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At least 487 records · Page 27

Milestone 1.2.9: Radiolytic Gas Generation Measurements from Helium Backfilled Samples of AA1100 and AA6061 Coupons

Nearly 18 metric tons of aluminum-clad spent nuclear fuel (ASNF) is safely managed by the U.S. Department of Energy (DOE). These assemblies are currently in interim storage, with the intention of extended storage (>50 years) until final disposal. Strategies for the continued safe storage of this material are under evaluation, of which a key criterion is the extent of molecular hydrogen gas (H2) formation from the radiolysis of hydrated (oxy)hydroxide aluminum corrosion layers arising from in-reactor and wet storage conditions. Radiation-induced H2 formation has the potential to compromise cladding and storage canister integrity, in addition to promoting the formation of unfavorable gaseous environments. Consequently, understanding this radiation-induced phenomenon is essential for the development of predictive modeling capabilities to support technical considerations and the identification of radiation related challenges for the extended storage of ASNF. Here, we report radiolytic H2 yields (G-values, G(H2)) from the gamma irradiation of ‘pristine’ and pre-corroded aluminum coupons in helium (He) environments as a function of alloy composition (AA1100 and AA6061), relative humidity, and absorbed gamma dose. Measured yields were lower than corresponding values reported for argon environments, a positive result for proposed extended dry storage strategies that would employ helium as a backfill gas. Interestingly, the presented G(H2)He values are comparable to those previously measured in nitrogen environments, suggesting a He mediated H2 inhibition process, attributed here to Penning ionization.

38 RADIATION CHEMISTRY, RADIOCHEMISTRY, AND NUCLEA↗

VAPoR - Volatile Analysis by Pyrolysis of Regolith - an Instrument for In Situ Detection of Water, Noble Gases, and Organics on the Moon

We present the Volatile Analysis by Pyrolysis of Regolith (VAPoR) instrument design and demonstrate the validity of an in situ pyrolysis mass spectrometer for evolved gas analyses of lunar and planetary regolith samples. In situ evolved gas analyses of the lunar regolith have not yet been carried out and no atmospheric or evolved gas measurements have been made at the lunar poles. VAPoR is designed to do both kinds of measurements, is currently under development at NASA's Goddard Space Flight Center, and will be able to heat powdered regolith samples or rock drill fines up to 1400 C in vacuo. To validate the instrument concept, evolved gas species released from different planetary analogs were determined as a function of temperature using a laboratory breadboard. Evolved gas measurements of an Apollo 16 regolith sample and a fragment of the carbonaceous meteorite Murchison were made by VAPoR and our results compared with existing data. The results imply that in situ evolved gas measurements of the lunar regolith at the polar regions by VAPoR will be a very powerful tool for identifying water and other volatile signatures of lunar or exogenous origin as potential resources for future human exploration.

ten Kate, I. L.↗

Disassembly and Initial Post-Irradiation Examination of the Mini99 Experiment

The Miniature Fuel Molybdenum-99 (Mini99) experiment is a first-of-a-kind experiment in the High Flux Isotope Reactor. Mini99 is the first MiniFuel irradiation experiment to use liquid metal inside the MiniFuel subcapsule for additional temperature control. In this work, the initial post-irradiation examination is reported. As-built simulations were conducted and compared with designs, and physical post-irradiation examinations were conducted to determine actual test temperatures via SiC thermometry samples, to evaluate the extent of fission gas release from the samples, and to remove the fuel from the subcapsules. As-built simulations compared well with experiment designs and were in reasonable agreement with the measured temperatures inferred from the passive SiC thermometers. Additionally, fission gas release values were relatively small (on the order of 3%); one sample reached approximately 8%. Although some of this behavior is attributable to recoil, most of the gas release was likely caused by the physics of the fuel behavior during the test. Finally, disassembly showed that at least four of the fuel samples degraded into small components and granules at some point during the test, with the state of the other two samples unproven. Additional work is planned for further examination of these samples via various microscopy techniques.

11 NUCLEAR FUEL CYCLE AND FUEL MATERIALS↗

NOAA WP-3D instrumentation and flight operations on AGASP-II

One component of the second Arctic Gas and Aerosol Sampling Program conducted in March and April 1986 was supported with an instrumented NOAA WP-3D atmospheric research aircraft, which was used to conduct measurements of wind, temperature, ozone, water vapor, the concentration of condensation nuclei, and aerosol scattering extinction coefficient in order to determine the locations and properties of haze layers. The WP-3D flights consisted of three missions north of Alaska and three in the Canadian Arctic near Alert. This paper describes the NOAA WP-3D aircraft; the meteorological, gas, and aerosol sampling systems utilized; and the flight operations of the six WP-3D flights.

Schnell, R. C.↗

Evaluation of the Interference of Tenax®TA Adsorbent With Dimethylformamide Dimethyl Acetal Reagent for Gas Chromatography-Dragonfly Mass Spectrometry and Future Gas Chromatography-Mass Spectrometry in Situ Analysis

Among future space missions, national aeronautics and space administration (NASA) selected two of them to analyze the diversity in organic content within Martian and Titan soil samples using a gas chromatograph – mass spectrometer (GC–MS) instrument. The Dragonfly space mission is planned to be launched in 2027 to Titan's surface and explore the Shangri-La surface region for years. One of the main goals of this mission is to understand the past and actual abundant prebiotic chemistry on Titan, which is not well characterized yet. The ExoMars space mission is planned to be launched in 2028 to Mars’ surface and explore the Oxia Planum and Mawrth Vallis region for years. The main objectives focus on the exploration of the subsurface soil samples, potentially richer in organics, that might be relevant for the search of past life traces on Mars where irradiation does not impact the matrices and organics. One recently used sample pre-treatment for gas chromatography – mass spectrometry analysis is planned on both space missions to detect refractory organic molecules of interest for astrobiology. This pre-treatment is called derivatization and uses a chemical reagent – called dimethylformamide dimethyl acetal (DMF-DMA) – to sublimate organic compounds keeping them safe from thermal degradation and conserving the chirality of the molecules extracted from Titan or Mars’ matrices. Indeed, the detection of building blocks of life or enantiomeric excess of some organics (e.g. amino acids) after DMF-DMA pre-treatment and GC–MS analyses would be both bioindicators. The main results highlighted by our work on DMF-DMA and Tenax®TA interaction and efficiency to detect organic compounds at ppb levels in a fast and single preparation are first that Tenax®TA did not show the onset of degradation until after 150 experiments – a 120 h at 300 °C experiment – which greatly exceeds the experimental lifetimes for the DraMS and GC-space in situ investigations. Tenax®TA polymer and DMF-DMA produce many by-products (about 70 and 46, respectively, depending on the activation temperature). Further, the interaction between the two leads to the production of 22 additional by-products from DMF-DMA degradation, but these listed by-products do not prevent the detection of trace-level organic molecules after their efficient derivatization and volatilization by DMF-DMA in the oven ahead the GC–MS trap and column.

DraMS-Dragonfly mission↗

Assessment of Thin Plastic Scintillation Detectors for Beta-Particle Measurements at the Advanced Test Reactor Critical Facility

The Fission Wire Measurement System is a custom measurement system designed in the 1960s to measure the beta-particle activity of irradiated uranium-aluminum fission wires. This measurement is conducted to determine the fission rate profile of the Advanced Reactor Test Critical facility. The Advanced Test Reactor Critical facility is an open-pool, low-power test reactor used to qualify experiment configurations and verify core models prior to full-power experiment irradiations in the Advanced Test Reactor. Power distribution measurements in ATR-C use uranium-aluminum wires that are distributed throughout the core to validate simulation and modeling results. These measurements require from 340 to 1500 wires to be irradiated and measured within a 12-hour window. The system consists of 4 measurement channels and one reference channel, each with a 2-pi proportional gas flow detector and the measurement channels each have an automated sample changer. The gas flow detectors are of a custom design for this detector system that use methane gas with a large anode wire compared to modern proportional counters. These detectors, which are nearly 60 years old are irreplaceable. The measurements from these gas detectors are affected by the gas flow rate, atmospheric and line pressure, and are very sensitive to the applied high voltage. Recent improvements have been made to the control and data acquisition system, but the detectors have remained the same. The nature of the measurement of the fission product decay activity is such that the energy spectrum of the signal is changing with time. Thin, 250-um thick, plastic scintillators were commercially obtained as a potential replacement for the gas flow detectors. The original calibration of the uranium-aluminum fission wires was conducted in 1965 using a series of irradiations of gold foils and the wires in a well-characterized thermal neutron field. These measurements provided a time-dependent fission rate conversion factor from the gold foil data to calibrate the fission wires based on the response from the 2-pi proportional gas detectors. Transitioning to the new detectors requires qualification and testing. The sensitivity of the scintillators to changes in the energy spectrum of the fission wires and translation of the calibration factor have been completed. These measurements indicated that the sensitivity of the scintillators over time changes at a different rate than the sensitivity of the gas flow detectors. However, the inverse activity of measurements of both detector types is linear with time. Initial results indicate that the scintillator detectors will be a sufficient replacement for the gas detectors with minor adjustments to the fission rate conversion factor. Replacement of the detectors will improve the fission wire measurements and provide a more stable and reliable measurement system.

46 - INSTRUMENTATION RELATED TO NUCLEAR SCIENCE AN↗

Research on miniature gas analysis systems

Technology for fabricating very small valves, whose function will be to introduce a small sample of the gas to be analyzed into the main carrier gas stream flowing through the chromatograph column is described. In addition, some analyses were made of the factors governing the resolution of gas chromatographs, particularly those with miniature columns. These analyses show how important the column lining thickness is in governing the ability of a miniature column to separate components of an unknown gas. A brief description of column lining factors is included. Preliminary work on a super small thermistor detector is included.

Angell, J. B.↗

Two-stage gas measurement system

A quick-response, real-time gaseous measurement system allows for the continuous sampling of a low pressure gaseous environment. A sample of test gas from the low pressure gaseous environment is continuously extracted and pumped to a structural tee joint which is open to the atmosphere at one end to maintain the test gas at a constant pressure. The structural tee joint communicates at the other end with a heater for maintaining the test gas at a constant temperature. From the heater, the test gas is sent to a sensor which develops a voltage that is proportional to the partial pressure of the gaseous component to be measured in the test gas, a constant flow rate of test gas being provided through the heater and sensor. Since test gas pressure, temperature, and flow rate are being held constant, changes in sensor voltage are attributable only to changes in the concentration of the measured gas component.

Sprinkle, Danny R.↗

Differential thermal analysis and gas release studies of Apollo 11 samples.

The liquidus-solidus behavior of Apollo 11 lunar fines and the evolution characteristics of CO, nitrogen, He, Ne, and Ar were investigated by use of the combined techniques of high-vacuum differential thermal analysis (DTA) and mass spectrometry between 100 and 1500 C. The DTA thermogram has shown that the lunar fines undergo partial melting over a broad range of temperature from about 915 to 1300 C, with a significant initial melting of glassy and crystalline components within the fines at about 1140 C. The lunar material becomes a homogeneous melt at about 1300 C.

Wachi, F. M.↗

An NMR Study of Microvoids in Polymers

An understanding of polymer defect structures, like microvoids in polymeric matrices, is most crucial to their fabrication and application potential. In this project guest atoms are introduced into the microvoids in PMR-15 and NMR is used to determine microvoid sizes and locations. Xenon is a relatively inert probe that would normally not be found naturally in polymer or in NMR probe materials. There are two NMR active Xenon isotopes, Xe-129 and Xe-131. The Xe atom has a very high polarizability, which makes it sensitive to the intracrystalline environment of polymers. Interactions between the Xe atoms and the host matrix perturb and Xe electron cloud, deshielding the nuclei, and thereby expanding the range of the observed NMR chemical shifts. This chemical shift range which may be as large as 5000 ppm, permits subtle structural and chemical effects to be studied with high sensitivity. The Xe-129-NMR line shape has been found to vary in response to changes in the pore symmetry of the framework hosts in Zeolites and Clathrasil compounds. Before exposure to Xe gas, the PMR-15 samples were dried in a vacuum oven at 150 C for 48 hours. The samples were then exposed to Xe gas at 30 psi for 72 hours and sealed in glass tubes with 1 atmosphere of Xenon gas. Xenon gas at 1 atmosphere was used to tune up the spectrometer and to set up the appropriate NMR parameters. A series of spectra were obtained interspersed with applications of vacuum and heating to drive out the adsorbed Xe and determine the role of Xe-Xe interactions in the observed chemical shift.

Toy, James↗

Rarefied piezometric uptake apparatus and method for measuring gaseous uptake

A rarefied piezometric uptake apparatus and method for measuring gaseous uptake for large solid samples with little or no sample preparation. Past systems and methods require extensive sample preparation. The method includes providing a rarefied piezometric uptake apparatus having a dosing chamber and uptake chamber in an improved selective fluid communication. The apparatus and method improve the measurement of gaseous uptake into solid samples resulting in improved prediction of gas migration through solid samples such as geologic formations.

Paul, Matthew J.↗

A versatile system for biological and soil chemical tests on a planetary landing craft. II - Hardware development

A system has been under development which is designed to seek remotely for clues to life in planetary soil samples. The basic approach is a set of experiments, all having a common sensor, a gas analysis mass spectrometer which monitors gas composition in the head spaces above sealed, temperature controlled soil samples. Versatility is obtained with up to three preloaded, sealed fluid injector capsules for each of eleven soil test cells. Tests results with an engineering model has demonstrated performance capability of subsystem components such as soil distribution, gas sampling valves, injector mechanisms, temperature control, and test cell seal.

Martin, J. P.↗

Properties of a constricted-tube air-flow levitator

The properties of a constricted-tube gas flow levitator first developed by Berge et al. (1981) have been investigated experimentally in order to predict its behavior in a gravity-free environment and at elevated temperatures. The levitator consists of a constricted (quartz) tube fed at one end by a source of heated air or gas. A spherical sample is positioned by the air stream on the downstream side of the constriction, where it can be melted and resolidified without touching the tube. It is shown experimentally that the kinematic viscosity is the important fluid parameter for operation in thermal equilibrium at high temperatures. If air is heated from room temperature to 1200 C, the kinematic viscosity increases by a factor of 14. To maintain a given value of the Reynolds number, the flow rate would have to be increased by the same factor for a specific geometry of tube and sample. Thus, to maintain stable equilibrium, the flow rate should be increased as the air or other gas is heated. The other stability problem discussed is associated with changes in the shape of a cylindrical sample as it melts.

Rush, J. E.↗

Pseudo continuous wave instrument

Acoustic properties and their changes in a sample of liquid, gas, plasma or solid are measured by applying a variable frequency source to the sample by means of a transducer to produce sound waves within the sample. The application of the variable frequency source to the sample is periodically interrupted for a short duration. Means are connected to the transducer for receiving the resulting acoustic signals during the interruptions for producing a control signal indicative of a difference in the frequency of the output of the variable frequency source and the frequency of a mechanical resonant peak in the sample. The control signal is applied to the variable frequency source to maintain its output frequency at the frequency of the mechanical resonant peak. The change in frequency of the variable frequency source indicates the shift in frequency of the mechanical resonant peak and the amplitude of the acoustic signals indicates the attenuation of the acoustic signals in the sample.

Heyman, J. S.↗

A Fully Redundant On-Line Mass Spectrometer System Used to Monitor Cryogenic Fuel Leaks on the Space Shuttle

This paper presents an on-line mass spectrometer designed to monitor for cryogenic leaks on the Space Shuttle. The topics include: 1) Hazardous Gas Detection Lab; 2) LASRE Test Support; 3) Background; 4) Location of Systems; 5) Sample Lines for Gas Detection; 6) Problems with Current Systems; 7) Requirements for New System (Nitrogen and Helium Background); and 8) HGDS 2000. This paper is in viewgraph form.

Griffin, T. P.↗

In situ measurements of thermospheric composition, temperature, and winds by mass spectrometry

Mass spectrometry, in which a beam of electrons ionizes a sample of atmospheric gas and then analyses the ions thus produced to determine the concentration of each species in the sample, is presently evaluated as a basis for the study of earth atmosphere and other planetary atmospheres' properties. Recent applications of in situ mass spectrometry have measured thermospheric neutral gas composition, temperatures, and winds, with a spatial resolution sufficiently high to reveal previously unsuspected atmospheric variability. It is expected that analyses of these data will lead to a more detailed understanding of the deposition processes governing the thermosphere's highly variable structure.

Spencer, N. W.↗

OSIRIS-REx Curation: The First Year with Bennu Samples on Earth

The OSIRIS-REx (Origins, Spectral Interpretation, Resource Identification, and Security – Regolith Explorer) sample return capsule landed on the Utah Test and Training Range (UTTR) on September 24, 2023. Preparations for the curation of the sample from asteroid Bennu inside of this capsule spanned more than a decade. On the morning of landing, the sample return capsule was brought to a temporary cleanroom at UTTR for initial de-integration and connection of the sample canister to a nitrogen gas purge to protect the sample from modification by the terrestrial atmosphere. In the week following landing, the sample canister was flown to Houston while on nitrogen purge, transferred to a nitrogen atmosphere glovebox at NASA Johnson Space Center in which the canister lid was removed revealing small amounts of sample on the inside of the canister lid and avionics deck, some of this sample was allocated rapidly to the mission sample analysis team as “quick look” samples. Next, the Touch-and-Go sample acquisition mechanism (TAGSAM) head was disassembled inside of a specially designed glovebox. A challenge arose during one of the last stages of disassembly when two fasteners resisted being loosened. The curation team was able to remove 70.3 grams of asteroid sample from the TAGSAM head with those fasteners in-place and began initial sample processing which supported long-term curation of hermetically sealed and frozen samples, transfer of some samples to remote storage, and allocation of aggregate samples to the mission sample analysis team. Meanwhile, curation engineers developed a tool to remove the stubborn fasteners without contaminating the remaining sample, enabling the remaining bulk sample to be transferred to long-term storage trays in January 2024. With this second part of the bulk sample, the returned bulk asteroid sample reached 121.6 grams. During disassembly and prior to sealing the bulk sample trays into long-term storage containers, archival photographs were collected. Select particles are gradually being XCT scanned while inside of containers that hold a nitrogen atmosphere. The initial OSIRIS-REx sample catalog was released in spring 2024 with an update in fall 2024. The curation team will be busy working to allocate samples to scientists around the world for the foreseeable future.

Curation↗