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NASA NTRSDate not supplied

The Effect of Temperature on the Preservation of Volatile-Rich Lunar Samples

Introduction. The Moon’s south pole is a high-priority target for human exploration and scientific study. This interest is, in part, due to the presence of Permanently Shadowed Regions (PSRs), which could contain high concentrations of unique volatiles at cryogenic temperatures [1]. Returned samples from PSRs may include a unique combination of rocks, regolith, and volatile species, providing unprecedented insights into the history of the Solar System and the potential for resource utilization on the Moon. However, because PSR samples are cryogenic up-on collection, lunar polar sample return will eventually require cold stowage for the journey from the Moon to Earth. Without cold stowage, PSR sample return will likely result in phase changes and chemical reactions within the volatile component of the sample, which would negatively impact the resulting scientific studies of those samples. This abstract summarizes the initial results from an ongoing characterization of analog PSR samples at a range of temperatures, with the goal of defining the temperatures needed for a flight cold stowage freezer. Background. Based on remote sensing observations of the Moon [2], south polar PSRs range in temperature from ~120K for small and/or shallow PSRs to ~20K at the most extreme locations in large, deep PSRs. A range of volatiles have been hypothesized to exist at the surface or subsurface of the lunar poles [3-5 and others]. This hypothesis was verified when the LCROSS mission impacted the <50-K PSR in the crater Cabeus, detecting a range of volatiles from water to low condensation temperature species such as H2S and methane [6]. Species such as H2S and ammonia (also detected by LCROSS) are also highly reactive, and increase the likelihood of chemical reactions at elevated (non-cryogenic) temperatures. At the Johnson Space Center’s Planetary Exploration and Astromaterials Research Laboratory (JSC-PEARL), we have developed a volatile-bearing lunar simulant that incorporates several of the species detected by LCROSS [Table 1] mixed cryogenically with the USGS Lunar Highlands Type (LHT) regolith simulant. The new volatile-regolith simulant will be used to assess the degree of sample alteration at room temperature, -20°C, -80°C, and -196°C (liquid nitro-gen), over a two-week period. Room temperature samples represent those likely to be returned during initial missions without cold stowage, -20°C provides an analog to Apollo cold curated samples, -80°C is the temperature of multiple flight payload freezers (e.g., MELFI), and -196°C is analogous to lunar PSRs. Two weeks is an approximation of the time between sample collection and Earth return for initial Artemis missions. Over this period of time, sample head-space gases will be analyzed using a Universal Gas Analyzer (UGA, a type of mass spectrometer) coupled with a Baratron pressure sensor. After testing, the regolith component of the simulant will be purged of volatiles and preserved for future electron beam and/or FTIR analysis. Experimental Procedure. Volatile-regolith simulants will be produced as an initial homogenous batch; this batch will then be distributed into aliquots (gas chromatography/GC vials or cryo vials), ensuring that each sample has the same starting composition and conditions [Fig. 1]. In addition to the “full” simulant shown in Table 1, less complex simulant compositions will be used as baseline and control samples [Table 2]. Aliquots will be produced in triplicate for each simulant composition, storage temperature, and date of sampling. Headspace gases in all Day 0 samples will be analyzed by the UGA immediately. Cold storage samples for future analytical days will be placed in freezers appropriate to their target temperatures (-20°C, -80°C, -196°C). For ambient-temperature samples, regolith and regolith-water samples will be stored in a fume hood, while the full simulant will be stored in a sealed Parr vessel for safety; no other simulants (RWCM/ RWCM+) will be stored at ambient temperature for this test. Samples will be analyzed by UGA in this manner on each Analysis Day outlined in Table 2. Analytical Data. The UGA measures the partial pressures in a single sample aliquot over a set mass range of 0-105 atomic mass units (AMU) [Figure 2]; this set range was selected to slightly exceed the mass of the highest-mass expected reaction product (H2SO4). The Baratron complements the UGA by measuring the total pressure in the headspace of a sample vial. Coupled together, the quantitative abundances of gases will be monitored throughout the test. UGA analyses of the triplicate samples for each storage temperature, day, and simulant composition will be averaged, and standard deviations for each will be calculated. The compositions of starting species (shown in Table 1) will be characterized as a function of time, and the presence of any new compounds (reaction products) will be monitored as well. Total pressures will be recorded for each sample analysis, and any samples that show signs of leakage (e.g., a significant reduction in pressure or simulant volatiles) will be discarded. Anticipated Results. Testing is planned to begin in January 2022. The resulting data will allow compositional and phase changes in the volatile component of the simulants to be determined. Both the reduction in initial compounds and the addition of reaction products are expected to be observed. In addition, the relative efficacy of the different temperatures at pre-serving the initial composition of the simulants will be quantified. Finally, the regolith component of each sample will be argon-purged and stored in a controlled environment for future laboratory analysis. Compositional and morphological changes in the regolith are expected for samples above 0°C. This test will be repeated three times over the course of 2022. Understanding the effect of temperature on both the volatile and regolith components of analog lunar materials will allow requirements for a cold stowage freezer to be developed. The implementation of cold stowage for lunar polar missions will maximize the preservation of returned samples, enabling ground-breaking lunar and Solar System volatiles science for decades to come.

J L Mitchell↗
DOE OSTI2022

A density-wave-like transition in the polycrystalline V 3 Sb 2 sample with bilayer kagome lattice

Recently, transition-metal-based kagome metals have aroused much research interest as a novel platform to explore exotic topological quantum phenomena. Here we report on the synthesis, structure, and physical properties of a bilayer kagome lattice compound V 3 Sb 2 . The polycrystalline V 3 Sb 2 samples were synthesized by conventional solid-state-reaction method in a sealed quartz tube at temperatures below 850 °C. Measurements of magnetic susceptibility and resistivity revealed consistently a density-wave-like transition at T dw ≈ 160 K with a large thermal hysteresis, even though some sample-dependent behaviors were observed presumably due to the different preparation conditions. Upon cooling through T dw , no strong anomaly in lattice parameters and no indication of symmetry lowering were detected in powder x-ray diffraction measurements. This transition can be suppressed completely by applying hydrostatic pressures of about 1.8 GPa, around which no sign of superconductivity was observed down to 1.5 K. Specific-heat measurements revealed a relatively large Sommerfeld coefficient γ = 18.5 mJ∙mol –1 ∙K –2 , confirming the metallic ground state with moderate electronic correlations. Density functional theory calculations indicate that V 3 Sb 2 shows a non-trivial topological crystalline property. Furthermore, our study makes V 3 Sb 2 a new candidate of metallic kagome compound to study the interplay between density-wave-order, nontrivial band topology, and possible superconductivity.

36 MATERIALS SCIENCE↗
NASA NTRS1968

Deflection circuit monitors force on object under water

Capsule containing samples for radiation testing is guided under through a seal to an exact position within a nuclear reactor. A Linear Variable Differential Transformer /LVDT/ flexplate deflection circuit monitors the force on the capsule as it is positioned within the reactor.

Roller, R.↗
NASA NTRS1974

Extendible probe for atmosphere sampling

Sampling probe is extended through small plug in heat shield by loaded bellows to sample planetary atmosphere for compositional analysis and total pressure during entry of space probe. Assembly prevents contamination of sample by gases from pyrotechnic device and serves as sealed plenum for atmospheric pressure sensor.

Jones, W. J.↗
NASA NTRS1976

Viking GC/MS mechanisms design and performance

The Viking Lander gas chromatograph/mass spectrometer will analyze pyrolyzed samples of the Martian surface for organic content. The surface-sample loader and pyrolyzer assembly (SSPLA) is described, along with the major problems encountered during design and testing. Three mechanisms were developed to implement the required SSLPA functions: (1) a soil loader that forces soil from a filled rotating funnel into each of three ovens located on a carriage, (2) a Geneva drive for rotating and precisely indexing the ovens to receive sample, and (3) a toggle-clamp mechanism for sealing the ovens by forcing circular double knife edges into gold sealing surfaces.

Chase, C. P.↗
NASA NTRS1992

Integration mockup and process material management system

Work to define and develop a full scale Space Station Freedom (SSF) mockup with the flexibility to evolve into future designs, to validate techniques for maintenance and logistics and verify human task allocations and support trade studies is described. This work began in early 1985 and ended in August, 1991. The mockups are presently being used at MSFC in Building 4755 as a technology and design testbed, as well as for public display. Micro Craft also began work on the Process Material Management System (PMMS) under this contract. The PMMS simulator was a sealed enclosure for testing to identify liquids, gaseous, particulate samples, and specimen including, urine, waste water, condensate, hazardous gases, surrogate gasses, liquids, and solids. The SSF would require many trade studies to validate techniques for maintenance and logistics and verify system task allocations; it was necessary to develop a full scale mockup which would be representative of current SSF design with the ease of changing those designs as the SSF design evolved and changed. The tasks defined for Micro Craft were to provide the personnel, services, tools, and materials for the SSF mockup which would consist of four modules, nodes, interior components, and part task mockups of MSFC responsible engineering systems. This included the Engineering Control and Life Support Systems (ECLSS) testbed. For the initial study, the mockups were low fidelity, soft mockups of graphics art bottle, and other low cost materials, which evolved into higher fidelity mockups as the R&D design evolved, by modifying or rebuilding, an important cost saving factor in the design process. We designed, fabricated, and maintained the full size mockup shells and support stands. The shells consisted of cylinders, end cones, rings, longerons, docking ports, crew airlocks, and windows. The ECLSS required a heavier cylinder to support the ECLSS systems test program. Details of this activity will be covered. Support stands were designed and built for each module to sufficiently move and rotate each module. Secondary structures such as floors, ceilings, bulkheads, standoffs, racks, etc. were developed and built.

Verble, Adas James, Jr.↗
NASA NTRS2002

Renal effects of fresh water-induced hypo-osmolality in a marine adapted seal

With few exceptions, marine mammals are not exposed to fresh water; however quantifying the endocrine and renal responses of a marine-adapted mammal to the infusion of fresh water could provide insight on the evolutionary adaptation of kidney function and on the renal capabilities of these mammals. Therefore, renal function and hormonal changes associated with fresh water-induced diuresis were examined in four, fasting northern elephant seal ( Mirounga angustirostris) (NES) pups. A series of plasma samples and 24-h urine voids were collected prior to (control) and after the infusion of water. Water infusion resulted in an osmotic diuresis associated with an increase in glomerular filtration rate (GFR), but not an increase in free water clearance. The increase in excreted urea accounted for 96% of the increase in osmotic excretion. Following infusion of fresh water, plasma osmolality and renin activity decreased, while plasma aldosterone increased. Although primary regulators of aldosterone release (Na(+), K(+) and angiotensin II) were not significantly altered in the appropriate directions to individually stimulate aldosterone secretion, increased aldosterone may have resulted from multiple, non-significant changes acting in concert. Aldosterone release may also be hypersensitive to slight reductions in plasma Na(+), which may be an adaptive mechanism in a species not known to drink seawater. Excreted aldosterone and urea were correlated suggesting aldosterone may regulate urea excretion during hypo-osmotic conditions in NES pups. Urea excretion appears to be a significant mechanism by which NES pups sustain electrolyte resorption during conditions that can negatively affect ionic homeostasis such as prolonged fasting.

NASA Center ARC↗
NASA NTRS2008

Part Marking and Identification Materials on MISSE

Many different spacecraft materials were flown as part of the Materials on International Space Station Experiment (MISSE), including several materials used in part marking and identification. The experiment contained Data Matrix symbols applied using laser bonding, vacuum arc vapor deposition, gas assisted laser etch, chemical etch, mechanical dot peening, laser shot peening, and laser induced surface improvement. The effects of ultraviolet radiation on nickel acetate seal versus hot water seal on sulfuric acid anodized aluminum are discussed. These samples were exposed on the International Space Station to the low Earth orbital environment of atomic oxygen, ultraviolet radiation, thermal cycling, and hard vacuum, though atomic oxygen exposure was very limited for some samples. Results from the one-year exposure on MISSE-3 and MISSE-4 are compared to those from MISSE-1 and MISSE-2, which were exposed for four years. Part marking and identification materials on the current MISSE -6 experiment are also discussed.

Finckenor, Miria M.↗
NASA NTRS2016

Micro Acoustic Resonant Chambers for Heating/Agitating/Mixing (MARCHAM)

A variety of applications require the mixing and/or heating of a slurry made from a powder/fluid mixture. One of these applications, Sub Critical Water Extraction (SCWE), is a process where water and an environmental powder sample (sieved soil, drill cuttings, etc.) are heated in a sealed chamber to temperatures greater than 200 degrees Celsius by allowing the pressure to increase, but without reaching the critical point of water. At these temperatures, the ability of water to extract organics from solid particulate increases drastically. This paper describes the modeling and experimentation on the use of an acoustic resonant chamber which is part of an amino acid detection instrument called Astrobionibbler [Noell et al. 2014, 2015]. In this instrument we use acoustics to excite a fluid- solid fines mixture in different frequency/Amplitude regimes to accomplish a variety of sample processing tasks. Driving the acoustic resonant chamber at lower frequencies can create circulation patterns in the fluid and mixes the liquid and fines, while driving the chamber at higher frequencies one can agitate the fluid and powder and create a suspension. If one then drives the chamber at high amplitude at resonance heating of the slurry occurs. In the mixing and agitating cell the particle levitation force depends on the relative densities and compressibility’s of the particulate and fluid and on the kinetic and potential energy densities associated with the velocity and pressure fields [Glynne-Jones, Boltryk and Hill 2012] in the cell. When heating, the piezoelectric transducer and chamber is driven at high power in resonance where the solid/fines region is modelled as acoustic transmission line with a large loss component. In this regime, heat is pumped into the solution/fines mixture and rapidly heats the sample. We have modeled the piezoelectric transducer/chamber/ sample using Mason’s equivalent circuit. In order to assess the validity of the model we have built and tested a variety of chambers. This paper describes the experimental results which are in general agreement with theory within the limitations of the modeling.

fluid particle interaction↗
NASA NTRS2013

Performance and Analysis of Perfluoropolyalkyl Ether Grease Used on Space Shuttle Actuators--A Case Study

Actuators used on the United States space shuttle fleet are lubricated with unspecified amounts of Braycote 601 (Castrol Braycote) grease consisting of a perfluoropolyalkyl ether (PFPAE) base oil thickened with a polytetrafluoroethylene (PTFE) filler. Each shuttle has four body flap actuators (BFAs) (two on each wing) on a common segmented shaft and four rudder speed brake (RSB) actuators. The actuators were designed to operate for 10 years and 100 flights without periodic relubrication. Visible inspection of two partially disassembled RSB actuators in continuous use for 19 years raised concerns over possible grease degradation due to discoloration of the grease on several places on the surfaces of the gears. Inspection revealed fretting, micropitting, wear and corrosion of the bearings and gears. A small amount of oil dripped from the disassembled actuators. Whereas new grease is beige in appearance, the discolored grease consisted of both grey and reddish colors. Grease samples taken from the actuators together with representative off-the-shelf new and unused grease samples were analyzed by gravimetry for oil content; by inductively coupled plasma spectroscopy (ICP) for metals content; Fourier transform infrared (FTIR) spectroscopy for base oil decomposition; and by size exclusion chromatography (SEC) for determination of the molecular weight distributions of the grease oil. The Braycote 601 grease was stable after 19 years of continuous use in the sealed RSB actuators and was fit for its intended purpose. There were no significant chemical differences between the used grease samples and new and unused samples. Base oil separation was not significant within the sealed actuators. No corrosive effect in the form of iron fluoride was detected. The grey color of grease samples was due to metallic iron. The red color was due to oxidation of the metallic wear particles from the gears and the bearings comprising the actuators.

Morales, Wilfredo↗
NASA NTRSDate not supplied

X-Ray Computed Tomography During Preliminary Examination of Apollo Drive Tube 73001

Introduction: Starting in 2019, the Apollo Next Generation Sample Analysis (ANGSA) Program has enabled consortium studies of specially curated Apollo samples that were previously unstudied (or under studied). This began with unsealed core tube 73002 [1,2] that is the upper part of a station 3 double drive tube. More recently the pro-gram extended to the study of a variety of frozen Apollo 17 samples [3], as well as the gas extraction [4] and dis-section [5] of 73001, the lower half of the station 3 double drive tube, that was sealed under vacuum on the Moon. In this abstract we will examine the role of X-ray Computed Tomography (XCT) during the preliminary examination process for sealed core 73001, including: (1) engineering scans to aid in understanding the gas extraction process, whole-core scanning prior to opening to inform extrusion and dissection work, and (3) individual particle scanning to characterize rock fragment lithologies for follow on studies. Methodology: Sample 73001 is a 33 cm long, 4 cm diameter regolith sample collected inside a drive tube (~1 mm aluminum walls). That drive tube was sealed inside a 0.5 mm thick stainless steel (SS) Core Sample Vacuum Container (CSVC). XCT scans for engineering purposes were done on the Nikon XTH 320 system at Johnson Space Center using the 225 kV multi-metal reflection source at 215 kV, 179 A, and a 38.49 m voxel size. Individual >4 mm particles separated from the core during processing (then triply sealed in Teflon bags) were also scanned at JSC using the 180 kV source at 90 kV, 33 A, and a 2.98 – 10.65 m voxel size. Whole-core scans were done at the University of Texas High-Resolution X-ray Computed Tomography Facility (UTCT) on the 225 kV reflection source on the North Star Imaging cabinet XCT system. These scans included: (1) a series of 9 overlapping super-resolution scans each covering a ~4 cm length of the tube at 190 kV, 180 µA, and a 12.9 µm voxel size and (2) a lower resolution continuous helical scan of the entire core at 190 kV, 180 µA, and a 51.8 µm voxel size. Progress and Results: Before piercing and extracting the gas from sample 73001, an XCT scan of the bottom portion of the CSVC was used to confirm the location of the Teflon cap on the inner drive tube, to ensure it was not accidentally pierced during gas extraction. Similarly, after piercing, the bottom and top portions of the CSVC were scanned in order to capture engineering knowledge about the results of the piercing process, as well as the metal knife edge vacuum seal (SS into In-Ag alloy). Both scans will provide constraints on future work of this type, particularly for samples collected during the Artemis mission. Another finding from these "engineering" scans was that the device in the drive tube that immobilizes the regolith (the keeper) was not seated in the tube properly. This meant that (1) the drive tube could not be removed from the CSVC for the trip to UTCT, and (2) the procedure for opening and extruding the drive tube had to be modified. Had either of these things not been known prior to opening the CSVC, it could have led to an inability to XCT scan the whole core at high resolution and/or potential disruption of the core stratigraphy during extrusion. At UTCT, the entire length of the core was scanned at high resolution (12.9 microns per voxel). This scan serves multiple purposes: (1) A lower resolution (and uncorrected) version of these scans stitched together was used to help inform the processors of potential pitfalls during extrusion and dissection; and (2) the full resolution corrected data will serve as the permanent in situ record of the stratigraphy of the sample and will enable future researchers to perform a variety of analyses. So far, 92 of the 121 >4 mm particles separated during dissection pass 1 of sample 73001 have been individually scanned. These scans clearly show the lithology of each particle while keeping the particles in pristine condition. Because of the dust adhering to particle exteriors it would otherwise be impossible to determine lithologies in a non-contaminating way. Thus far the types of lithologies seen in sample 73001 (e.g., regolith breccias, impact-melt breccias, agglutinates, and basalts) are similar to those previously identified in sample 73002 [2]. By the time of the meeting, all particles from all 3 dissection passes will have been scanned and statistics on the different lithologies in 73001 compiled. References: [1] Shearer et al. (2020) 51st LPSC, abstract 1181. [2] Zeigler et al. (2020) 51st LPSC, abstract 3023. [3] Kent et al. (2022) This Volume. [4] McDonald et al. (2022) European Lunar Symposium. [5] Gross et al (2022) This volume.

Moon↗
DOE OSTI2024

MR13A-3183: Microbial and Geochemical Characterization of Groundwater: Implications for Underground Hydrogen Storage Leakage

Underground hydrogen storage (UHS) in geological formations is a key element of the clean energy transition as it enables the decarbonization of the transportation and industrial sectors by decoupling hydrogen production and storage. UHS has many benefits, including low cost, much wider availability, large storage capacity, well-established infrastructure, and increased safety because of geological sealing capabilities. However, the impact of hydrogen (H2) biogeochemical interactions in the presence of subsurface microorganisms is largely neglected from UHS perspectives. These interactions might affect the effectiveness of storage and can even cause H2 to leak into the shallow aquifers. Leakage of H2 into groundwater can change the geochemistry and induce several microbial-driven processes. Microorganisms, such as sulfate-reducers, are naturally abundant in groundwater and consume H2 to produce hydrogen sulfide (H2S), which can contaminate the freshwater drinking groundwater and cause damage to infrastructure. Hydrogen leakage can also trigger microbial reactions responsible for metal mobility, which can impact the water quality. However, the kinetics of these reactions and the temporal impact of hydrogen leakage in groundwater are still unknown. Therefore, a time series hydrogen-groundwater interaction experiment was conducted, and the changes in fluid chemistry and headspace gas composition will be analyzed along with DNA sequencing results to understand the extent and kinetics of biogeochemical reactions that occur if hydrogen leaks into groundwater. In the experiments, Ultra High Purity (UHP) hydrogen gas will be injected into glass vials with groundwater samples, for a designated time period. For each glass-sealed vial, 16S rRNA gene sequencing, IC, ICP-MS, and GC-TCD will be performed. The experiments provide insights into plausible impacts of hydrogen leakage into shallow drinking water aquifers.

Clark, Allison [West Virginia University (WVU)]↗
NASA NTRSDate not supplied

Investigation of Lunar-Inspired Geopolymer Concrete Formulations Mixed and Cured in Microgravity on the International Space Station (ISS)

The research outlined in this presentation investigates the use of various lunar regolith simulants in geopolymer lunar concrete mixes mixed and cured on the International Space Station (ISS). The motivation for this work is to study the effects of gravity on the microstructure of alkali-activated materials cured with heat, and to develop materials for the construction of long-term infrastructure on the lunar surface with in-situ resource utilization (ISRU). ISRU for construction materials reduces the cost and mass of payloads related to lunar construction. The advantage of geopolymer concrete as opposed to traditional portland cement concrete is that water acts as a medium for the polymerization reaction and leaves the system throughout the process, reducing its demand. Twelve samples of lunar regolith simulant and a solution composed of sodium hydroxide and sodium silicate were sent to the ISS. The three simulants were OPRH2N, OPRL2N, and JSC-1AF, using only particles less than 53 µm in diameter to increase reactivity of the simulant. Simulant to solution ratios were determined by workability while mixing. The simulant and solution were sealed Burst Pouches® along with 2 other sealed bags to prevent material from leaking. Crew member F-14 conducted testing on the ISS by introducing the solution to the simulant in the Burst Pouch®, mixing the sample with a spatula, and then clamping the specimen in the fresh state to prevent flow inside the Burst Pouch®. These specimens were then put in a thermos heated to 80C via sealed drinking water bags to cure for 24 hours with a temperature logger. The cured specimens remained in microgravity for at least 28 days and were returned from the ISS in February 2025. The specimens were then brought to the NASA Marshall Space Flight Center (MSFC) to analyze. Material characterization consisted of conducting Micro-CT tests of entire samples in their sealed apparatus to a resolution of 25µm. 2D image slices were saved in each orthogonal direction of each specimen at a 0.03 mm step size from the 3D model to conduct analytical porosity calculations. Representative samples from each specimen were sampled to perform helium gas pycnometery and were then mounted in resin for SEM imaging, EDS, and nanoindentation. Porosity was analyzed analytically using micromechanics modelling with the assistance of the NASA Multiscale Analysis Tool (NASMAT), as well as the NASA Advanced Supercomputing (NAS) servers (V. Saseendran & N. Yamamoto, 2024). Density was measured using helium gas pycnometery and was then compared to the theoretical density for experimental porosity calculation. Due to the samples’ non-uniform shape being cured in a pouch, traditional compression and tensile strength testing could not be performed. Nanoindentation was conducted at Clarkson University to determine the microhardness and reduced modulus of elasticity. Results from flight samples can be compared to ground samples currently in DLR’s possession to determine the effect on microstructure from being mixed and cured in microgravity. This study gives further insight and understanding of geopolymer lunar concrete and its viability as a lunar construction material with ISRU.

Adam Johnson↗
NASA NTRSDate not supplied

New Hayabusa2 and OSIRIS REx Curation Facilities at Nasa Johnson Space Center

Asteroids are made up of rocky material that is left over from the formation of our solar system [1]. This material holds the key to unlocking information about the history of the planets and our sun. Hayabusa2 and OSIRIS-REx are two sample return missions that have collected rocky material from carbonaceous asteroids which are rich in water, carbon, and organic compounds [1]. Hayabusa2 is a spacecraft that collected samples from asteroid Ryugu launched by the Japan Aerospace Exploration Agency (JAXA). Samples were returned to Earth in December 2020 and 10 percent of the collected material is currently housed in a state-of-the-art laboratory at NASA Johnson Space Center (JSC) dedicated to Ryugu material [1]. OSIRIS-REx is a spacecraft launched by NASA that collected samples from asteroid Bennu. The samples are on their journey to Earth and will arrive in September 2023. They will be stored in a separate cleanroom dedicated to Bennu material. From these two missions, scientists will examine dust particles and rocky material to research clues on how the early solar system formed and how life began [2]. Because these samples are so precious and rare, it is important to keep them free from Earth contamination. In September of 2020, a massive construction project began to provide curation facilities to meet the needs of two incoming asteroid collections, Hayabusa2 and OSIRIS-REx. Despite numerous setbacks caused by the coronavirus pandemic, these facilities have been completed in the fall of 2021. Some of these setbacks included strict PPE requirements, keeping safe working distances as well as access to the facilities as NASA was operating under a Stage 3 condition in response to the pandemic. These facilities will provide curation laboratories to safely house the precious asteroid samples as well as facilities to manipulate samples, do sample preparation and process samples into and out of the labs for future studies by the scientific community. The lab suite consists of several different rooms including an initial anteroom (ISO 7), a staging area (ISO 7), two gowning areas (one for OSIRIS-REx and one for Hayabusa2; both ISO 6)), the Haybusa2 Curation Laboratory (ISO 5), the OSIRIS-REx Curation Laboratory (ISO 5), an ultramicrotomy laboratory (ISO 7) and a thin section laboratory (not a cleanroom). To maintain cleanliness levels necessary for these lab spaces quarterly to monthly Balazs organic and inorganic sampling has been conducted on a regular basis before, during and after the construction project to monitor the cleanliness levels in the new labs that will house the asteroid samples. These new facilities feature a Ruuvi (Grafana) monitoring system that measures temperature, humidity, and pressure of the lab suite. This is a small puck shaped sensor that sends signals to the Grafana cloud where the data can be plotted and set up on dashboards within the lab suite. These sensors are easy to set up and install and they run off a cell battery that is good for 3-5 years before needing replacement. This system can deliver text messages and emails to the appropriate personnel when values fall outside of set limits. In addition to the monitoring system, this new lab suite features viewing windows from several different locations and sliding motion censored doors. We have obtained some state-of-the-art equipment to outfit the lab spaces (desiccators, microscopes, ultramicrotome) and are in the process of outfitting the suite with additional items such as: nitrogen gloveboxes, additional desiccators, micromanipulators, etc. The Hayabusa2 samples provided to NASA by JAXA included 23 millimeter sized grains and 4 containers with finer material. OSIRIS-REx is expected to return as much as 400 grams of asteroid Bennu. Samples will be stored in a nitrogen glove box and separated into nitrogen sealed transfer containers. Small Bennu and Ryugu particles will be handled and prepared (e.g., ultra-thin sections for scanning electron microscopy (SEM) or transmission electron microscopy (TEM)) using an Axis Pro micromanipulator and Leica EM UC7 ultramicrotome. Analyzing samples at the atomic scale will provide greater insight to the origins of the solar system and life formation on Earth. All the curation preparation for these sample collections is essential to ongoing research and efforts to understand our solar system, both nowand for future generations.

Curation↗
NASA NTRS2017

Heating and Thermal Control of Brazing Technique to Break Contamination Path for Potential Mars Sample Return

The potential return of Mars sample material is of great interest to the planetary science community, as it would enable extensive analysis of samples with highly sensitive laboratory instruments. It is important to make sure such a mission concept would not bring any living microbes, which may possibly exist on Mars, back to Earth’s environment. In order to ensure the isolation of Mars microbes from Earth’s Atmosphere, a brazing sealing and sterilizing technique was proposed to break the Mars-to-Earth contamination path. Effectively, heating the brazing zone in high vacuum space and controlling the sample temperature for integrity are key challenges to the implementation of this technique. The break-the-chain procedures for container configurations, which are being considered, were simulated by multi-physics finite element models. Different heating methods including induction and resistive/radiation were evaluated. The temperature profiles of Martian samples in a proposed container structure were predicted. The results show that the sealing and sterilizing process can be controlled such that the samples temperature is maintained below the level that may cause damage, and that the brazing technique is a feasible approach to breaking the contamination path.

Bao, Xiaoqi↗
DOE OSTI2021

Salt Vessel-Sample Generator Interface

The goal of the salt sampling program at Argonne is to develop and deploy automated molten salt sampling approaches for interfacing relevant unit operations with salt analysis to improve the timeliness and accuracy of sampling-based accountancy measurements. One technology under development is a vacuum sampler loop module. In this system, molten salt is drawn from a process vessel through a heated sampling line and into a charge vessel. Next, one or more samples are split from the volume in the charge vessel and the remaining salt is returned to the process. The vacuum sampler loop module is being developed to interface with other sample processing and analysis modules to enable rapid at-line sample characterization. The main purpose of the vacuum sampling loop module is to enable the collection of samples that are more representative of the bulk salt by replacing traditional point samplers (i.e., dip probes) with a sampling approach that captures a larger cross section of salt. Additionally, the vacuum sampling approach eliminates the risk of dross contamination of samples and avoids the use of moving parts in the salt. Two methods of interfacing the vacuum sampling loop with a precision pneumatic sample generator were investigated in FY21. This report covers the testing of fluidic coupling between the two modules. Two iterations of the fluidically coupled modules were tested. The first iteration system coupled the two modules using a freeze valve to seal the vacuum sampler during filling and to control flow into the pneumatic sample generator. While this integrated system functioned as intended, some changes were implemented to make the system more robust and better suited to remote deployment. Specifically, the system was made to be more modular and active control of the vacuum filling operation was replaced with a passive control mechanism. For passive filling, the salt charge vessel was vented to a small gas tank that was at negative pressure, causing salt to be drawn into the vessel until the force of the fluid head was in equilibrium with the gas pressure. The passive control system performed well and will be used in future iterations. Another change in the second system was a newly configured pneumatic sample generator in which sample ejection occurred through a hole in the reservoir’s stainless-steel side wall instead of through a non-wetted sapphire orifice on the bottom. This alternate configuration may be better suited for near-process deployment because it enables on-line orifice maintenance and an orifice bypass drain back to the process. A third change in the second iteration system was the transition to a two-chamber charge vessel which split off a fraction of the sampled salt as a liquid aliquot. The goal was to create a buffer mechanism that would allow reproducible aliquoting of samples, independently of variability in the charge vessel fill height. While the two-chamber design was functional, the sample size reproducibility was below target values. To improve reproducibility and overcome many of the impediments to remote deployment of the vacuum sampling loop module, separate work was conducted to replace the two-chamber liquid aliquoting mechanism with aliquoting into single-use sample tubes. Solid salt transfer in the sample tubes will replace fluidic coupling for integrating the vacuum sampler with downstream modules. Because the proposed operations can all be executed with simple overhead actuation mechanisms or other existing hot-cell technology, there will be no need for large investments in novel hot cell sample handling technologies using this alternate approach. As such, near-term deployment of the vacuum sampling technology will be achievable. This new approach for automated coupling of sample tubes with down-stream modules is covered in a separate FY21 report, and a remotely operated version of the vacuum sampler loop module with the tube aliquoting feature is planned for FY22.

22 GENERAL STUDIES OF NUCLEAR REACTORS↗
NASA NTRSDate not supplied

Summary of Apollo Next Generation Sample Analysis (ANGSA) and Insights for Artemis Preliminary Examination Activities

Analyses of Apollo samples have provided fundamental insights into the origin and history of the Earth-Moon system and the solar system broadly. With great foresight, a subset of samples from Apollo were left unprocessed so that they could be studied by future generations with their modern technology. To prepare for the return of samples from the Moon by the Artemis Program, NASA initiated the Apollo Next Generation Sample Analysis Program (ANGSA) to analyze a subset of the previously unprocessed Apollo samples. The ANGSA consortium consisted of 9 original teams funded by NASA that combined into a single science team referred to as the ANGSA Science Team. ANGSA was designed to function like the sample analysis phase of a sample return mission with a goal to investigate the lower portion of a double drive tube previously sealed on the lunar surface (73001), the upper portion of that drive tube that had remained unopened (73002), and a variety of Apollo 17 samples that had remained stored at -20 ºC for approximately 50 years.

Francis M. McCubbin↗
DOE OSTI2024

Mini-Canister Radiolysis Testing of ASNF Materials and Surrogates

An experimental irradiation campaign to investigate radiolysis behavior of ASNF was conducted using in situ gas monitoring of small, sealed stainless-steel vessels (mini-canisters) containing aluminum samples with adherent (oxy)hydroxide films under helium backfill. The samples were irradiated with gamma radiation from a Co-60 irradiator. The samples tested included aluminum plate assemblies with lab-grown (oxy)hydroxides as surrogates for fuel as well as an end cropping from an actual ASNF assembly retrieved from long-term wet storage. These experiments enabled investigation of the impacts of various fuel drying approaches on the radiolytic generation rate and measurement of the H 2 yield associated with a reactor exposed sample with reactor-formed (oxy)hydroxide. The resulting data can be incorporated into model development for ASNF in dry storage. This report presents the cumulative results from four surrogate assemblies tested after application of different preparation (drying) conditions as well as the ASNF cropping; some post-irradiation testing was included. The mini-canister results are compared to data from related experimental campaigns that also tested the impact of drying conditions using samples irradiated in glass ampoules and discusses implications of the combined data

12 MANAGEMENT OF RADIOACTIVE AND NON-RADIOACTIVE W↗