrow federal definition of CO 2 , FERC’s and STB’s decisions that CO 2 pipelines are not within their jurisdiction, and the considerable variation in state and local governments’ laws regulating CO 2 pipeline technologies—are extremely difficult to resolve. Adding the required scale of CO 2 pipeline expansion and the currently identified narrow window of time in which to reach climate target goals, the task becomes even more difficult—and raises a host of urgent questions for regulators. How should CO 2 be defined in federal regulations to ensure consistent safety standards across the country? What is the potential impact radius of a CO 2 pipeline rupture, and how should that inform local emergency response? In the absence of centralized federal oversight, what should state legislatures do to increase alignment for interstate CO 2 pipeline projects? This paper intends to serve as a primer for regulators and stakeholders who seek to better understand the regulatory challenges and opportunities facing this critical infrastructure.

42 ENGINEERING↗