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At least 55 records · Page 3

Transport of Highly Volatile Gases Related to Noble Gases and Tritium in the MSRE

This study aims to comprehend mass transfer in the closed-loop circulation of highly volatile gases, including noble gases and tritium. We explore the impact of steady-state xenon-135 and tritium on the MSRE and reveal their isotopic distributions using online noble gas stripping of fuel salts. The MSRE was engineered to extract fission product gases from fuel salts and efficiently eliminate inert gases with the help of helium bubbles within a circulating fuel pump. These reactors introduce significant theoretical challenges in estimating interfacial area and mass transfer coefficients, crucial for modeling mass transfer processes. An essential component of our analysis is the mass transfer coefficient. These coefficients are important for understanding how radionuclides move during various phase transitions within a nuclear reactor. Xenon-135 and tritium are found in both liquid and gas phases within the reactor system. In the liquid phase, they dissolve in molten salts, while in the gas phase, they manifest as bubbles. These elements have significant adverse effects on reactor operation due to their strong neutron absorption properties, influencing both safety and performance. The Mole code, which predicts the behavior of chemical species under steady-state conditions, facilitates multiphysics coupling with Griffin to update species distributions and address inherent MSR safety.

Lee, Kyoung↗

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↗

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↗

Pre-Transient Characterization of MLOF-1 Test Pin

This study focuses on the pre-transient characterization of U-10Zr test and sibling fuel pins for the THOR-M-LOF test series. Using neutron radiography, element contact profilometry (ECP), precise gamma scan (PGS), and gas assay, sampling, and recharge (GASR) analysis, it was confirmed that the fuel pins were intact and suitable for testing. Key fuel behaviors quantified include axial elongation, diametral strain, fluff structure geometry, axial isotope distribution, and fission gas release. Any deviations from historically expected behaviors were investigated and attributed to factors other than the irradiation behavior of the fuel pin. These pre-transient measurements establish a baseline for future post-transient analysis, which will be used to inform fuel performance models and safety criteria for sodium-cooled fast reactors (SFRs). The results will enhance understanding of transient fuel behavior and expand limited data on LOF scenarios.

11 - NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Rapidity distributions of Z = 1 isotopes and the nuclear symmetry energy from Sn+Sn collisions with radioactive beams at 270 MeV/nucleon

The rapidity distributions of hydrogen isotopes emitted from central collisions of neutron-rich 132 Sn+ 124 Sn and neutron-deficient 108 Sn+ 112 Sn systems at 270 MeV/nucleon were investigated at RIKEN-RIBF. The data are compared with antisymmetrized molecular dynamics (AMD) calculations and the rapidity distributions can be reproduced after adjusting the in-medium nucleon-nucleon cross sections. The double ratios between the two reaction systems taken for the relative yields of deuteron to proton (d/p) and triton to proton (t/p) are further examined in the midrapidity domain, where the adjustments in the AMD calculations do not affect much on them. The d/p and t/p double ratios at midrapidity agree well with the ratio of the system neutron numbers and its squared value, respectively, and the rapidity dependence of these double ratios is consistent with a picture of partial mixing of colliding nuclei. By comparing with the AMD model which shows a strong symmetry energy dependence of the t/p double ratio, the experimental result in the midrapidity domain favors the calculation with a symmetry-energy slope parameter around L = 46 MeV rather than L = 108 MeV.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Neutron Irradiation Induced Changes in Isotopic Abundance of 6Li and 3D Nanoscale Distribution of Tritium in LiAlO2 Pellets Analyzed by Atom Probe Tomography

Tritium, a radioactive isotope of hydrogen is produced by neutron irradiation of 6Li enriched LiAlO2 pellets in Tritium producing burnable absorber rods (TPBARs). Three-dimensional nanoscale mapping of Tritium in irradiated pellets is critical to understand its spatial variation and its association with various microstructural features in the pellets. Spatially resolved analysis of 6Li isotopic enrichment in such ceramic pellets before and after irradiation can provide insights to heterogeneities in Li isotopic distribution. However, Li being a light isotope, its spatially resolved compositional or isotopic analysis is a challenging task to most analytical methods. Here we used atom probe tomography, to evaluate the Li isotopic enrichment in both the LiAlO¬2 matrix and the Li deficient secondary phase LiAl5O8 before irradiation. These results were then compared with 6Li isotopic ratio measured by APT analysis of neutron irradiated pellets to clearly demonstrate the unique capability of APT to quantitatively analyze the isotopic enrichment of 6Li as well as for other light elements present in these materials. Evidence for heterogenous nanoscale distribution of 3H and O3H within irradiated pellet microstructure is also provided, which is attributed to 3H trapping in irradiation induced vacancy clusters or voids within the LiAlO2 matrix. The characterization results given here, now prove the feasibility for using APT for analyzing nanoscale spatially resolved isotopic enrichment of Li as well as other light elements such as Tritium in TPBARs. This work also paves way to adopt APT for analyzing light elements such as Li and tritium in materials used for nuclear fusion reactor applications, geochemistry, astrophysics as well as for energy storage applications.

Devaraj, Arun↗

Triple oxygen isotope compositions of globally distributed soil carbonates record widespread evaporation of soil waters

The stable isotopic composition of pedogenic carbonates is central to many studies of past climate and topography, providing a basis for our understanding of Earth's terrestrial history. A core assumption of many applications of oxygen isotope values (δ 18 O) of pedogenic carbonate is that they reflect the δ 18 O value of precipitation (rain/snow). Here, this assumption is violated if soil carbonates form in evaporated soil waters. In this work, we develop a means to identify evaporation in ancient soils using the triple oxygen isotope composition ( 16 O- 17 O- 18 O) of pedogenic carbonates.

58 GEOSCIENCES↗

First Examination of Irradiated Fuel with Pulsed Neutrons at LANSCE (Preliminary Results)

We present preliminary results on the characterization of an irradiated U-lOZr-lPd fuel sample that was prepared from the irradiated AFC-3A-R5A sample. U-lOZr metallic fuels are researched as host materials for potential transmutation fuels and the addition of palladium strives to bind lanthanides, thus preventing fuel-cladding chemical interactions (FCCI). These interactions limit the lifetime of metallic fuels and are caused by migration of lanthanide fission products to the periphery of the fuel slug, where they start to interact with the D9 or HT9 steel cladding, ultimately leading to failure of the mechanical integrity of the cladding. Neutrons offer bulk characterization of irradiated materials for which X-ray tomography methods are not suitable due to the immense gamma background emitted from the samples. In particular pulsed neutrons provide information from the ability to resolve the neutron energy using their time-of-flight and thus the potential to utilize neutron absorption resonance to characterize the spatial distribution of isotopes. This, in turn, may allow to characterize the distribution of fission and neutron capture products non-destructively and may ultimately be applied to the bulk of an irradiation capsule prior to destructive post-irradiation examination to identify regions of interest. To allow the characterization of entire irradiation capsules, a cask is under development in the advanced post-irradiation work package at LANL and progress on this development was reported elsewhere. In parallel, an irradiated U-lOZr-lPd sample cut from the AFC-3AR5A irradiation was shipped to LANL and will be fully characterized with an NSUF funded rapid turnaround experiment (RTE) in the 2020 LANSCE run cycle. The sample emits at a dose rate of ~3R/hr on contact and is therefore manageable with remote handling, without requiring a cask. The disk-shaped material is larger than samples prepared for analysis using electron or X-ray methods and is therefore an intermediate step towards characterization of bulk samples at LANSCE. However, since it covers the full diameter of the irradiated fuel slug, some insight on redistribution of elements, spatially resolved information on microstructure, e.g. phase composition and texture, will be possible using the pulsed neutron-based methods developed for fuel characterization at LANSCE. This report describes the development of procedures to handle the sample at LANSCE as well as preliminary data and results from tests conducted in December 2019 on the energy-resolved neutron imaging (ERNI) beam line at flight path 5 and the high pressure-preferred orientation diffractometer (HIPPO) at LANSCE. This effort is a collaboration between LANL, INL, and ORNL. To compare our capabilities with prior work, we present an overview of previously reported bulk characterization of irradiated or spent fuels. The overview addresses neutron diffraction and neutron absorption resonance spectroscopy, both of which have only few reported applications on irradiated or spent nuclear fuel, as well as neutron radiography. This literature review was already described in a previous report but is repeated here to put our current efforts in context of previous work.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

A statistical approach to screening isotopic signatures in monitoring for underground nuclear explosions

The ability to differentiate between atmospheric radionuclide signatures from underground nuclear explosions (UNEs) and signals from other sources, such as medical isotope-production facilities and nuclear reactors, can be critical to the detection and monitoring of unannounced, low-yield nuclear events. Signatures having anomalously high amplitudes, compared to background levels, remain the best indicator in screening for a UNE. However, isotopic composition can further validate a suspected UNE signature, but separation from any atmospheric background composition is first necessary. To date, evaluating the challenges of performing this separation has typically involved comparing an observed background with a highly idealized deterministic model of radioxenon signature production by a UNE that does not consider the influence of post-detonation chemical/physical processes in the detonation cavity or the subsequent gas transport mechanisms that can also affect the isotopic composition of the detected gas signature. In addition, purely deterministic models, as previously employed, overlook the uncertainty inherent in estimating critical parameters characterizing the UNE and its detonation environment. In this paper, we create detailed, multi-parameter models of radionuclide evolution using the widely accepted England and Rider post-detonation radionuclide decay-chain network coupled to detailed models simulating physical production and transport processes affecting the gas signature. Because these models are governed by uncertain parameters including barometric fluctuations, realistic ranges of variation for each of the parameters influencing isotopic composition are then defined. A Latin-Hypercube sampling approach is used to obtain a random distribution of isotopic production and gas transport results associated with a given value of each parameter. We apply these results to background histories of two stations, one providing 4-isotope background measurements and the other providing two-isotope measurements associated with the 2013 DPRK announced UNE.

98 NUCLEAR DISARMAMENT, SAFEGUARDS, AND PHYSICAL P↗

Isotope engineering for spin defects in van der Waals materials

Abstract Spin defects in van der Waals materials offer a promising platform for advancing quantum technologies. Here, we propose and demonstrate a powerful technique based on isotope engineering of host materials to significantly enhance the coherence properties of embedded spin defects. Focusing on the recently-discovered negatively charged boron vacancy center ($${{{{{{{{\rm{V}}}}}}}}}_{{{{{{{{\rm{B}}}}}}}}}^{-}$$ V B − ) in hexagonal boron nitride (hBN), we grow isotopically purified h 10 B 15 N crystals. Compared to$${{{{{{{{\rm{V}}}}}}}}}_{{{{{{{{\rm{B}}}}}}}}}^{-}$$ V B − in hBN with the natural distribution of isotopes, we observe substantially narrower and less crowded$${{{{{{{{\rm{V}}}}}}}}}_{{{{{{{{\rm{B}}}}}}}}}^{-}$$ V B − spin transitions as well as extended coherence timeT 2 and relaxation timeT 1 . For quantum sensing,$${{{{{{{{\rm{V}}}}}}}}}_{{{{{{{{\rm{B}}}}}}}}}^{-}$$ V B − centers in our h 10 B 15 N samples exhibit a factor of 4 (2) enhancement in DC (AC) magnetic field sensitivity. For additional quantum resources, the individual addressability of the$${{{{{{{{\rm{V}}}}}}}}}_{{{{{{{{\rm{B}}}}}}}}}^{-}$$ V B − hyperfine levels enables the dynamical polarization and coherent control of the three nearest-neighbor 15 N nuclear spins. Our results demonstrate the power of isotope engineering for enhancing the properties of quantum spin defects in hBN, and can be readily extended to improving spin qubits in a broad family of van der Waals materials.

Science & Technology - Other Topics↗

Polycyclic aromatic hydrocarbons in samples of Ryugu formed in the interstellar medium

Polycyclic aromatic hydrocarbons (PAHs) contain ≲20% of the carbon in the interstellar medium. They are potentially produced in circumstellar environments (at temperatures ≳1000 kelvin), by (~10 kelvin) interstellar clouds, or by processing of carbon-rich dust grains. We report isotopic properties of PAHs extracted from samples of the asteroid Ryugu and the meteorite Murchison. The doubly- 13 C substituted compositions (Δ2× 13 C values) of the PAHs naphthalene, fluoranthene, and pyrene are 9 to 51‰ higher than values expected for a stochastic distribution of isotopes. The Δ2× 13 C values are higher than expected if the PAHs formed in a circumstellar environment, but consistent with formation in the interstellar medium. By contrast, the PAHs phenanthrene and anthracene in Ryugu samples have Δ2× 13 C values consistent with formation by higher-temperature reactions.

Science & Technology - Other Topics↗

Reconciling evidence of oxidative weathering and atmospheric anoxia on Archean Earth

Evidence continues to emerge for the production and low-level accumulation of molecular oxygen (O 2 ) at Earth’s surface before the Great Oxidation Event. Quantifying this early O 2 has proven difficult. Here, we use the distribution and isotopic composition of molybdenum in the ancient sedimentary record to quantify Archean Mo cycling, which allows us to calculate lower limits for atmospheric O 2 partial pressures ( P O 2 ) and O 2 production fluxes during the Archean. We consider two end-member scenarios. First, if O 2 was evenly distributed throughout the atmosphere, then P O 2 > 10 –6.9 present atmospheric level was required for large periods of time during the Archean eon. Alternatively, if O 2 accumulation was instead spatially restricted (e.g., occurring only near the sites of O 2 production), then O 2 production fluxes >0.01 Tmol O 2 /year were required. Archean O 2 levels were vanishingly low according to our calculations but substantially above those predicted for an abiotic Earth system.

58 GEOSCIENCES↗

SCALE 6.2 Lattice Physics Performance Assessment

The US Nuclear Regulatory Commission relies on the lattice physics analysis capabilities of the SCALE code system to perform confirmatory licensing analyses. Either SCALE lattice physics code—TRITON/NEWT or Polaris—can be used to generate cross section data used by the PARCS nodal core simulator for full-core neutronics calculations. This report presents an assessment of the accuracy of SCALE lattice physics codes for preparation of lattice physics data that are used to support simulator codes such as the NRC’s PARCS, for UO 2 -mixed oxide (MOX)/Zr fueled light water reactor (LWR) analyses. Due to the nature of lattice physics calculations, critical reactor experiment benchmarks cannot be modeled in explicit detail in a lattice physics code. However, this limitation does not mean that these measurement data are not usable for lattice physics studies. Therefore, either geometry approximations or axial buckling must be implemented to determine the critical water height. These modeling limitations have led to development of a three-phase assessment strategy. In the first phase, selected critical experiment benchmarks are modeled using the SCALE 3D continuous-energy (CE) Monte Carlo (MC) code KENO, which is the most rigorous neutron transport method available in SCALE, with no approximations in the spatial, angle, or energy treatments. Biases and statistical uncertainties in quantities of interest such as k eff and pin power distributions are determined by comparing CE KENO results to experimental data. This first phase in the accuracy assessment is to demonstrate and establish the use of CE KENO as a reference solution for the second phase. In the second phase, 14 numerical test suites are used to compare SCALE lattice physics calculations with CE KENO as a reference solution. In the third phase, SCALE lattice physics depletion calculations are performed, and the spent fuel isotopic results are compared with available radiochemical assay measurements. Isotopic measurement comparisons provide quantitative assessment of isotopic density distribution predictions with the depletion models in SCALE lattice physics codes. This report documents results for all test suites. The assessment was performed using standard production techniques unless otherwise noted. Both TRITON/NEWT and Polaris exhibited acceptable accuracy for most test cases. For the few test cases in which acceptable accuracy criteria were not met, further code and data development are planned. The computer codes used in this assessment are as follows: SCALE 6.2 rev19189 (pre-release of 6.2.1) was used for CE KENO, TRITON/NEWT and Polaris (PWR only) calculations; SCALE 6.2.2 was used for Polaris calculations to address several updates in support of support boiling water reactor (BWR) lattice geometries. For this work, there is no difference between SCALE 6.2.1 and SCALE 6.2.2 beyond the inclusion of the Polaris BWR analysis capability; The ENDF/B-VII.1 continuous energy and 252 group libraries deployed in SCALE 6.2 were generated with AMPX 6.2 that is distributed with SCALE.

73 NUCLEAR PHYSICS AND RADIATION PHYSICS↗

Calcareous organic matter coatings sequester siderophores in alkaline soils

Although most studies on organic matter stabilization in soils have focused on adsorption to aluminosilicate and iron oxide minerals due to their strong interactions with organic nucleophiles, stabilization within alkaline soils has been empirically correlated with exchangeable Ca concentrations. Yet the extent of competing processes within natural soil remain unclear. We employed sub-micron scale techniques to investigate the minerology and organic carbon on individual fine particles within an alkaline soil from Eastern Washington. XRD, Mössbauer spectroscopy, TEM-EDX-SAED, and XPS analysis demonstrated a mineral assemblage dominated by quartz, feldspars, iron oxides, and calcite. Although exposed Si, Al, and Fe accounted for ~30% of the surface elemental composition, most of the organic carbon and nitrogen was associated with Ca-rich coatings. Adsorption isotherms of two siderophores with the same soil showed greater adsorption of pyoverdine compared with less polar enterobactin. Using NanoSIMS to map the distribution of isotopically labeled siderophores across the surfaces of fine grains, we observed a preference for binding to surfaces heavily coated with organic matter. We propose a mechanism of adsorption by which organic molecules aggregate within calcareous soils via calcium bridging, favoring the stabilization of larger molecules with a greater number of nucleophilic functional groups.

54 ENVIRONMENTAL SCIENCES↗

Understanding Reaction Networks through Controlled Approach to Equilibrium Experiments Using Transient Methods

We report a combined experimental/theoretical approach to studying heterogeneous gas/solid catalytic processes using low-pressure pulse response experiments achieving a controlled approach to equilibrium that combined with quantum mechanics (QM)-based computational analysis provides information needed to reconstruct the role of the different surface reaction steps. We demonstrate this approach using model catalysts for ammonia synthesis/decomposition. Polycrystalline iron and cobalt are studied via low-pressure TAP (temporal analysis of products) pulse response, with the results interpreted through reaction free energies calculated using QM on Fe-BCC(110), Fe-BCC(111), and Co-FCC(111) facets. In TAP experiments, simultaneous pulsing of ammonia and deuterium creates a condition where the participation of reactants and products can be distinguished in both forward and reverse reaction steps. This establishes a balance between competitive reactions for D* surface species that is used to observe the influence of steps leading to nitrogen formation as the nitrogen product remains far from equilibrium. Here, the approach to equilibrium is further controlled by introducing delay timing between NH 3 and D 2 which allows time for surface reactions to evolve before being driven in the reverse direction from the gas phase. The resulting isotopic product distributions for NH 2 D, NHD 2 , and HD at different temperatures and delay times and NH 3 /D 2 pulsing order reveal the role of the N 2 formation barrier in controlling the surface concentration of NH x * species, as well as providing information on the surface lifetimes of key reaction intermediates. Conclusions derived for monometallic materials are used to interpret experimental results on a more complex and active CoFe bimetallic catalyst.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Impurity Monitoring During Multiple Recycles of Mo Targets for Accelerator-Produced Mo-99

Accelerator-based methods have been developed to produce kilocurie quantities of low specific-activity 99 Mo from Mo targets. The irradiation of enriched 100 Mo, in place of nat Mo, greatly reduces the activity of side-reaction products formed from other Mo isotopes, which have a fairly wide distribution of natural isotopic abundances: 92 Mo (14.8%), 94 Mo (9.3%), 95 Mo (15.9%), 96 Mo (16.7%), 97 Mo (9.5%), and 98 Mo (21.4%). The side-reaction impurities of chief concern are 91m Nb and 88 Zr/ 88 Y (from 92 Mo), 92m Nb (from 94 Mo), and 95 Nb, 96 Nb, and 97 Nb (from 98 Mo). The new production technologies also require new chemical processing and purification schemes that emphasize low-waste recycling of the expensive, enriched Mo material.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

Simultaneous Absorption and Desorption Isotherms of Various Hydrogen and Deuterium Mixtures between 20 and 120 °C Are Used to Determine the Activity Coefficients for Palladium-Hydride Solutions

A test bed was constructed to measure the absorption and desorption isotherms for palladium hydride using H 2 , D 2 , and various H 2 /D 2 mixtures for temperatures in the range 20 °C ≤ T ≤ 120 °C. The pressure–composition–temperature isotherms were measured. The pressures obtained with mixtures between each pure isotope were monotonic, yet nonlinear. This nonlinear dependence of total pressure with feed gas protium concentration reveals the mixed isotope hydride system behaves nonideally. A thermodynamic model was adapted from the literature, which accounts for the nonideal nature of the mixed-isotope system. The measured data were used as constraints in this model in order to calculate the protium mole fractions in the hydride phase and the protium activity coefficients for palladium hydride at various temperatures and protium concentrations in the system. Knowing the protium mole fraction and activity coefficients allows for a priori calculation of the isotopologue distribution in the gas phase and the isotope distribution in the hydride phase, given a palladium temperature and equilibrium pressure.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗

Foundations of Molecular 'Isotomics'

The naturally occurring rare isotopes are versions of common elements, such as hydrogen, carbon and oxygen, that contain a larger than usual number of neutrons in their atomic nuclei and therefore are higher in mass than the common atoms of that element. Isotopes exist for most elements and are found in most natural and synthetic materials, but are uneven in their distribution because chemical and physical processes are isotope-selective (e.g., a chemical reaction may proceed more rapidly for one isotope than for another). For this reason, abundances of isotopes in a material of interest can provide a record, or ‘signature’ of various features of that material’s origin and history. These signatures have been used in the geo, life, chemical and physical sciences in a wide variety of ways over close to 8 decades. However, many such applications struggle to reach unique interpretations of isotopic data because multiple factors combine to control a given sample’s overall isotopic content. That is, the factors controlling isotopic content are too numerous and complex to fully constrain from a simple measurement of a material’s isotope abundances. However, the distribution of isotopes within materials, at molecular scales potentially provides a vastly larger number and diversity of constraints on the chemical and physical processes that comprise a material’s history. The rare isotopes may be concentrated into one atomic position in a molecule relative to another, some proportion of molecules in a sample may contain two or more rare isotopes, and those multiply-isotope-substituted forms of molecules may also have uneven distributions of those isotopes across individual atomic sites. For these reasons, even small, seemingly simple molecules, such as sugars, amino acids or drug compounds, actually exist in a vast number of isotopically unique forms (often millions or more), and each one of those forms is in some sense an independent ‘vote’ on that sample’s history. This project has focused on opening this rich archive of information by enabling the creation of routinely and widely applicable ways of measuring and interpreting isotopic structures of molecules. This work has included the development of core technologies and analytical methods, advancing fundamental understanding of the physical and chemical properties of isotopic versions of molecules, and conducting proof of concept studies of illustrative geochemical, cosmochemical and forensic problems in order to show how these technologies, methods and principles come together to solve problems in new ways. A key to the success of this project was the adaptation of ‘Fourier transform mass spectrometry’ (FTMS) to the task of precisely measuring proportions of the rare, naturally occurring isotopic forms of molecules. FTMS is a highly specialized form of mass spectrometry that traps ions within magnetic or electrostatic cavities and, effectively, ‘listens’ (through registering of subtle electrical signals) to the harmonic signals they make while rapidly orbiting within those cavities. These signals have periods that are a function of their mass and strength (or ‘loudness’) that is proportional to their abundances. Thus, these signals constrain relative amounts of molecules that differ in their mass due to various isotopic substitutions. This technology has been essential to the identification of organic molecules in the life, chemical and environmental sciences for over 4 decades, but generally has lacked the control, stability and precision to meaningfully measure rare isotope forms of molecules. This project’s most fundamental contribution has been to modify FTMS, both in terms of hardware and methods, to enable such measurements. The raw data of molecular isotopic structure is tremendously voluminous and complex, so another important activity of this project has been developing the theoretical and data-science tools needed to interpret the data generated by this new form of isotopic measurement. A particularly challenging part of this task has been predicting molecular isotopic structure, as only through the comparison of measurements with predictions can we make progress on hypothesis driven research questions. We have attacked this this prediction task through a combination of first-principles chemical-physics models of the effects of isotope substitution on molecule properties and data-science models that permit us to generalize that chemical physics to cases that have not yet been studied by detailed chemical physics theory. The proof of concept applications we have pursued over the course of this study include biological reactions of amino acids and other biomolecules, non-biological synthesis of organic molecules in extra-terrestrial settings such as meteorites, petroleum geoscience questions concerning the origin and evolution of natural gas, oil and kerogen compounds, and forensic questions such as the sourcing of chemical weapons. The successes of these applications have laid the groundwork for the next phase of this field’s development, which will include larger scale and more ambitious studies of molecular isotopic structure as a means of diagnosing human diseases, such as cancer, and reconstructing detailed interpretations of the origin and evolution of organic molecules in modern and geological environments.

Cesar, Jaime↗