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DOE OSTI2021

PERFORMANCE CHARACTERIZATION OF THE DIRECT CONTACT MEMBRANE DISTILLATION MODULE OPERATED WITH HIGHLY CONCENTRATED SOLUTION

The experimental study was conducted to characterize the performance of the flat sheet Direct Contact Membrane Distillation. The length degradation was studied in a short and long module with and without spacers. The experimental study is validated using the predicted flux for a wide range of operating conditions using deionized water. Three different membranes are used in the parametric study for feed Reynolds number varied between 500 and 2000, and inlet feed temperature varied between 45°C and 80°C. PTFE membrane was shown to be more effective than the PVDF due to its higher permeability coefficient and higher hydrophobicity. Fouling study was conducted on the selected PTFE membrane with various feed Reynolds numbers between 500 and 2000 and feed inlet temperature between 50°C and 80°C. Membranes used in the fouling study were characterized using scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS) for the morphology and chemical composition of the fouling layer. 36 hours of operation with 10 wt% NaCl (100,000 ppm) at feed inlet temperatures 80°C and 60°C and fixed Reynolds 2000 demonstrated a drop in flux by 31% and 27%, respectively. Low flow rate and high temperature are favorable conditions for fouling formation and reduced permeate flux for highly concentrated solutions. The spacers improved the flux by 30.8% and 27.6% at the operating Reynolds numbers 2000 the short and long channel modules. This study helps to design and optimize DCMD modules for industrial-size desalination and water treatment applications.

Kim, Deliya↗

DOE OSTI2023

Godiva IV Central Cavity Neutron Environment Characterization with Threshold Neutron Detectors

Godiva IV is a cylindrical fast burst reactor comprised of approximately 65 kg of highly enriched uranium that is operated by Los Alamos National Laboratory and sited at the National Criticality Experiments Research Center at the Nevada National Security Site in Nevada in the United States. Godiva IV is typically operated at delayed critical and in the regime spanning from sub-prompt to super-prompt bursts. Godiva IV is used for sample irradiations, criticality safety demonstrations, dosimetry studies, and for studying super-prompt behavior. In preparation for both an upcoming experiment to reduce uncertainties in the prompt fission spectrum for 235 U using threshold neutron detectors, and for future research using Godiva IV, it was desired to exercise the process of the selection of threshold neutron detectors/activation foils, radiation metrology, and the subsequent adjustment of the neutron spectrum. For this exercise, nine high purity threshold neutron detectors/activation foils were irradiated in a Godiva IV burst. The foils were then analyzed using a high purity germanium detector in the NCERC counting laboratory to determine end of irradiation specific activities for available IRDFF-II reactions. This work summarizes the Godiva IV foil irradiation, radiation metrology results, and adjusted neutron spectrum. The results of this exercise ultimately characterized the neutron environment inside the sample irradiation cavity inside Godiva IV to a higher degree than previously performed, informed decisions for the upcoming larger scale experiment, and will inform future neutron spectrum characterizations at NCERC.

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2020

Application of On-Line Monitoring and Real-Time Characterization of Low Level Waste Samples from Hanford Tanks

Waste and treatment stream characterization is an essential part of safe, efficient, and cost-effective processing of Hanford materials. The demand for materials characterization, including chemical, radionuclide, and physical attributes during waste management, transfer, and staging operations in the Hanford tank farms, is expected to significantly increase as the U.S. Department of Energy Office of River Protection (ORP) progresses toward Hanford waste treatment and immobilization. The application of on-line monitoring can greatly improve operation timeframes and reduce costs by providing real-time data and supporting the reduction of necessary grab sample collection. Recently, our team applied Raman online monitoring and chemometric modeling to the supernate of Hanford tank 241-AP-105, and demonstrated the quantitative measurement of nine analytes within this waste. Application of this method has been expanded to additional Hanford tank wastes, AW-102 and AP-107. The performance of the process monitoring instruments and the accuracy of the chemometric models will be assessed. On-line monitoring results will be compared to anion results determined from the current standard, ion-chromatographic and inductively coupled plasma mass spectrometry methods. Comparisons of both determined values and uncertainties of results will be presented. Results will be shared with personnel working on flowsheet interfaces for the Direct-Feed Low Activity Waste mission at Hanford.

Lines, Amanda M.↗

DOE OSTI2021

Advancements of On-Line Monitoring and Real-Time Characterization of Actual Low-Level Hanford Tank-Waste Samples

Waste and process stream characterization is essential to the safe, efficient, and cost-effective processing of Hanford Site materials. The demand for materials characterization including chemical, radionuclide, and physical attributes during waste management, transfer, and staging operations in the Hanford tank farms is expected to significantly increase as the U.S. Department of Energy River Protection Project progresses toward Hanford waste treatment and immobilization. Our past work has applied Raman on-line monitoring and chemometric modeling to the supernate of Hanford tank 241-AP-105 and has demonstrated the quantitative measurement of nine analytes within this waste. To demonstrate broader applicability, this method has now been expanded to waste from two additional Hanford tanks, AW-102 and AP-107, and the offgas condensate from lab-scale melter runs of actual-tank waste feeds. To enhance the performance of the Raman method, instruments with various excitation wavelengths were compared, since it is known that the Raman response is enhanced by shorter wavelength excitation. The laser excitations for the three systems tested were 404 nm, 532 nm, and 671 nm. In addition to laser wavelength selection, the laser power, measurement integration times, and signal averaging techniques were also investigated to determine their effect on detection limits for oxy-anion analytes within tank wastes. These advancements in Raman capability are compared with past standards and will be presented.

Bryan, Samuel A.↗

DOE OSTI2023

AFRRI TRIGA Reactor Neutron and Gamma Dose Characterization Preliminary Results

Integral Experiment Request (IER) 484 is part of a series of dose characterization and nuclear accident dosimeter (NAD) exercises performed under the Department of Energy (DOE) Nuclear Criticality Safety Program (NCSP). The Armed Forces Radiobilogy Research Institute (AFRRI) 1.1 MW Training, Research, Isotopes, General Atomics (TRIGA) Mark-F reactor is the third facility to undergo a dose study to establish reference dose values. A preliminary measurement was performed earlier this year, where a variety of foils were irradiated and activation gamma rays were measured using a high-purity germanium (HPGe) detector. The data was taken and analyzed to calculate the neutron spectrum in the irradiation facility. This paper will present preliminary results of the neutron dose measured. The characterization of the AFRRI dose field is planned in August.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2023

Oxadiazole-based Heterocycles as Building Block for Material Property Control: Design, Synthesis, and Characterization of 3,4-Bis(3-(4-nitro-1,2,5-oxadiazol-3-yl)- 1,2,4-oxadiazol-5-yl)-1,2,5-oxadiazole (LLM-210)

This paper presents an approach to novel oxadiazole-based melt-castable energetic material, LLM-210. Used in pour-in process and 3D printing, melt-castable energetic materials (MCEM) must possess required physical and safety properties of industry-standard energetic materials, also a narrow range of melting point between 80-100 °C. Melting point is difficult to accurately predict, therefore, searching for MCEM is challenging. 3,4-Bis(5-(4-nitro-1,2,5-oxadiazol-3-yl)-1,2,4-oxadiazol3-yl)-1,2,5-oxadiazole (LLM-205), composed of five-oxadiazole rings allied via carbon-carbon bonds, was selected as new MCEM candidate. The target molecule was synthesized and characterized, showing a density of 1.807g/cm3 ; thermal decomposing temperature at 299 °C; and insensitive to external stimuli, but the melting point of 104 °C was out of the rang. Based on the molecular properties and ab initio calculations, 3,4-bis(3-(4-nitro-1,2,5-oxadiazol-3-yl)-1,2,4-oxadiazol-5-yl)- 1,2,5-oxadiazole (LLM-210), an isomer of LLM-205, was designed and synthesized from a different way. LLM-210 was characterized as MCEM, possessing melting point of 87 °C; density of 1.812 g/cm3 ; and exothermally decomposing temperature at 314 °C; being insensitive to external stimuli. In this study, the relationship of molecular structure to properties of LLM-205 and LLM-210 based on the results of Density Functional Theory (DFT) and X-ray crystallographic analysis is also briefly discussed.

Chemistry - Chemical explosives↗

DOE OSTI2020

Application of On-Line Monitoring and Real-Time Characterization of Low Level Waste Samples from Hanford Tanks - 20380

Waste and treatment stream characterization is an essential part of safe, efficient, and cost-effective processing of Hanford materials. The demand for materials characterization, including chemical, radionuclide, and physical attributes during waste management, transfer, and staging operations in the Hanford tank farms, is expected to significantly increase as the U.S. Department of Energy Office of River Protection (ORP) progresses toward Hanford waste treatment and immobilization. The application of on-line monitoring can greatly improve operation time frames and reduce costs by providing real-time data and supporting the reduction of necessary grab sample collection. Recently, our team applied Raman online monitoring and chemometric modeling to the supernate of Hanford tank 241-AP-105, and demonstrated the quantitative measurement of nine analytes within this waste. Application of this method has been expanded to additional Hanford tank wastes, AW-102 and AP-107. The performance of the process monitoring instruments and the accuracy of the chemometric models will be assessed. On-line monitoring results will be compared to anion results determined from the current standard, ion-chromatographic and inductively coupled plasma mass spectrometry methods. Comparisons of both determined values and uncertainties of results will be presented. Results will be shared with personnel working on flowsheet interfaces for the Direct-Feed Low Activity Waste mission at Hanford. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

Development of Electrochemical Detectors for Elemental Characterization of Actinides - 20563

The characterization of the actinides contained in radioactive waste involves complex and expensive separation processes. Electrochemical methods allow identifying and quantifying quickly and accurately the elementary concentration of actinides such as Th, U, Pu, Am, and Cm in liquid waste. The objective of this research proposal is to build a low-cost portable miniaturized electrochemical detector, which can be an alternative for an initial characterization of actinides in liquid waste. Therefore, this work proposes the use of an electrochemical graphite detector modified with phthalocyanine, to detect and quantify actinides in aqueous media. The electrochemical response of the modified graphite electrodes was performed by cyclic voltammetry, and so the detection and quantification limits for U and Th were determined. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

Integrating Electrical Resistivity Tomography with Vadose Zone Characterization - 20246

The environmental management mission at the U.S. Department of Energy Hanford Site includes addressing subsurface contaminants that are present in the vadose zone because of historical waste discharges. Characterization is needed to support evaluation of whether contaminants at specific disposal sites will migrate to and contaminate the groundwater in the future. Drilling of boreholes and analysis of retrieved sediment samples is a standard approach to evaluating contaminant distribution in the vadose zone for the types of inorganic and radionuclide contaminants at the Hanford Site. However, borehole sampling has limitations for understanding the volumetric distribution of contaminants. The Hanford Site is now applying electrical resistivity tomography to characterize the path and volumetric extent of contaminant migration in the vadose zone. This information aids selection of appropriate locations for obtaining borehole samples and provides three-dimensional contaminant distribution information for incorporation into conceptual site models and to help configure fate and transport models. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

Characterization Strategy of a Limited Number of Radioactive Waste Effluent Tanks in View of Decommissioning a Large Number of Tanks - 20286

In order to organize the D and D of the former effluent treatment facility at the CEA Cadarache Center (France), the key data to gather through the facility characterization are the following:: volumes and masses, liquid/solid distribution and specific activity. By studying the treatment processes and the history of the facility, families of tanks have been defined and a reference tank chosen for investigation in each family. The intrusive investigations (video, residue thickness, dose rate..), the gamma spectrometry measurements carried out on site on the residue samples and radiochemical results collected in laboratories, led us to conclude that there was a relative radiological homogeneity (for specific activity and Am-241/Cs-137 ratio) within each tank. The next step consisted in extrapolating the specific activity evaluated for the reference tanks, to the other tanks of each family by using data such as geometry, dose rate or the function of the tanks within the process. Thus, a cartography of the 130 tanks of the facility is available. Finally, the conclusions drawn from the radiological homogeneity of the tanks and their affiliation to homogeneous, well-identified tank clusters lead to a simple and efficient operational approach for the D and D of the 130 tanks of the facility. Indeed, because of the residue characteristics (homogeneous activity and strong differentiation of Cs/Am ratio), a sample collected when opening the tank, and measured on site by gamma spectrometry will allow us to validate the operational design and the emptying techniques defined during the D and D study phase thanks to the characterization of a limited number of reference tanks. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2020

Verification of Reactor Activation Modelling with Physical Characterization Data and the Impact on Long Term Assessments - 20303

Whiteshell Laboratories, located in Manitoba, Canada, provided research facilities for the Canadian nuclear industry since the early 1960's. The facility was centered on Whiteshell Reactor 1 (WR-1), an organically cooled, heavy water moderated nuclear reactor. WR-1 was safely shut down in 1985, defueled and drained, and has been in a safe Storage with Surveillance (Deferred Decommissioning) state until present day. In support of an Environmental Assessment for proposed in-situ disposal of WR-1, detailed characterization information regarding the reactor core components (calandria, calandria tubes, and pressure tubes) was necessary to provide confidence that the long-term impacts of the facility can be assessed adequately. A simplified estimate of the total activation of core components was completed in 1992 using conservative assumptions, expected reactor configuration and computer models built with WIMS-CRNL, ONEDANT and ORIGEN-S. Due to the simplification, and age of the work, there was considerable doubt that the modelled inventory estimate of the core components was sufficient to support long-term performance modeling of the planned in-situ decommissioning. Additional data would be required to provide this confidence. Several options were considered for characterizing the WR-1 core components, but it was decided to collect only a limited number of samples in an effort to validate the 1992 simplified estimate as bounding. The limited number of samples reduced risks to workers, both radiological and non-radiological, and significantly reduced the costs required to confidently define and bound the radiological inventory of activation products in the core. The results of the sampling were compared to the simplified activation estimation. There was good agreement between the modelled and sampled results, with all major contributors to total activity showing similar relative quantities. The samples were generally lower than predicted by the models, with few exceptions. Notable exceptions included Nb-94, which were higher in the sample results than the model. This was determined to be caused by the use of Niobium containing steel alloys in the stainless steel pressure tube that were not accounted for in the models. The comparison of results provided confidence that the original inventory estimates produced through the simplified model are conservative and bounding, and therefore suitable for use in the long-term assessment of in situ disposal of the WR-1 reactor. This paper provides details of the simplified computer model results, their comparison to results of the sampling, and the changes adopted in the assessment of the in-situ decommissioning of WR-1 as a result. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2024

Core Characterization: Computer Tomography, Geochemical, and Core Petrophysical Workflows for Emerging Critical Mineral Plays

The National Energy Technology Laboratory’s geoimaging lab in Morgantown, WV has been performing core characterization using multi-resolution Computed Tomography (CT) imaging and multisensor corelogger which allows for cm-resolution elemental and petrophysical measurements along whole core. This workflow has historically been used in unconventional gas plays and potential carbon storage locations. This rapid core characterization leads itself well as a first phase process in CM/REE evaluation efforts allowing for high-resolution, non-destructive investigation of elemental concentration using X-Ray Fluorescence and examination of core features through CT imaging.

Paronish, Thomas J.↗

DOE OSTI2024

Characterization of Non-Science Grade DESI CCDs and Creating Additional ICARUS Monitoring Metrics for Data Quality

DESI, otherwise known as the Dark Energy Spectroscopic Instrument, is an astronomical project measuring millions of optical spectra to characterize Dark Energy. The survey has been running for 3 years. My work delves into the data taking/analysis side of the DESI CCDs (Charge-Coupled Devices) which will help in swapping out broken CCDs on the instrument. Additionally, I worked on making new metrics for ICARUS, Imaging Cosmic and Rare Underground Signals for their monitoring of run data. This paper will talk about the types of characterizations done for DESI and additional metrics for data quality and tools used for ICARUS monitoring.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2024

Synthesizing, Compounding, and Characterizing a Heat Labile Polyurethane Foam

ABSTRACT A need exists for a packaging foam material that can be converted from solid to gaseous degradation products at reasonably low energy levels or temperatures, such as 100O C. This paper will primarily discuss the approaches currently being used to synthesize and characterize such a material. These approaches include the incorporation of novel polyols such as azo containing diols, polycarbonate diols, and polypropylene carbonate polyols into polyurethane foams. Characterization methods include NMR, FTIR, TGA, finite element analysis, impact strength, and others. This project will be funded for a duration of three years. Year 1 focused on developing the proposed test methods and producing an initial rigid polyurethane foam. Year 2 focuses on refining the materials and test methods. If appropriate, design of experiment (doe) techniques will be used to optimize components, component levels, density and other variables to attain required final material properties (TGA weight loss, impact strength, etc.). Year 3 focuses on scaling up to larger engineering quantities. The application for this material is in load securement for transportation of low level radioactive waste materials within the US Department of Energy (DOE) complex. Foam in place process equipment and operators will be shielded using this novel method over current practice. Current practice can involve time consuming methods of load securement in low level radiation environments. This new technique would eliminate exposure time securing the load and greatly improve the As Low As Reasonably Attainable (ALARA) conditions. The objective is to progress to higher Technical Readiness Levels (TRL) and larger pilot scale quantities. This paper discusses methodologies and presents current results to date.

Kranjc, Mark D.↗

DOE OSTI2024

The Rise of Intelligent Materials Science: Unleashing the Power of Machine Intelligence in Characterization

Machine intelligence has the potential to revolutionize materials science, enabling autonomous synthesis, self-driving characterization, and accelerated modeling. However, despite the promise, successful implementation of these methods in day-to-day research remains a challenge. This talk will delve into the reasons behind this, exploring how truly intelligent experiments are hindered by opaque experiment control, a lack of domain-specific models, and human-centric design. Through a focus on the characterization of next-generation microelectronics and energy storage materials, I will share insights from both successful and failed attempts to implement machine intelligence. We will then explore the next steps necessary to unlock the full potential of machine intelligence in materials science, creating a future where intelligent systems work seamlessly alongside researchers to drive innovation and discovery.

autonomous↗

DOE OSTI2024

Pre-Transient Characterization of Historic EBR-II Pins for Transient Testing

Current interest in sodium-cooled fast reactor (SFR) designs, such as TerraPower’s Natrium Reactor, has highlighted the need for advanced reactor fuel technology development. Modern U-Zr and U- Pu-Zr pin designs are primary candidates to fuel SFRs and boast high fuel utilization capacity, increased fuel-cladding compatibility, and improved safety through inherent feedback mechanisms. Despite over 60 years of metallic fuel irradiation, uncertainties exist in the performance of the fuel system, particularly under transient overpower (TOP) and loss of flow (LOF) scenarios. Throughout historical testing within the Experimental Breeder Reactor II (EBR-II) and the Fast Flux Test Facility (FFTF), fuel behavior has demonstrated benign response to transient reactor conditions; however, accurate predictions of failure thresholds to inform operational limitations rely heavily on fuel composition, burnup, and irradiation history. In expanding TOP and LOF testing, the Transient Heat sink Overpower Response (THOR) Capsule will be used to test modern fuel technologies in a static sodium environment in the Transient Reactor Test (TREAT) Facility. The THOR capsule is highly instrumented and will provide time-dependent thermal behavior of SFR fuel pins subjected to accident conditions within TREAT. The THOR-Metallic (THOR- M) campaign aims to validate and expand historical TOP and LOF testing on high burnup U-Zr and U-Pu- Zr fuel alloys previously irradiated in EBR-II by running the rods to failure. This contribution focuses primarily on the pre-transient engineering-scale destructive and non- destructive characterization that has been conducted on both the test and sibling pins used for the TOP and LOF tests. All pins underwent visual examination, neutron radiography, element contact profilometry, and precise gamma scan. The sibling pins used for each test were further analyzed using gas assay, sampling, and recharge analysis (GASR), and optical microscopy. The results from each technique confirmed that the fuel pins were intact and devoid of any atypical developments when compared to historical data. Additionally, the analyzed measurements establish a baseline for comparison to post-transient analysis. Key fuel behaviors quanitifed include axial elongation of the fuel column, diametral strain of the pin, patterns in fluff structure geometry, changes in axial isotope distribution, evolution of constituent redistribution, porosity, and fission gas release. The pre-transient measurements and changes attributed to transient behavior from post-transient measurement will be compared to historical data to capture the behavioral dependence on composition, burnup, and irradiation history. Results from this work advance the initiatives of the THOR-M campaign, which aid in informing fuel performance models and establishing safety criteria for SFR operational limits. The novel combination of test environment, in-situ instrumentation, and comprehensive suite of characterization methods provides greater understanding of transient fuel behavior. Overall, information on the time and condition of pin failure for high burnup U-Pu-Zr will greatly expand the limited existing TOP and LOF test data.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Pre-Transient Characterization of Historic EBR-II Pins for Transient Testing

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2024

Dynamic Modeling and Characterization of Nuclear-grade Graphite

Idaho National Labs serves as the spearhead for many innovative energy solutions to the world's energy crisis. One such solution is the INL's Microreactor which is designed to deploy to extreme/remote environments where other sources of power are either unavailable or unreliable. In order to best design these energy solutions for their operational environments, it is crucial to understand how the design, components, and materials will respond to the environmental conditions. One key material in these innovative designs is a nuclear-grade graphite known as PCEA. This study examines the behavior of PCEA graphite under dynamic loading, similar to that which may occur in extreme environments. The objective is to characterize the dynamic behavior and produce an accurate, reliable constitutive model suitable for use in simulation tools such as INL's MOOSE. Graphite specimens were tested using a Split Hopkinson Pressure Bar (SHPB) to administer the dynamic compressive load. The SHPB was charged at various pressures to produce a range of strain rates on the material in compression. Data was acquired via strain gauges on the SHPB setup, from which stress, strain, and time data were collected. Analysis revealed the stress-strain behavior of the material as well as insights into the material behavior's relationship to strain rate. Further work must continue to characterize the various other dynamic behaviors of the material which will combine to create a substantially trustworthy constitutive model for this grade of nuclear-grade graphite. Ultimately, this will allow for realistic simulation of the material in reactor designs, allowing for prediction of design weaknesses and leading to improved designs for increased resilience, security, and reliability.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗