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DOE OSTI2015

UV-Vis Spectroscopy as a Tool for Safeguards; Instrumentation installation and fundamental data collection

Two spectrophotometric process monitors, one optimized for high concentration (approximately 10 g/L) and one for trace levels (approximately 10 ppm),were developed at Argonne and installed at the SRS H-Canyon facility for field testing. These systems were built of Commercial-Off-The-Shelf components utilizing a custom, facility-specific hardware interface. The systems directly provide a qualitative measurement of process chemistry (i.e. valence state). With appropriate calibrations the systems could provide quantitative data. Laboratory tests were performed to determine the spectrophotometric molar absorptivity coefficients for relevant actinide and transition metals of interest.

36 MATERIALS SCIENCE↗

DOE OSTI2022

Kiwi-TNT Simulation Model [Slides]

The Kiwi-TNT Test (Toonerville Trolley) was performed on January 12, 1965. LANL has the objective: "LANL will develop a defensible methodology for establishing the maximum number of fissions for postulated inadvertent criticality events. The methodology may include several methods, such as hand calculations, sophisticated modeling, and the use of historical data.” The historic test, Kiwi TNT, posed a starting point for predictive simulations to determine the number of fissions and excursion understanding. This presentation gives results of that effort.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

DOE OSTI2023

Material Property Determinations for Rock Valley Legacy Samples in Support of Source Physics Experiment

The Source Physics Experiment (SPE) is a long-term NNSA research and development effort designed to improve nonproliferation verification and monitoring capabilities. The overarching goals of the SPE program are to improve understanding of prompt signals and physical signatures that develop from underground chemical explosions and associated modeling capabilities. Our work focuses on a primary factor controlling chemical explosion induced signals and signatures: the material properties of the rocks in which the chemical explosion takes place. This document reports on material property determinations of legacy core USGS Test Well F and outcrop analogs for the subsurface stratigraphy for the third phase of SPE in the Rock Valley (RV) area of the Nevada National Security Site (NNSS). The objective of this work is to establish a baseline set of lithologic descriptions and material properties expected prior to observatory borehole drilling in support of the SPE-RVDC (Rock Valley Direct Comparison) experiment. We determine for each rock type the compressional failure envelope, elastic properties as a function of stress (bulk modulus versus mean stress, shear modulus versus shear stress, Young’s modulus versus axial stress and Poisson’s ratio versus axial stress), indirect tensile strength, and porosity. Geologic characterization, both at the core-scale and microscale, provides context for using the data in modeling efforts and to inform interpretations for the material properties testing.

36 MATERIALS SCIENCE↗

DOE OSTI2019

Technical Basis and Implementation of Groundwater Pathway Models Used for INL's RH LLW Disposal Facility Performance Assessment - 19440

The Idaho National Laboratory's (INL's) Remote-Handled Low-Level Waste (RH LLW) Disposal Facility has been designed and constructed to receive waste generated by INL in support of the Office of Nuclear Energy (NE) and Naval Reactors (NR) missions. RH LLW is generated on the INL site from spent nuclear fuel handling and operations at the Naval Reactors Facility (NRF), the Advanced Test Reactor (ATR), and at the Material and Fuels Complex (MFC) in addition to other miscellaneous research activities. The facility has been designed to receive RH LLW currently in storage at INL facilities and new waste generated by nuclear research programs. RH LLW received at the facility is solid waste consisting of surface contaminated materials, ion exchange resins used to purify cooling water, and activated metals generated during reactor core change outs, Naval spent fuel management, and nuclear R and D. The facility has been designed to meet the requirements of DOE Order 435.1, Radioactive Waste Management for all-pathways including groundwater and air, radon emissions limits, and inadvertent intrusion limits. The facility design includes a vault system incorporating robust concrete vaults oriented vertically in close-packed arrays, a hydraulic drainage system designed to limit water contact with the stainless steel waste canisters and concrete vaults, and a robust monitoring system. Per the environmental assessment (EA), all waste will be disposed of in stainless steel waste canisters. During facility design and construction, site-specific data was collected to provide laboratory and field scale performance characteristics for the concrete vault and hydraulic drainage systems. Field-scale infiltration tests were conducted and monitoring data was interpreted using numerical simulation. Based on interpretation of the observed laboratory and field test data, the facility performance assessment (PA) was developed. The PA groundwater pathway source release model differentially credits release from surface contaminated waste, ion exchange resins, and activated metals. It also credits steel waste canisters with failure rates based on actual corrosion data. Once released, radionuclide transport through the vadose zone and aquifer to downgradient receptor locations was simulated in the PA using a one-dimensional modeling approach based on three-dimensional modeling of historically-contaminated INL sites. This paper provides an overview of the groundwater pathway source release models and their technical implementation in the PA. It also describes the one-dimensional transport model used for the vadose zone and multi-dimensional model used for the aquifer. (authors)

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗

DOE OSTI2022

Development and validation of a quantitative proton NMR method for the analysis of pregnenolone

Pregnenolone (PREG) is an endogenous steroid frequently sold as an over-the-counter dietary supplement touted to promote neurological and immunological health. While the PREG dietary supplement is added to the diet for health benefits, there are no FDA approved PREG drugs. However, compounded PREG drug products are available to U.S. patients. The FDA works with state regulatory authorities on the oversight of compounding activities, including developing 503A and 503B lists of bulk substances that compounders are permitted to use. PREG is one of the substances publicly nominated to be included on the 503B list. Compounded hormone therapies such as those using PREG are of interest given the lack of standardization in compounded drug products which may increase the possibility of underdosing, overdosing, or contamination. However, no USP monograph currently exists to evaluate the quality of PREG drug substance or product. To address knowledge gaps and assist in quality control, a simple and rapid quantitative proton nuclear magnetic resonance spectroscopy (qNMR) method for the identification and assay of PREG in different types of PREG products was developed and validated. PREG samples were characterized using 1D 1 H and 2D 1 H– 13 C HSQC NMR spectra. The qNMR assay method (taking approximately 10 min per NMR spectrum) was validated for precision, accuracy, specificity, robustness and linearity per ICH Q2(R1) guidance. The method was validated in a range from 0.032 to 3.2 mg/mL. As a proof of concept, seven PREG bulk substance samples, three tablet and two capsule PREG dietary supplements were assessed by the qNMR analytical procedure. NMR data from all tested samples met the expected criteria for identification and assay. The results demonstrate the potential of qNMR for the quality assessment of different types of PREG samples.

60 APPLIED LIFE SCIENCES↗

DOE OSTI2017

The Area Between Exchange Curves as a Measure of Conformational Differences in Hydrogen-Deuterium Exchange Mass Spectrometry Studies

Hydrogen-deuterium exchange mass spectrometry (HDX-MS) provides information about protein conformational mobility under native conditions. The area between exchange curves, A{sub bec}, a functional data analysis concept, was adapted to the interpretation of HDX-MS data and provides a useful measure of exchange curve dissimilarity for tests of significance. Importantly, for most globular proteins under native conditions, A{sub bec} values provide an estimate of the log ratio of exchange-competent fractions in the two states, and thus are related to differences in the free energy of microdomain unfolding. .

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2025

Conceptual Designs for Irradiation Creep Testing of SiC in HFIR

Understanding irradiation creep of nuclear fuel cladding is important to properly size the initial fuel-cladding gap and understand when pellet-cladding contact is expected to occur due to a combination of fuel swelling and cladding creep-down. Irradiation creep also plays a role in relaxing stresses that develop in-pile. Silicon carbide fiber–reinforced silicon carbide matrix (SiC/SiC) composites are the leading long-term accident-tolerant fuel cladding concept for light-water reactors (LWRs). Although some limited data are available regarding irradiation creep of the individual constituents (fibers, matrix), data regarding irradiation creep of SiC/SiC composites are currently insufficient. Additional data regarding irradiation creep compliance and the rupture lifetime (combination of creep and slow crack growth) are needed to understand material limitations. This work describes the design and development of two irradiation vehicles that are being pursued for testing SiC/SiC concepts in the High Flux Isotope Reactor (HFIR). The first is a passive experiment, referred to as the PRECISE experiment, that leverages the constant coolant pressure of HFIR to compress a metallic bellows and provide a well-characterized load to drive creep in a SiC/SiC dog bone specimen. The total creep strain would be quantified post-irradiation by measuring dimensional changes of the specimen length as well as local dimensional changes within the gauge region. Non-stressed specimens would also be irradiated under the same conditions to provide an indication of dimensional changes due to radiation-induced swelling in the absence of creep. A second, more complex experiment, referred to as the INSITE experiment, is being designed in parallel that would use pneumatics to pressurize a metal bellows and linear variable differential transformers (LVDTs) to measure the specimen displacement in situ during irradiation. Such an experiment would provide significantly more data regarding the evolution of the creep compliance as a function of dose and applied stress within a single experiment but would require significantly more development time and cost to execute. The primary concern with the INSITE experiment is the accuracy, reliability, and expected lifetime of the LVDTs during irradiation at elevated temperatures. Efforts are being made to adjust the experiment design and operating procedure to limit LVDT temperatures and mitigate or otherwise compensate for uncertainties due to factors such as temperature fluctuations, creep in the surrounding structural materials, and drift of the LVDTs. This work describes the experiment designs, thermal and structural analysis that were performed to ensure that the desired temperature and stress conditions can be achieved, some initial sensitivity analyses to predict the evolution of the radiation-induced specimen displacements, and potential sources of uncertainty in the measurements. Out-of-pile testing is being performed in parallel to confirm that the test trains achieve the expected stress states in the specimens and do not result in prohibitive stress concentrators (e.g., in the grip regions) that might risk pre-mature failure. The PRECISE experiments are proceeding toward fabrication and assembly with HFIR insertion planned during fiscal year 2026. The INSITE experiment is progressing toward out-of-pile demonstrations, which will provide more conclusive evidence regarding the feasibility of executing these tests in HFIR or whether alternative displacement monitoring techniques may need to be considered.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2017

Technical Evaluation Report for the NDMAS AGR-5/6/7 TRISO Irradiation Monitoring System

The Nuclear Data Management and Analysis System (NDMAS) manages irradiation experiment data collected under the Advanced Gas Reactor (AGR) Fuel Development and Qualification program within the Advanced Reactor Technologies Technology Development Office. The AGR-5/6/7 irradiation experiment combines the fifth, sixth, and seventh planned irradiation campaigns of the U.S. Department of Energy AGR Fuel Development and Qualification Program. These combined irradiation tests will consist of fuel qualification tests (AGR-5/6) and a margin test (AGR-7) for the industrially produced uranium oxycarbide (UCO) tristructural isotropic (TRISO) coated particle fuel developed by the AGR program. The objective of the AGR-5/6/7 irradiation experiment is to establish the performance of UCO TRISO fuel fabricated using engineering-scale equipment in a production environment under and beyond normal operating conditions (PNL-5245). Experimental irradiation measurements for this experiment (i.e., thermocouple temperature, gas flow rate, fission product release rate, gross gamma count, and Advanced Test Reactor (ATR) operational parameters) are captured automatically to the NDMAS database. Data derived from numerical simulation or other mathematical analyses (i.e., fast fluence, burnup, temperature, and fission product release to birth ratio) are captured to the database when provided by the researchers. The NDMAS database is a relational database accessed via structured query language and managed with Microsoft SQL Server. While select users can directly access the database, that is not the most convenient way to interact with the data. The NDMAS team constructs numerous tables that combine related datasets, and delivers those data to researchers via graphs and spreadsheets on a Microsoft SharePoint-based website. For the AGR-5/6/7 experimental data, a new subsite has been developed, along with a set of web pages. These pages will be used by members of fuel irradiation team for monitoring irradiation conditions according to specification (SPC-1749), by the physics modelers to access necessary model inputs, and by the nuclear engineering community to view and access data such as fuel temperatures, fission product release from capsules, and ATR operational parameters. The deliverable represented in this document is a SharePoint website containing tables of the AGR-5/6/7 measured and calculated data, graphs displaying the data, and links to source documents and references.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2017

AGR-5/6/7 Irradiation Monitoring Web Site Design

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

DOE OSTI2015

FRONT-END ELECTRONICS FOR UNATTENDED SAFEGUARDS SYSTEMS: TESTING OF A CANDIDATE DEVICE

The International Atomic Energy Agency (IAEA) deploys unattended monitoring systems to provide continuous monitoring of nuclear material within safeguarded facilities around the world. As the number of unattended monitoring instruments increases, the IAEA is challenged to become more efficient in the implementation of those systems. In 2010, the IAEA initiated the Front-End Electronics for Unattended Measurement (FEUM) project with the goals of greater flexibility in the interfaces to various sensors and data acquisition systems, and improved capabilities for remotely located sensors (e.g., where sensor and front-end electronics might be separated by tens of meters). In consultation with the IAEA, a technical evaluation of a candidate FEUM device produced by a commercial vendor is being performed. This evaluation is assessing the device against the IAEA’s original technical specifications and a broad range of important parameters that included sensor types, cable types, and industrial electromagnetic noise that can degrade signals from remotely located detectors. Testing has been performed in a laboratory and also in environments representative of IAEA deployments. The results are expected to inform the IAEA about where and how FEUM devices might be implemented in the field. Data and preliminary findings from the testing performed to date are presented.

Smith, Leon E.↗

DOE OSTI2016

Scaling and Design Analysis of a Sub-Scale, Reduced Temperature Stratified Flow Separate Effects Test Facility for the Experimental Investigation of Air Ingress in a High Temperature Reactor System

High temperature gas reactors (HTGR) are poised to spearhead the next generation of nuclear reactors, due to their passive safety characteristics and their applications flexibility. Able to provide base load power or process heat for industrial applications, HGTRs may be a critical component to reducing greenhouse gas emissions in the United States and abroad. However, increased interest and development has also highlighted areas requiring further investigation, one of which being the air-ingress accident. Air ingress may occur following a break in the coaxial cross duct and pressure vessel depressurization. The initial mode of ingress is hypothesized to be density driven cross flow as the cold air enters the lower plenum, at which point molecular diffusion and/or local buoyancy phenomena will dominate until a global natural circulation current is established. While computational simulations support this progression, little or no experimental data exists to validate and support this phenomenology. Therefore, it is necessary to generate such data; this research seeks to do so through the use of a sub-scale separate effects test facility - the Stratified Flow Separate Effects Test Facility (SFSETF). The goal of this facility is more specifically to focus on the transition to global natural circulation starting from air ingress after a double-ended guillotine break (DEGB) while neglecting depressurization. This paper will provide analyses performed in the design of this facility, including the geometric and hydraulic scaling analyses, safety analysis and instrumentation selection. (authors)

21 SPECIFIC NUCLEAR REACTORS AND ASSOCIATED PLANTS↗

DOE OSTI2026

Quasielastic $\overrightarrow{^{3}He}$ $(\overrightarrow{e},e′)$ asymmetry in the threshold region with a longitudinally polarized target

We report on the measurements of the double-spin asymmetry from electron- 3 He scattering in the threshold region of two- and three-body breakup of 3 He for 4-momentum transfer values of 0.1 and 0.2 (GeV/c) 2 . The measurement was done at Jefferson Lab using a polarized 3 He target with its spin aligned parallel to the beam direction. This asymmetry is sensitive to a combination of spin-dependent response functions not previously measured and may highlight differences in two body forces, meson-exchange currents and final-state interactions. The results of this measurement serve as a test of our understanding of few-body systems. When compared with calculations from plane wave impulse approximation and Faddeev calculations, we found that the latter, which use modern nuclear potentials and prescriptions for meson-exchange currents, demonstrate an overall good agreement with data.

Few-body nuclei↗

DOE OSTI2021

Preliminary NoMAD Results of the MUSIC Experiment

The Measurement of Uranium Subcritical and Critical (MUSiC) experiment was carried out from December 2020 through April 2021 at the National Criticality Experiments Research Center (NCERC). This measurement campaign featured bare configurations of the Rocky Flats highly-enriched uranium (HEU) shells, with each configuration having different numbers of these shells. The goal of the experiment was to test multiple neutron multiplicity detectors and measurement methods for a large range of neutron multiplication values, to see when the combination of detectors and methods break down as the configurations reach the delayed supercritical window. Adding subcritical integral benchmarks gives additional validation to nuclear data. These benchmarks provide additional parameters against which to validate the data. While critical benchmarks have just a single value, $K_{eff}$ , subcritical benchmarks can be used to infer multiple parameters. As an example, recent subcritical benchmarks utilizing the Hage-Cifarelli formalism have three quantities of interest ($R_{1}$, $R_{2}$, and $M_{L}$). This gives nuclear data evaluators additional data to use when performing their evaluations, and allows for these benchmarks to be useful for additional types of nuclear data.

46 INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AND ↗

DOE OSTI2020

Shockwave Arrival Times from Operation Redwing and Operation Upshot-Knothole

Back in the 1940s, 50s, and 60s, 210 nuclear tests were conducted in the atmosphere. As part of the testing program, EG&G performed shockwave arrival-time measurements for different shots in different operations using pressure transducers at different distances from ground zero. They then developed correlations unique to each set of data. They did not attempt to correlate all data onto one curve. As a fireball moves, material is picked up and pulled in, which is called entrainment. This extra material increases the mass of the fireball, and as the energy is spread out over a larger and larger mass, the specific internal energy of the fireball gases drops, which causes the temperature to drop as well. When the energy in the solid angle of a spherical shockwave hits the surface, it is reflected. Shortly thereafter, it catches up with the outward-moving shockwave and re-combines with it, causing it to expand at a slightly faster rate. As the shockwave grows, it approaches a hemispherical shape. The purpose of this project is to demonstrate that the shockwave arrival-time data can, in fact, be correlated onto a single function when the shockwave time-dependent solution is modified to include a geometric factor, θ, and is corrected for an entrainment coefficient.

45 MILITARY TECHNOLOGY, WEAPONRY, AND NATIONAL DEF↗

DOE OSTI2025

Analyze the real-time performance of the optimized fiber-PTR instrument

An instrument to perform in-reactor, real-time thermal property measurements of nuclear fuels and materials was recently designed, optimized, and tested at Massachusetts Institute of Technology Research Reactor. It was the second insertion experiments of a total of two rounds. Here we report the collection and analysis of the real-time captured thermal diffusivity data on the preloaded SiC. With the optimized design, the instrument temperature had been successfully raised as we expected. Only one probe (the top one) returned real-time thermal diffusivity in a time span of approximately two days. Measured thermal diffusivity of the preloaded SiC was significantly lower than the literature value at the same temperature, indicating a significant influence from the irradiation induced microstructure damage. Meanwhile, the real-time thermal diffusivity value continuously reduced with time, indicating the dynamic microstructure evolution. The possible reasons of the probes that did not return data were hypothesized. The further optimization of the instrument with the objective to improve the measurement accuracy and instrument survivability is also discussed.

36 MATERIALS SCIENCE↗

DOE OSTI2026

Quality Assurance of Legacy Post-Irradiation Examination Data for Metallic Fuels

The U.S. DOE-NE’s Advanced Reactor Technologies (ART) Fast Reactor Program (FRP) and the NE-4 Advanced Fuels Campaign (AFC) have jointly undertaken the qualification of the legacy post-irradiation examination (PIE) data held in the Fuels Irradiation & Physics Database (FIPD), covering metallic fuel experiments conducted in the Experimental Breeder Reactor II (EBR-II) and the Fast Flux Test Facility (FFTF). In FY26 this effort reached a milestone: six major types of PIE data—contact profilometry, isotopic gamma scan, fission gas chemistry, fission gas release, laser profilometry, and neutron radiography—have been qualified for all available experiments in FIPD, and the U.S. nuclear industry can now draw on them with confidence in licensing activities for metallic fuel-based advanced fast reactors. This report documents the qualification process and the resulting status of the PIE data.

Mo, Kun↗

NASA NTRS1989

Improved silicon carbide for advanced heat engines

The development of high strength, high reliability silicon carbide parts with complex shapes suitable for use in advanced heat engines is studied. Injection molding was the forming method selected for the program because it is capable of forming complex parts adaptable for mass production on an economically sound basis. The goals were to reach a Weibull characteristic strength of 550 MPa (80 ksi) and a Weibull modulus of 16 for bars tested in four-point loading. Statistically designed experiments were performed throughout the program and a fluid mixing process employing an attritor mixer was developed. Compositional improvements in the amounts and sources of boron and carbon used and a pressureless sintering cycle were developed which provided samples of about 99 percent of theoretical density. Strengths were found to improve significantly by annealing in air. Strengths in excess of 550 MPa (80 ksi) with Weibull modulus of about 9 were obtained. Further improvements in Weibull modulus to about 16 were realized by proof testing. This is an increase of 86 percent in strength and 100 percent in Weibull modulus over the baseline data generated at the beginning of the program. Molding yields were improved and flaw distributions were observed to follow a Poisson process. Magic angle spinning nuclear magnetic resonance spectra were found to be useful in characterizing the SiC powder and the sintered samples. Turbocharger rotors were molded and examined as an indication of the moldability of the mixes which were developed in this program.

Whalen, Thomas J.↗

DOE OSTI2019

Embedded Fiber-Optic Sensors for In-Pile Applications

Qualification and commercialization of new nuclear fuels and materials requires a comprehensive set of data regarding behavior under irradiation. There are currently very limited options for in-situ monitoring of material evolution during irradiation due to the extremely harsh environment (i.e., high temperatures and intense radiation) of materials test reactors. This paper describes work being performed at Oak Ridge National Laboratory to embed metal-coated fiber-optic sensors into in-core irradiation experiments to enable measurement of radial dimensional changes and spatially distributed temperature and strain. Some critical issues that must be addressed before embedded fiber optics can be deployed in-core include (1) embedding of metal-coated fibers without failure or prohibitively large signal attenuation, (2) embedding in curved channels to allow for radial dimensional measurements, and (3) demonstrating that embedded fibers can survive the large stresses that result from differential thermal expansion between the glass fiber and the surrounding metal matrix. This work shows how optical fibers have been successfully embedded in aluminum and copper alloys in both straight and curved channels with various bend radii. The embedded fibers have also survived heating to temperatures of 500°C and cooling to room temperature. This paper presents some of the experimental results including measured light attenuation resulting from embedding with and without bends and high-temperature testing.

Petrie, Christian↗