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DOE OSTI2013

Recent Results of the Investigation of a Microfluidic Sampling Chip and Sampling System for Hot Cell Aqueous Processing Streams

A Fuel Cycle Research and Development project has investigated an innovative sampling method that could evolve into the next generation sampling and analysis system for metallic elements present in aqueous processing streams. Initially sampling technologies were evaluated and microfluidics sampling chip technology was selected and tested. A conceptual design for a fully automated microcapillary-based system was completed and a robotic automated sampling system was fabricated. The mechanical and sampling operation of the completed sampling system was investigated. In addition, the production of a less expensive, mass produced sampling chip was investigated to avoid chip reuse thus increasing sampling reproducibility/accuracy. The microfluidic-based robotic sampling system’s mechanical elements were tested to ensure analytical reproducibility and the optimum robotic handling of microfluidic sampling chips.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2013

Recent results of the investigation of a micro-fluidic sampling chip and sampling system for hot cell aqueous processing streams

A Fuel Cycle Research and Development project has investigated an innovative sampling method that could evolve into the next generation sampling and analysis system for metallic elements present in aqueous processing streams. Initially sampling technologies were evaluated and micro-fluidic sampling chip technology was selected and tested. A conceptual design for a fully automated microcapillary-based system was completed and a robotic automated sampling system was fabricated. The mechanical and sampling operation of the completed sampling system was investigated. Different sampling volumes have been tested. It appears that the 10 μl volume has produced data that had much smaller relative standard deviations than the 2 μl volume. In addition, the production of a less expensive, mass produced sampling chip was investigated to avoid chip reuse thus increasing sampling reproducibility/accuracy. The micro-fluidic-based robotic sampling system's mechanical elements were tested to ensure analytical reproducibility and the optimum robotic handling of micro-fluidic sampling chips. (authors)

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2020

Consequence Analysis of Residual Water in a Storage Canister - 20484

Recent observations from projects sponsored under the DOE-Nuclear Energy Spent Fuel and Waste Disposition campaign show that residual free water, well above the 0.4 gm-moles that correspond to a 3 torr rebound pressure after a 30-minute hold following prototypic drying, may remain within SNF canisters used for long-term dry storage. Specifically, experimental observations in an Integrated Research Project showed subzero temperatures and a local pocket of frozen water in a mockup fuel assembly subjected to an industry practiced drying process. In gas sampling and analysis from the High Burnup (HBU) Demonstration project, using a fully loaded and dried SNF canister, indicated presence of 100 g of residual water had remained in the canister. The effects of residual water in terms of potential adverse impacts on the condition of the SNF and the canister internals during long-term dry storage has been rigorously evaluated to address inadvertent residual water contents. The impact of residual water on the fuel and canister internals, with a focus on the oxidation of the cladding and of postulated exposed (breached-clad) fuel, were evaluated using an integrated set of time-dependent environmental conditions with semi-empirical materials oxidation models. An 'integration model,' with coupled sub-models, developed and previously used by the Center for Nuclear Waste Regulatory Analysis (CNWRA), was applied and expanded with improved sub-models for water radiolysis, and for cladding and fuel oxidations. Cladding oxidation models for various alloys were developed using the rate constants for various cladding alloys in the dry storage temperature range. A burnup-dependent fuel oxidation model was developed; it accounted for inhibition effect of fission products on fuel oxidation rates. The potential for extension of the initial breach flaw (1 mm hole) was evaluated by two separate mechanics criteria. In the first case, a critical cladding strain criterion was used. In the second case, a critical stress intensity was used to evaluate stability of a planar axial flaw postulate. A failure condition exists when a sufficient amount of fuel oxidation (at the postulated breached-clad location) causes fuel pellet swelling to load the cladding to meet a mechanics criterion for flaw extension. The integration model's results provide the following insights. The radiolysis-generated oxygen is consumed with a partitioning between the cladding and the fuel. The extent of cladding oxidation is no more than 2 μm additional consumption of the cladding metal even with 10 moles of residual water, indicating that changes in cladding conditions due to water are expected to be negligible. The conditions for cladding failure (breach opening size extension) directly correlates with the extent of fuel oxidation. Fuel oxidation significant to extend the breach could occur even with 5.5 moles of residual water. The results indicate that fuel oxidation vis-a-vis cladding oxidation is more likely under a higher radiation field, i.e., when radiolytic decomposition of the residual water occurs in few years compared to several decades, and that the conditions to cause failure are increased with fuel and cladding temperatures approaching the peak storage temperature limit of 400 deg. C. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2026

Exploring the potential of using L-Band InSAR for the mapping of flooded vegetation in tropical wetlands

Wetlands play a critical role in global water and carbon cycles, yet monitoring their water extent remains difficult, particularly beneath dense vegetation. SAR-based techniques such as backscatter thresholding are limited by complex scattering mechanisms, while fully polarimetric SAR (PolSAR) data capable of detecting doublebounce scattering remain scarce. To address these challenges, this study evaluates the potential of Interferometric SAR (InSAR) for mapping water surfaces beneath vegetation, termed flooded vegetation, using the Atrato floodplain in Colombia as a case study. We develop an automated workflow combining InSAR fringe detection with local phase homogeneity analysis and random sampling of processing parameters to generate probabilistic flooded vegetation maps. Applied to ALOS PALSAR-1 L-band image pairs from 2007–2011, the workflow captures seasonal fluctuations in flooded extent ranging from 500 to 1,500 km2. Compared to other L-band SAR inundation products, the InSAR-based maps identify broader flooded areas, with ~70% agreement in pairwise comparisons. Around 84% of detections align with existing wetland inventories and seasonal changes correspond with regional hydrological indicators, including terrestrial water storage anomalies and water gauge measurements. PolSAR analysis shows that InSAR complements backscatter-based methods by detecting inundation in areas with weak double-bounce signals. These findings suggest that combining InSAR with backscatter-based methods can improve detection of flooded vegetation, which is especially relevant for the upcoming NISAR mission that will offer frequent global L-band observations.

Coastal inundation↗

DOE OSTI2014

Microfluidic-Based Robotic Sampling System for Radioactive Solutions

A novel microfluidic based robotic sampling system has been developed for sampling and analysis of liquid solutions in nuclear processes. This system couples the use of a microfluidic sample chip with a robotic system designed to allow remote, automated sampling of process solutions in-cell and facilitates direct coupling of the microfluidic sample chip with analytical instrumentation. This system provides the capability for near real time analysis, reduces analytical waste, and minimizes the potential for personnel exposure associated with traditional sampling methods. A prototype sampling system was designed, built and tested. System testing demonstrated operability of the microfluidic based sample system and identified system modifications to optimize performance.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Performance Testing of a Moving-Bed Gasifier Using Coal, Biomass, and Waste Plastic Blends with Washed and Unwashed Legacy Coals and Other Waste Fuels to Generate White Hydrogen

The objective of this effort, primarily funded by the United States Department of Energy (DOE), and led by the Electric Power Research Institute, Inc. (EPRI), with support by Hamilton Maurer International (HMI) and Sotacarbo S.p.A. (Sotacarbo), has been to qualify coal, biomass, and plastic waste blends based on performance testing of selected fuel pellet compositions in a pilot-scale updraft moving-bed (UDMB) gasifier. The testing provided relevant data to advance the commercial-scale design of the moving-bed gasifier to be able to successfully use these feedstocks to produce hydrogen. In particular, the effects of waste plastics on feedstock development (i.e., blending and pelletizing) and the resulting products (i.e., syngas compositions, organic condensate production, and ash characteristics) are the focus. The gasifier used for testing is HMI’s moving-bed gasifier, which has been proven capable of gasifying nearly all coal ranks. It has also shown the ability in prior testing work to gasify wood chips (biomass). However, mixtures of these fuels with plastic wastes have not been prepared and gasified together. The three feedstocks were densified and pelletized by California Pellet Mill (CPM) to meet the feedstock size required by Sotacarbo’s 30mm ID UDMB gasifier, under contract to HMI. The technical tasks and results from this two-year research project included: (1) Feed Procurement and Preparation: Nine different tri-fuel pellets were prepared from varying compositions of fresh mined PRB coal, corn stover biomass, and car fluff waste plastics. Tri-fuel pellets were produced by CPM and shipped to Sotacarbo’s test facility in Carbonia, Sardinia, Italy. (2) Test Plan Development: A test plan was created to define the test runs to be performed. The test plan detailed the different UDMB gasification tests to be performed in Sotacarbo’s 12-inch ID pilot scale gasifier, the process monitoring instrumentation used, and the extractive samples recovered for analysis of the total gasification process mass and energy balance. (3) Gasifier Testing: Nine different gasification runs were performed in the pilot-scale gasifier at Sotacarbo using nine different fuel feedstock compositions generated from varying mixtures of PRB coal, biomass, and plastic wastes. The testing generated performance data on gasification reaction efficiency and performance, yielding relevant data for models used to scale up the gasifier design. This task also included work to refurbish and reassemble the pilot gasifier at Sotacarbo and perform a baseline 100% PRB coal run. (4) Data Analysis and Reporting: Review of the data, determination of figures of merit, and interpretation of the results are reported in the project’s final report, published in March 2024. The results show that all tri-fuel pellets gasified well and maintained structural integrity throughout the gasification process. The syngas generated can be shifted to hydrogen by using commercial syngas shifting technologies. (5) High Fidelity computational fluid dynamics (CFD) Simulation: The National Energy Technology Laboratory (NETL) team performed CFD simulations of the UDMB gasifier for two of the tri-fuel pellets gasified in Sotacarbo’s pilot scale gasifier. The kinetic mechanisms for the pyrolysis of each constituent, PRB coal, corn stover biomass, and waste plastics are based on thermogravimetric analysis performed by Sotacarbo. The gasification model was validated by comparing the predicted syngas composition at the exit of the gasifier with the measured syngas composition. In addition, the reactor’s measured internal temperature profile agreed well with the predicted internal reactor temperature profile. These results validate that the model can be used to predict the performance of the updraft moving bed gasifier for different feedstocks and operating conditions. This paper summarizes the results of the completed work in which the pelletizing procedure was validated to ensure the viability of the tri-fuel pellets for the gasification runs performed at Sotacarbo’s 30 mm UDMB gasifier. The gasification performance data from this series of nine runs will enable modeling of a full-scale HMI industrial scale gasifier supporting both combined heat and power, and Hydrogen production from coal (both fresh mined and legacy) combined with various biomass and waste plastics. Additionally, plans and progress on a follow-up project, being executed by the same project team, will be presented. In this project, a total of twenty (20) different feedstocks are being prepared from varying compositions of biomass (both woody biomass and corn stover) with a mixture of legacy coal waste, plastic waste, and refuse-derived fuel (RDF). The testing will provide information on gasification reaction efficiency/performance, yielding relevant data for models used to scale up the gasifier design to 50 megawatt electric (MWe) (equivalent hydrogen production). Tests will also be performed on a bench-scale fluidized-bed gasifier for comparison purposes. The results of this testing will be used to specify the range of feedstock blends that can be successfully gasified as well as quantify gasifier outputs based on specific blends.

08 HYDROGEN↗

DOE OSTI2021

Nanoscale biochemical sample preparation and analysis

Provided herein are methods and systems for biochemical analysis, including compositions and methods for processing and analysis of small cell populations and biological samples (e.g., a robotically controlled chip-based nanodroplet platform). In particular aspects, the methods described herein can reduce total processing volumes from conventional volumes to nanoliter volumes within a single reactor vessel (e.g., within a single droplet reactor) while minimizing losses, such as due to sample evaporation.

Kelly, Ryan T.↗

DOE OSTI2025

Leveraging unlabeled SEM datasets with self-supervised learning for enhanced particle segmentation

Scanning Electron Microscopes (SEMs) are widely used in experimental science laboratories, often requiring cumbersome and repetitive user analysis. Automating SEM image analysis processes is highly desirable to address this challenge. In particle sample analysis, Machine Learning (ML) has emerged as the most effective approach for particle segmentation. However, the time-intensive process of manually annotating thousands of SEM images limits the applicability of supervised learning approaches. Self-Supervised Learning (SSL) offers a promising alternative by enabling knowledge extraction from raw, unlabeled data. This study presents a framework for evaluating SSL techniques in SEM image analysis, focusing on novel methods leveraging the ConvNeXtV2 architecture for particle detection. A dataset comprising 25,000 SEM images is curated to benchmark these proposed SSL methods. The results demonstrate that ConvNeXtV2 models, with varying parameter counts, consistently outperform other techniques in particle detection across different length scales, achieving up to a 34% reduction in relative error compared to established SSL methods. Furthermore, an ablation study explores the relationship between dataset size and SSL performance, providing actionable insights for practitioners regarding model selection and resource efficiency. This research advances the integration of SSL into autonomous analysis pipelines and supports its application in accelerating materials science discovery.

Rettenberger, Luca↗

NASA NTRS2005

[Corrected Title: Solid-Phase Extraction of Polar Compounds from Water] Automated Electrostatics Environmental Chamber

A solid-phase extraction (SPE) process has been developed for removing alcohols, carboxylic acids, aldehydes, ketones, amines, and other polar organic compounds from water. This process can be either a subprocess of a water-reclamation process or a means of extracting organic compounds from water samples for gas-chromatographic analysis. This SPE process is an attractive alternative to an Environmental Protection Administration liquid-liquid extraction process that generates some pollution and does not work in a microgravitational environment. In this SPE process, one forces a water sample through a resin bed by use of positive pressure on the upstream side and/or suction on the downstream side, thereby causing organic compounds from the water to be adsorbed onto the resin. If gas-chromatographic analysis is to be done, the resin is dried by use of a suitable gas, then the adsorbed compounds are extracted from the resin by use of a solvent. Unlike the liquid-liquid process, the SPE process works in both microgravity and Earth gravity. In comparison with the liquid-liquid process, the SPE process is more efficient, extracts a wider range of organic compounds, generates less pollution, and costs less.

Sauer, Richard↗

DOE OSTI2019

On-Line Monitoring and Real-Time Characterization of Low Level Waste and Off-Gas Condensate Samples using Raman Spectroscopy - 19274

The demand for Hanford waste property analysis is expected to significantly increase as the U.S. Department of Energy River Protection Project progresses toward transferring waste to the Hanford Waste Treatment and Immobilization Plant. The analysis of waste includes chemical, radionuclide, and physical property characterizations, with the goal of achieving safe/informed transfer and processing. Waste sampling followed by offline laboratory analysis is the current baseline analytical approach. The addition of field-deployed/in situ instruments has the potential to provide improvements and benefits over offline analysis in the areas of 1) Worker Safety: by reducing the need for sampling and thereby reducing the need for worker interaction with waste during sample handling; 2) Operational Efficiency: by reducing analysis turnaround times and offsetting demand on analytical laboratories; and 3) Accuracy: continuous analysis of a flowing waste stream allows cumulative results to be produced for the batch, which is more representative than discrete samples of batch properties. This paper describes the development and application of an online monitor to provide chemical characterizations; specifically, Raman spectroscopy is utilized to identify and quantify tank components. Accurate quantification is achieved through the use of chemometric analysis, which can be configured to provide real-time analysis in field deployment settings. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2025

Effects of magnetic field assisted heat treatment on the microstructure and mechanical properties of Fe-0.63 %C alloy

This study investigates the influence of an applied magnetic field on the microstructural evolution and mechanical properties of hypoeutectoid steels subjected to heat treatment. Tensile tests and microstructural analysis were performed on samples processed under varying magnetic field strengths (0 T, 5 T, and 9 T) and different austenitization incubation times. The results indicate that the application of a magnetic field alters the fraction of proeutectoid ferrite phase without changing the cooling rates and heat treatment process. Additionally, pearlite microstructural features such as lamellar spacing and misorientation angles exhibit variations under different field strengths. While the pearlite nodule diameter remains largely unaffected, an increase in percentage elongation and strength is observed in the 5 T treated sample, attributed to changes in microstructural features with the magnetic field. Additionally, the percentage elongation is reduced in the samples heat treated with reduced austenitization incubation times. The study further demonstrates that low-angle misorientations increased in the samples taken parallel to the magnetic field direction, influencing the mechanical response. These findings suggest that applying a magnetic field during heat treatment provides an additional driving force for phase transformations, offering a manufacturing process for tailoring microstructures and optimizing mechanical properties. Moreover, integrating magnetic fields in heat treatment processes has potential benefits in energy efficiency.

High magnetic field↗

DOE OSTI2013

Evaluating HDEHP Based Polymer Ligand Film (PLF) for Rapid Extraction of Plutonium

A method was developed to produce a thin Polymer Ligand Film (PLF) using di(2-ethylhexyl) orthophosphoric acid (HDEHP) ligand for rapid extraction of plutonium. The ligands were incorporated into a polymer matrix to generate a thin film substrate. HDEHP is an efficient extractant for a wide variety of metal ions. It is an amphiphillic molecule with two long hydrocarbon chains and a polar end with a phosphoryl oxygen (P=O) and an acidic –OH group. The extraction of lanthanides and other +3 oxidation state elements is highly dependent on the molarity of nitric acid in liquid/liquid extraction. The distribution factors for lanthanides generally decrease as molarity of nitric acid increases. Plutonium and uranium are less dependent on the molarity of the nitric acid. Still the distribution factors are higher at lower a nitric acid concentration. The main benefit of a PLF is that it eliminates the need for extensive and time consuming chemical processes to prepare samples for analysis. PLFs were tested using 239 Pu tracer, and all of the samples were analyzed with alpha spectroscopy to measure the recovery of plutonium. The pH of the plutonium tracer solutions and exposure time were varied to study effectiveness of PLFs in different conditions.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

NASA NTRS1988

Terrestrial imaging spectroscopy

Recent advances in imaging spectroscopy for remote sensing applications are discussed, reviewing the results of recent investigations. The advantages offered by the higher spectral resolution of imaging spectroscopy relative to scanners such as Landsat MSS and TM are explained; the design and performance of the Airborne Imaging Spectrometer (Vane et al., 1984) are described and illustrated with drawings, photographs, and sample images; data processing and analysis techniques are outlined; and applications to geological and botanical research are considered.

Vane, Gregg↗

NASA NTRS1988

Martian oxidation processes and selection of ancient sedimentary samples for bio-organic analysis

The results obtained by the Viking Missions concerning organic and biological analysis are summarized and it is indicated that these results do not preclude the existence in buried or protected regions of the planet, organic molecules or fossil life. The use of automated instruments is suggested for the analyses of samples obtained from certain regions of the planet, as a preliminary step before they are selected, retrieved, and returned to Earth for more complete analysis.

Oro, J.↗

NASA NTRSDate not supplied

Maximizing Spaceflight Biological Data with Omics Analytics: The NASA GeneLab Database

NASA’s GeneLab includes an open-access repository of some 250+ omics datasets generated by biological experiments relevant to spaceflight including simulated cosmic radiation and microgravity. In order to maximize the intelligibility of these data, particularly for users with limited bioinformatics background, GeneLab has become a knowledgebase platform converting raw genetic and proteomic signatures found in flight samples into biological and physiological meanings. A large community of more than 100 scientists has rallied behind GeneLab and organized into four Analysis Working Groups (AWGs: Animal, Plant, Microbe, and Multi-Omics). Together, the AWGs have gained scientific recognition worldwide by establishing a consortium in charge of adopting new complex standards for data analysis workflows and omics sample processing in a rapidly evolving field. We will demonstrate the usage of the repository with smart search capability, an online controlled-access toolshed "Galaxy" to process user data with vetted standard workflows, a workspace for data sharing and a data submission portal with ontology control for better metadata curation. The GeneLab visualization portal will also be demonstrated, showing how anyone without formal training in bioinformatics can now browse the space biology omics data to discover new biology and potential solutions to improve life in space.

Sylvain Vincent Costes↗

NASA NTRSDate not supplied

GeneLab: The NASA System Biology Platform for Space Omics Repository, Analysis and Visualization

GeneLab↗

NASA NTRSDate not supplied

Carbon Tracers of Aqueous Processes: Isotopic Analysis of Cr Carbonate Grains With Implications for Bennu Samples

Carbonate grains in carbonaceous chondrites record aqueous alteration events on the asteroidal parent bodies, including evidence for episodic alteration, timing of alteration, and time and temperature evolution of volatiles. Spectral features in the 3.4 μm region at asteroid Bennu have been interpreted as coming from carbonate minerals. Coordinated analysis of carbonate grains will be a valuable tool for analysis of Bennu samples, and related analysis of analog materials provides important context for understanding aqueous alteration of carbonaceous asteroids more broadly. To that end, our team is analyzing carbonates in Bennu analog materials, using Raman spectroscopy to identify carbonates and assess the maturity of related organic materials, vacuum reflectance spectroscopy from the ultraviolet through thermal infrared range to constrain contributions from carbonates and organics, X-ray microtomography and electron probe microanalysis (EPMA) to assess the distribution of void space, transmission electron microscopy to characterize space weathering effects, and EPMA and secondary ion mass spectrometry (SIMS) to measure composition and isotopic ratios. Here, we describe in situ analysis of carbon and oxygen isotopes from carbonates in Grosvenor Mountains (GRO) 95577.

K E Miller↗

DOE OSTI2016

Analysis of Time Dependent Data and PRA

In the past decades, several numerical simulation codes have been employed to simulate accident dynamics (e.g., RELAP5-3D, MELCOR, MAAP). In order to evaluate the impact of uncertainties into accident dynamics, several stochastic methodologies have been coupled with these codes. These stochastic methods range from classical Monte-Carlo and Latin Hypercube sampling to stochastic polynomial methods. Similar approaches have been introduced into the risk and safety community where stochastic methods (such as RAVEN, ADAPT, MCDET, ADS) have been coupled with safety analysis codes in order to evaluate the safety impact of timing and sequencing of events. These approaches are usually called Dynamic PRA or simulation-based PRA methods. These uncertainties and safety methods usually generate a large number of simulation runs (database storage may be on the order of gigabytes or higher). The scope of this paper is to present a broad overview of methods and algorithms that can be used to analyze and extract information from large data sets containing time dependent data. In this context, 'extracting information' means constructing input-output correlations, finding commonalities, and identifying outliers. Some of the algorithms presented here have been developed or are under development within the RAVEN statistical framework. (authors)

22 GENERAL STUDIES OF NUCLEAR REACTORS↗