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All sourcesNASA NTRSDOE OSTI
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 OSTI2022

Cosmogenic nuclide and solute flux data from central Cuban rivers emphasize the importance of both physical and chemical mass loss from tropical landscapes

We use 25 new measurements of in situ produced cosmogenic 26 Al and 10 Be in river sand, paired with estimates of dissolved load flux in river water, to characterize the processes and pace of landscape change in central Cuba. Long-term erosion rates inferred from 10 Be concentrations in quartz extracted from central Cuban river sand range from 3.4–189 Mg km –2 yr –1 (mean 59, median 45). Dissolved loads (10–176 Mg km –2 yr –1 ; mean 92, median 97), calculated from stream solute concentrations and modeled runoff, exceed measured cosmogenic- 10 Be-derived erosion rates in 18 of 23 basins. This disparity mandates that in this environment landscape-scale mass loss is not fully represented by the cosmogenic nuclide measurements. The 26 Al / 10 Be ratios are lower than expected for steadystate exposure or erosion in 16 of 24 samples. Depressed 26 Al/ 10 Be ratios occur in many of the basins that have the greatest disparity between dissolved loads (high) and erosion rates inferred from cosmogenic nuclide concentrations (low). Depressed 26 Al/ 10 Be ratios are consistent with the presence of a deep, mixed, regolith layer providing extended storage times on slopes and/or burial and extended storage during fluvial transport. River water chemical analyses indicate that many basins with lower 26 Al/ 10 Be ratios and high 10 Be concentrations are underlain at least in part by evaporitic rocks that rapidly dissolve. Our data show that when assessing mass loss in humid tropical landscapes, accounting for the contribution of rock dissolution at depth is particularly important. In such warm, wet climates, mineral dissolution can occur many meters below the surface, beyond the penetration depth of most cosmic rays and thus the production of most cosmogenic nuclides. Our data suggest the importance of estimating solute fluxes and measuring paired cosmogenic nuclides to better understand the processes and rates of mass transfer at a basin scale.

54 ENVIRONMENTAL SCIENCES↗
NASA NTRS1984

Spatial variation analyses of Thematic Mapper data for the identification of linear features in agricultural landscapes

A need exists for digitized information pertaining to linear features such as roads, streams, water bodies and agricultural field boundaries as component parts of a data base. For many areas where this data may not yet exist or is in need of updating, these features may be extracted from remotely sensed digital data. This paper examines two approaches for identifying linear features, one utilizing raw data and the other classified data. Each approach uses a series of data enhancement procedures including derivation of standard deviation values, principal component analysis and filtering procedures using a high-pass window matrix. Just as certain bands better classify different land covers, so too do these bands exhibit high spectral contrast by which boundaries between land covers can be delineated. A few applications for this kind of data are briefly discussed, including its potential in a Universal Soil Loss Equation Model.

Pelletier, R. E.↗
DOE OSTI2025

A hybrid neural architecture: Online attosecond x-ray characterization

The emergence of high-repetition-rate x-ray free-electron lasers (XFELs), such as SLAC’s LCLS-II, serves as our canonical example for autonomous controls that necessitate high-throughput diagnostics paired with streaming computational pipelines capable of single-shot analysis with extremely low latency. We present the deterministic characterization with an integrated parallelizable hybrid resolver architecture, a hybrid machine learning framework designed for fast, accurate analysis of XFEL diagnostics using angular streaking-based sinogram images. This architecture integrates convolutional neural networks and bidirectional long short-term memory models to denoise input, identify x-ray sub-spike features, and extract sub-spike relative delays with sub-30 attosecond temporal resolution. Deployed on low-latency hardware, it achieves over 10 kHz throughput with 168.3 μs inference latency, indicating scalability to 14 kHz with field-programmable gate array integration. By transforming regression tasks into classification problems and leveraging optimized error encoding, we achieve high precision with low-latency performance that is critical for real-time streaming event selection and experimental control feedback signals. This represents a key development in real-time control pipelines for next-generation autonomous science, generally, and high repetition-rate x-ray experiments in particular.

Accelerator Physics (physics.acc-ph)↗
NASA NTRS2004

Extraction of Martian valley networks from digital topography

We have developed a novel method for delineating valley networks on Mars. The valleys are inferred from digital topography by an autonomous computer algorithm as drainage networks, instead of being manually mapped from images. Individual drainage basins are precisely defined and reconstructed to restore flow continuity disrupted by craters. Drainage networks are extracted from their underlying basins using the contributing area threshold method. We demonstrate that such drainage networks coincide with mapped valley networks verifying that valley networks are indeed drainage systems. Our procedure is capable of delineating and analyzing valley networks with unparalleled speed and consistency. We have applied this method to 28 Noachian locations on Mars exhibiting prominent valley networks. All extracted networks have a planar morphology similar to that of terrestrial river networks. They are characterized by a drainage density of approx.0.1/km, low in comparison to the drainage density of terrestrial river networks. Slopes of "streams" in Martian valley networks decrease downstream at a slower rate than slopes of streams in terrestrial river networks. This analysis, based on a sizable data set of valley networks, reveals that although valley networks have some features pointing to their origin by precipitation-fed runoff erosion, their quantitative characteristics suggest that precipitation intensity and/or longevity of past pluvial climate were inadequate to develop mature drainage basins on Mars.

Stepinski, T. F.↗
DOE OSTI2024

Targeted Rare Earth Element Extraction from Mine Drainage Treatment Solids Informed by Advanced Characterization

In support of a clean energy transition in the U.S., National Energy Technology Laboratory (NETL) has collaborated with staff at Hedin Environmental and students at the University of Pittsburgh to characterize critical mineral content and recovery potential from acid mine drainage treatment solids (AMD solids). AMD solids in Appalachia are an unconventional feedstock of rare earth elements (REEs), with potential of suppling 1,102 tons REE/year. To inform recovery efforts, select AMD solids were examined using synchrotron microprobe analysis in conjunction with USGS-developed geochemical modeling to indicate likely phases hosting critical minerals (REE, Co, Ni, etc.) and associated metals . More than 100 AMD solids were collected from 94 passive AMD treatment systems in Pennsylvania, where limestone aggregates are used for acidity neutralization. As pH increases, dissolved metals and critical minerals in AMD are attenuated as surface coatings on limestone. The collected AMD solids contained up to 2000 mg/kg REE, up to 13,000 mg/kg transition metals (Co, Ni, Zn) and up to 440 mg/kg Li. Regardless of the diverse chemical compositions from AMD solids (Al-rich, Mn-rich, or Al,Fe,Mn-rich), REEs were mostly associated with Al and Mn (hydr)oxides, while select heavy REEs (e.g., Gd, Dy) were co-localized with Fe (hydr)oxides. Co and Ni have different distribution zones, while both co-localized with Mn (hydr)oxides. Based on this characterization, NETL developed a patent-pending innovative step-leaching protocol, “Targeted Rare Earth Extraction (TREE)” to effectively recover up to 90% REE and 60% Co in separate steps. In addition, select post-TREE solid residuals (purified Al oxides, or Mn oxides) can be further developed into functional materials (e.g., lithium and CO2 sorbents) needed for green energy transition and carbon management. This characterization-informed approach as well as TREE processing from AMD solids can be used for other legacy wastes (e.g., coal ash, oil and gas drill cutting, mine tailings), and offers an opportunity to transform waste streams into environmental and economic assets that meet U.S. Department of Energy and U.S. Environmental Protection Agency goals.

characterization and extraction of rare earth elem↗
DOE OSTI2025

Geochemical Phosphorus Sequestration in Tundra Soils Impedes Delivery of Bioavailable Phosphorus to the Kuparuk River, Alaska, USA: Implications for the Broader Arctic Region

Long-term river monitoring of the Kuparuk River (North Slope, Alaska, USA) confirms significant increases in solutes that are indicative of active layer thickening due to thawing permafrost. However, there is no evidence of an increase in total dissolved phosphorus (TDP) or soluble reactive phosphorus (SRP), the nutrient that limits primary production in this and similar rivers in the region. Here, we show that Mehlich-3 extractable iron (Fe) and aluminum (Al) in active layer soils impart high P geochemical sorption capacities across a range of landscape features that we would expect to promote lateral movement of water and solutes to headwater streams in our study watershed. Reanalysis of a recently published pan-Arctic soils database that includes active layer and permafrost soil samples suggests that this high P sorption capacity could be common in other parts of the Arctic region. We conclude that soil minerals enhance P retention on hillslopes and propose pedogenic secondary Fe and Al minerals may continue to retain P in these soils and limit biological productivity in the adjacent river even as active layer thickening increases potential P mobility in the watershed. We suggest that similar interactions may occur in other areas of the Arctic where comparable geochemical conditions prevail.

Sutor, Frederick W. [Univ. of Vermont, Burlington,↗
DOE OSTI2022

DeepCare: Improving Patient Care using Deep Learning on Electronic Health Records

Coordinating patient care using electronic health records (EHR) data presents an exciting but formidable opportunity in data extraction, analysis and modeling. Traditional methods use a manual feature driven approach to model patients with age, family history and symptoms to predict disease outcomes. We propose a novel approach to model patients based on their streaming electronic health records data combined with information from medical knowledge bases, which has been gained over years of medical research. Using a combination of representation learning and long short term memory (LSTM) networks we plan to model patient evolution over time, leading to more accurate and individualized predictive models for patient’s diseases. Our approach will be transformative in providing critical decision support for patient care, enabling accurate understanding and evolution of diseases in patients.

60 APPLIED LIFE SCIENCES↗
NASA NTRS2009

Jet Noise Modeling for Suppressed and Unsuppressed Aircraft in Simulated Flight

This document describes the development of further extensions and improvements to the jet noise model developed by Modern Technologies Corporation (MTC) for the National Aeronautics and Space Administration (NASA). The noise component extraction and correlation approach, first used successfully by MTC in developing a noise prediction model for two-dimensional mixer ejector (2DME) nozzles under the High Speed Research (HSR) Program, has been applied to dual-stream nozzles, then extended and improved in earlier tasks under this contract. Under Task 6, the coannular jet noise model was formulated and calibrated with limited scale model data, mainly at high bypass ratio, including a limited-range prediction of the effects of mixing-enhancement nozzle-exit chevrons on jet noise. Under Task 9 this model was extended to a wider range of conditions, particularly those appropriate for a Supersonic Business Jet, with an improvement in simulated flight effects modeling and generalization of the suppressor model. In the present task further comparisons are made over a still wider range of conditions from more test facilities. The model is also further generalized to cover single-stream nozzles of otherwise similar configuration. So the evolution of this prediction/analysis/correlation approach has been in a sense backward, from the complex to the simple; but from this approach a very robust capability is emerging. Also from these studies, some observations emerge relative to theoretical considerations. The purpose of this task is to develop an analytical, semi-empirical jet noise prediction method applicable to takeoff, sideline and approach noise of subsonic and supersonic cruise aircraft over a wide size range. The product of this task is an even more consistent and robust model for the Footprint/Radius (FOOTPR) code than even the Task 9 model. The model is validated for a wider range of cases and statistically quantified for the various reference facilities. The possible role of facility effects will thus be documented. Although the comparisons that can be accomplished within the limited resources of this task are not comprehensive, they provide a broad enough sampling to enable NASA to make an informed decision on how much further effort should be expended on such comparisons. The improved finalized model is incorporated into the FOOTPR code. MTC has also supported the adaptation of this code for incorporation in NASA s Aircraft Noise Prediction Program (ANOPP).

Stone, James R.↗
DOE OSTI2024

A Simulated Evaluation of Powder Flowability Through a Partially Obstructed Consumable in Blown Powder Directed Energy Deposition Systems

Abstract In the interest of continued industrialization of metal additive manufacturing in modern production environments, cost is often referenced as a primary deterrent to new adopters. Conventional economic models for additive systems, processes, and supply chains often focus on specific process applications with little generalizability, or they neglect significant costs associated with production such as machine maintenance and consumable part replacement. Compounding the latter issue are substantial knowledge gaps in consumable part wear characterization for additive and other convergent manufacturing systems. In coaxial blown powder directed energy deposition systems, gas atomized metal powder is wasted during material deposition at a rate that is partly dependent on present wear phenomena in a consumable nozzle housed in the cladding head assembly. The price and lead time required to replace the nozzle incentivizes its reuse even when visibly worn. Often this initiates a process quality decline in the form of underbuilt geometry and internal defects due to losses in powder catchment efficiency. While depositing H13 steel using a hybrid manufacturing machine tool equipped with such a deposition system, a unique partial clog with a bridge-like structure formed at the consumable nozzle exit when supporting argon gas flows failed mid-process. To further understand coaxial multi-phase powder flow in the event of support gas failure, a computational fluid dynamics simulation is tailored to relevant process parameters, H13 powder material profile, and machine operator observations collected after the incident. The resulting differences in powder flow compared to control gas flow parameters is presented and discussed. The powder flowability and performance of the clogged nozzle is then assessed by using an optical profilometer to extract the profile of the clog and recreate the clog geometry within the simulation environment. In past work this simulation has been experimentally validated for a 316L steel powder material profile and used specifically for analyzing powder stream geometry and catchment efficiency. After the initial powder flow characterization, the clog is removed, and the nozzle is reprofiled. After removing the obstructing clog, the newly unobstructed nozzle geometry, the original off the shelf nozzle geometry, and additional nozzle profiles exploring different consumable refurbishment strategies are reevaluated in the simulation. Powder catchment efficiency for all variant nozzle geometries and relevant flow variables are compared and discussed, along with potential mitigation strategies for optimizing powder flowability with worn consumables. This work expands on the known morphology of blown powder obstructions and wear defects present in consumable coaxial nozzles while discussing pragmatic simulation driven responses to unanticipated subsystem failure in hybrid manufacturing machining platforms.

DeWitte, Lisa↗
DOE OSTI2021

HAIMOS Ensemble Forecasts for Intra-day and Day- Ahead GHI, DNI and Ramps

The objective of this research is to develop a hybrid physics-based/data-driven forecast model to improve direct normal and global horizontal irradiance (DNI and GHI) prediction for horizons ranging from 1 to 72 hours. Project objectives also address key gaps in state-of-the-art solar forecasting: accurate probabilistic solar forecasts and the forecasting of large irradiance ramps (ramp onset and magnitude). The proposed model ensembles Numerical Weather Prediction (NWP) forecasts, determinist physics-based algorithms, and new-generation cloud cover products (high-resolution rapid refresh satellite images and Large Eddy Simulations). The result is the Hybrid Adaptive Input Model Objective Selection (HAIMOS) ensemble model. HAIMOS blends state of the art machine learning methodologies with physics-based models for cloud cover and cloud optical depth forecasts. The technical activities followed a two-pronged strategy. First, the preprocessing of data, the selection of inputs to the nonlinear approximators, the type of approximator and objective functions, and post-processing ensembling techniques included in HAIMOS were all optimized adaptively to find the best model for a specific goal (reduce DNI/GHI forecast error, improve the prediction of ramp onset, etc.). Second, a large effort was put in improving cloud identification and the forecast of cloud cover and cloud optical depth. To this end, new-generation cloud parametrization products were developed in this work. These include improved algorithms to assist in cloud identification, cloud classification and cloud parametrization from satellite images – three key factors in the accuracy of 1 to 6-hours irradiance forecasts and prediction of ramp onset. Furthermore, we also included cloud information extracted from high resolution rapid refresh satellite images (GOES-16) and Large Eddy Simulations (LES). LES was used to model the atmosphere in detail over locations of interest and produce cloud optical depth forecasts. Once these data streams were validated, they were used as input data to the HAIMOS forecast. The model was developed using data from several climatologically distinct locations with potential for high solar penetration. In the last year of the project, we conducted a validation campaign according to the guidelines stipulated by the Topic Area 1 project as described in the FOA. This effort brings, for the first time, proven machine-learning methodologies for generating state-of-the-art solar forecasts interweaved with detailed physics-based models for cloud detection, and cloud optical depth forecasts. HAIMOS will generate accurate irradiance probabilistic forecast to assist in reducing solar generation prediction error. Globally optimized solar forecast models are more likely to impact solar energy stakeholders. The goal of this project was to increase the state-of-the-art forecast skill from their present values of 10 to 35%. At the end of the project, we achieved between 30% and 50% forecast skill across a wide range of horizons for both GHI and DNI.

14 SOLAR ENERGY↗
DOE OSTI2023

Functionalized Mesoporous Carbon Materials for Effective Recovery of Rare Earth Elements from NdFeB Magnet Scrap

The increasing demand and high dependence on international supplies of rare earth elements (REEs) have prompted the US to explore alternative resources and sustainable technologies for domestic REE production. One potential resource is the secondary electronic and industrial wastes at DoD complexes and across the US. These hazardous wastes require high costs for the maintenance and remediation, but their high-REE contents offer unique opportunities for REE recovery. Current hydrometallurgical technologies for REE extraction are energy intensive and costly, with low REE recovery efficiency and the generation of hazardous secondary wastes. Thus, it is crucial to develop high efficiency and environmental-friendly technologies for REE extraction and recovery from the secondary wastes. This project aims to develop novel functionalized mesoporous carbon materials for effective recovery of REEs from NdFeB magnet scrap. The proposed novel functionalized materials will be applied in a solid-liquid separation platform that can effectively extract, recover and separate REEs from NdFeB magnet scrap (the current focus), but also from other secondary electronic/industrial wastes in the future, minimize the generation of secondary hazardous wastes, and offset the management costs for existing waste streams.

36 MATERIALS SCIENCE↗
NASA NTRS1996

Spectral Quantitation Of Hydroponic Nutrients

Instrument continuously monitors hydroponic solution by use of absorption and emission spectrometry to determine concentrations of principal nutrients, including nitrate, iron, potassium, calcium, magnesium, phosphorus, sodium, and others. Does not depend on extraction and processing of samples, use of such surrograte parameters as pH or electrical conductivity for control, or addition of analytical reagents to solution. Solution not chemically altered by analysis and can be returned to hydroponic process stream after analysis.

Schlager, Kenneth J.↗
DOE OSTI2024

Hydrokinetic tidal energy resource assessment following international electrotechnical commission guidelines

Marine renewable energy can be used as a viable energy source to alleviate the impact of the climate crisis and have a carbon-free electricity sector in the future. Especially the energetic tidal streams are an attractive source of clean energy due to the periodic occurrence of high tidal flows daily. However, before any deployment of tidal turbine farms, it is essential to perform a resource assessment depending on the scope and scale of the project. Here, the International Electrotechnical Commission has developed a technical standard for assessing the tidal stream resource "IEC 62600-201 TS" to aid in this effort: determine a particular site's feasibility and perform the project layout design. In this study, we implemented and validated a high-resolution three-dimensional numerical model and provided results following the IEC TS for a project layout design in a highly energetic tidal channel, Tacoma Narrows of Puget Sound, in the State of Washington, USA. Implementation of the guidelines has helped adequately identify the undisturbed theoretical and technical resources with less bias, where the latter included energy extraction from the flow field arranging a hypothetical tidal energy converter (TEC) array. Also, following the standard, we carefully assessed the changes to channel flow properties from TECs, such as the kinetic energy flux and annual energy production (AEP), to provide the detailed information required for a larger project layout design. Ultimately, this work has shown the important role of IEC TS in tidal stream resource assessment, which can simultaneously act as a benchmark for other studies worldwide.

13 HYDRO ENERGY↗
DOE OSTI2024

Out-of-Distribution Detection and Radiological Data Monitoring Using Statistical Process Control

Abstract Machine learning (ML) models often fail with data that deviates from their training distribution. This is a significant concern for ML-enabled devices as data drift may lead to unexpected performance. This work introduces a new framework for out of distribution (OOD) detection and data drift monitoring that combines ML and geometric methods with statistical process control (SPC). We investigated different design choices, including methods for extracting feature representations and drift quantification for OOD detection in individual images and as an approach for input data monitoring. We evaluated the framework for both identifying OOD images and demonstrating the ability to detect shifts in data streams over time. We demonstrated a proof-of-concept via the following tasks: 1) differentiating axial vs. non-axial CT images, 2) differentiating CXR vs. other radiographic imaging modalities, and 3) differentiating adult CXR vs. pediatric CXR. For the identification of individual OOD images, our framework achieved high sensitivity in detecting OOD inputs: 0.980 in CT, 0.984 in CXR, and 0.854 in pediatric CXR. Our framework is also adept at monitoring data streams and identifying the time a drift occurred. In our simulations tracking drift over time, it effectively detected a shift from CXR to non-CXR instantly, a transition from axial to non-axial CT within few days, and a drift from adult to pediatric CXRs within a day—all while maintaining a low false positive rate. Through additional experiments, we demonstrate the framework is modality-agnostic and independent from the underlying model structure, making it highly customizable for specific applications and broadly applicable across different imaging modalities and deployed ML models.

Zamzmi, Ghada↗
DOE OSTI2023

Model Agnostic Bayesian Framework for Online Anomaly/Event Detection in PMU Data

Phasor measurement units (PMU) are integral to the modernization and automation plan of the electric power industry. A PMU data signature contains system-level events (e.g., faults, generation/load change, etc.) and any measurement/device-related errors. Therefore, the reliable and resilient operation of power systems is equivalent to the quality of the PMU data and the situation awareness provided by its data signature. Despite recent progress, current state-of-the-art methods are not fool-proof and have certain limitations tracing an error/abnormality to sensor sub-components and grid systems. This is because of technical challenges imposed by the scarcity of the labeled information, loss of data quality, and non-stationarity of data. In this paper, we consider the online PMU data stream as an output of a stochastic process and pose the anomaly/event detection as a changepoint detection problem dealing with detecting parameter changes in the underlying stochastic processes. The proposed model-agnostic framework relies on: (a) feature extraction utilizing the minimum volume enclosing ellipsoids (MVEE) method from raw PMU observations and (b) a Bayesian framework of changepoint detection. The validity of the proposed methodology is discussed through numerical experiments on real-world utility-scale PMU data.

Hossain, Ramij Raja↗
DOE OSTI2022

Technoeconomic evaluation of recent process improvements in production of sugar and high-value lignin co-products via two-stage Cu-catalyzed alkaline-oxidative pretreatment

Abstract Background A lignocellulose-to-biofuel biorefinery process that enables multiple product streams is recognized as a promising strategy to improve the economics of this biorefinery and to accelerate technology commercialization. We recently identified an innovative pretreatment technology that enables of the production of sugars at high yields while simultaneously generating a high-quality lignin stream that has been demonstrated as both a promising renewable polyol replacement for polyurethane applications and is highly susceptible to depolymerization into monomers. This technology comprises a two-stage pretreatment approach that includes an alkaline pre-extraction followed by a metal-catalyzed alkaline-oxidative pretreatment. Our recent work demonstrated that H 2 O 2 and O 2 act synergistically as co-oxidants during the alkaline-oxidative pretreatment and could significantly reduce the pretreatment chemical input while maintaining high sugar yields (~ 95% glucose and ~ 100% xylose of initial sugar composition), high lignin yields (~ 75% of initial lignin), and improvements in lignin usage. Results This study considers the economic impact of these advances and provides strategies that could lead to additional economic improvements for future commercialization. The results of the technoeconomic analysis (TEA) demonstrated that adding O 2 as a co-oxidant at 50 psig for the alkaline-oxidative pretreatment and reducing the raw material input reduced the minimum fuel selling price from $1.08/L to $0.85/L, assuming recoverable lignin is used as a polyol replacement. If additional lignin can be recovered and sold as more valuable monomers, the minimum fuel selling price (MFSP) can be further reduced to $0.73/L. Conclusions The present work demonstrated that high sugar and lignin yields combined with low raw material inputs and increasing the value of lignin could greatly increase the economic viability of a poplar-based biorefinery. Continued research on integrating sugar production with lignin valorization is thus warranted to confirm this economic potential as the technology matures.

09 BIOMASS FUELS↗
DOE OSTI2023

Use of Stable Mercury Isotopes to Assess Mercury and Methylmercury Transformation and Transport across Critical Interfaces from the Molecular to the Watershed Scale (Final Report)

This project titled “Use of Stable Mercury Isotopes to Assess Mercury and Methylmercury Transformation and Transport across Critical Interfaces from the Molecular to the Watershed Scale” represents a collaborative effort between the University of Michigan (Jason Demers, PI) and Oak Ridge National Laboratory (Scott Brooks, co-I). Much has been learned about mercury (Hg) cycling in stream ecosystems, and East Fork Poplar Creek (EFPC) in particular, through decades of previous research. Nevertheless, some of the most fundamental questions regarding the sources of bioavailable Hg and its transformation to toxic methylmercury (MeHg) have remained unanswered. These fundamental questions include: (1) what are the sources and biogeochemical processes that lead to the input of dissolved Hg to stream water across critical subsurface interfaces within stream ecosystems, and EFPC in particular? and (2) what are the sources and biogeochemical processes that control the production and fate of bioaccumulative MeHg within stream ecosystems, and in EFPC in particular? To address these fundamental questions, our project aimed to couple laboratory experiments and field observations, both utilizing natural abundance Hg stable isotope techniques, to identify the processes responsible for generating mobile, bioavailable dissolved Hg from recalcitrant legacy sources within critical subsurface zones (e.g., streambed hyporheic zone, riparian floodplain subsurface). We used the isotopic signature of this bioavailable dissolved Hg to track its mobilization across these critical interfaces in order to link diffuse subsurface sources of dissolved Hg with increases in surface water dissolved Hg flux measured at the watershed scale. Additionally, our research aimed to determine the isotopic composition of MeHg within these same critical subsurface zones. We directly assessed the isotopic composition of MeHg within biota in order to gain insight into which subsurface sources of inorganic Hg and toxic MeHg are available for bioaccumulation within the EFPC ecosystem. Net fluxes of dissolved Hg along the flow path of EFPC were shown to vary spatially and temporally. In the Upper EFPC, within the Y12 boundary, stream water flux of dissolved Hg consistently decreased between the outfall and the downstream boundary of Y12 (57% ± 29%, 1SD). Within the Upper EFPC, an assessment of Hg isotopic composition suggested that losses were strongly reaction-driven, although isotopic diagnostics did not conform to any known processes. Downstream of Y12, in the upper reach of the Lower EFPC, dissolved Hg fluxes tended to increase during the dormant season (net gain of 11-120%), and decrease during the growing season (net loss of 23% +/- 18%, 1SD). In the downstream-most reach of Lower EFPC, dissolved Hg fluxes increased by 12-108% in 9 out of 10 monthly assessments. Overall, diffuse fluxes from the non-Y12 watershed accounted for 34% (+/- 17%, 1SD) of all dissolved Hg exported during base flow. Within Lower EFPC, an assessment of Hg isotopic composition was consistent with the contribution of diffuse Hg inputs from high-concentration hotspots within riparian floodplains and streambed hyporheic pore water. To investigate remobilization of recalcitrant Hg from legacy sediment sources, we developed procedures that coupled isotopic analysis with sequential extractions of streambed sediment. We found that the proportion of weakly-bound Hg within EFPC streambed sediment was relatively small, but could still account for a large proportion of the annual flux of dissolved Hg from EFPC. These sequential extractions also showed that this weakly-bound Hg fraction could be replenished from the much larger fraction of recalcitrant Hg in sediment. The isotopic composition of these weakly-bound and remobilized recalcitrant Hg fractions within the sediment was consistent with high-concentration dissolved Hg hotspots within hyporheic pore water. Thus, this research provided novel evidence that legacy mercury sources within streambed sediment could provide an ongoing contribution of dissolved Hg to surface waters. Finally, we developed new methods for the direct determination of the MeHg isotopic composition of organisms, which allowed a more direct evaluation of inorganic Hg and MeHg sources accumulating in the food web. We found that fish and aquatic invertebrates in both EFPC and a regional background site obtained inorganic Hg and MeHg from multiple isotopically distinct sources, including sediment, suspended particulates, and periphyton. Photodemethylation was found to be an important reaction influencing MeHg dynamics at both sites. However, the balance of microbial methylation and demethylation processes differed between the two streams, with fractionation resulting from methylation and demethylation processes being relatively in balance within the regional background site, whereas microbial methylation appeared to be dominant over microbial demethylation within the EFPC ecosystem. Broadly, the application of Hg isotopic analysis in this study led to numerous novel insights regarding the biogeochemical cycling of Hg in stream ecosystems. This research project promoted the development of two new approaches, including the coupling of sequential extractions with Hg isotopic analysis to assess remobilization of recalcitrant Hg within sediments, and a new method for the isotopic analysis of MeHg isolated from environmental samples. Both of these efforts represent advances in capacity for the field of mercury isotopic analysis and environmental assessment. Overall, this study demonstrates that the application of Hg stable isotope techniques continues to provide new insights into the biogeochemical cycling of Hg in complex aquatic environments, both within the EFPC and beyond.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗