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Applicability of Micro X-Ray Fluorescence Spectroscopy to Astromaterials Curation and Research

Introduction: The Astromaterials Acquisition and Curation Office at NASA’s Johnson Space Center (JSC) curates NASA’s astromaterial sample collections which includes: Apollo samples, Luna samples, Ant-arctic meteorites, cosmic dust particles, microparticle impacts into space-flown materials, Genesis solar wind atoms, Stardust comet Wild-2 particles, Stardust inter-stellar particles, Hayabusa asteroid Itokawa particles, Hayabusa 2 asteroid Ryugu particles, and future OSIRIS-Rex asteroid Bennu particles (landing in Sep-tember, 2023) [1–3]. To enhance JSC’s advanced cu-ration capabilities, we have recently installed a high-performance micro-X-ray fluorescence (µXRF) spec-trometer to assist in sample characterization through rapid, non-destructive, in-situ elemental analyses that do not require the sample preparation protocols (i.e., polishing and carbon-coating) commonly needed for electron beam analyses. With this new instrument, we are capable of detecting all elements down to carbon in a variable-pressure or He-purged chamber for anal-ysis of a wide range of sample types. Here we describe the instrumental set-up, capabilities, and applicability of µXRF analysis to astromaterials curation and re-search. Instrumentation and Methodology: The X-ray fluorescence and computed tomography lab (X-FaCT) lab at JSC is now equipped with a Bruker M4 Tornado Plus µXRF (Fig. 1). This system is an energy-dispersive x-ray spectrometer equipped with two 60 mm2 silicon drift detectors (SDD) that are able to be used simulta-neously for output count rates ~500,000 cps. New light element windows allow detecting and analyzing the entire elemental range from carbon to americium. Two x-ray tubes (micro-focus Rh with polycapillary lenses and W with collimators of 0.5, 1.0, 2.0, and 4.5 mm) with max excitation parameters of 50 kV, 30 W and 50 kV, 40 W, respectively, allow for more flexibility of the analysis of high energy lines. The motorized X-Y-Z stage has a mapping range of 190 x 160 mm and can support samples up to 7 kg (~15.5 lbs) and a height of 120 mm [4]. Analytical modes include elemental analysis (down to ~20 µm spot size) via point, line, or area of bulk materials (rock surfaces, thin sections, thick sections, etc.) as well as coating analysis (determination of thickness and composition) of samples. This system has a variable vacuum chamber (1 mbar to 1 atm) that is also equipped with a He-purge system which accommodates vacuum sensitive samples while still allowing detection of light elements at atmospheric pressure. Utility and Applicability of µXRF in Astro-materials research and exploration science (ARES): Elemental analysis using µXRF is commonly em-ployed for both terrestrial and planetary geological science disciplines [5]. It is especially useful for analy-sis of astromaterials given the limited sample prepara-tion required, which is not feasible for certain materi-als. Here we show select applications of µXRF anal-yses of astromaterials that can, have, and will be done at JSC’s X-FaCT lab. Point analysis: In-situ spot analyses (~20 µm spot size) on a cut slab of Martian meteorite NWA 10922 allowed for the discovery, qualitative elemental analy-sis and determination of different feldspar minerals [6]. These point analyses served as an effective prelim-inary step for subsequent quantitative analyses. Ana-lytical standards can be employed for more accurate quantification of µXRF spot analyses. Area analysis: This analytical mode measures all detectable elements (from C to Am) at each pixel (>5 µm pixel size) in a user-defined area. The results are shown as elemental maps which can be extracted as 16-bit TIFF’s for further data processing. In Fig. 2. we show elemental distribution maps of the high-Ti basalt 73001,531 that have been processed using ImageJ software. From these maps you can accurately and quickly (this map took ~50 mins.) identify mineral components, such as pyroxene, plagioclase, oxides, and phosphates, compositional zoning, and mineral textures. Detection of high-Z phases: µXRF techniques are es-pecially effective at analyzing trace minerals with high-atomic-number (high-Z) elements because the high-energy characteristic X-rays used (relative to SEM EDS) allow for mapping of K lines in elements up to La (typically SEM maps use L X-ray lines for elements >Zn, and these can often have interferences). Thus, µXRF is especially suited for identifying minerals like zircon, baddeleyite, REE-rich phosphates, Fe-rich met-als, oxides, sulfides, and phosphides [4]. In Fig. 3 we show elemental distribution maps for 73001,530 where we are able to correlate the original video image with, Zr, Si, Y and Hf elemental maps together identi-fying the location of a zircon. In this location you would expect lower Si compared to surrounding mate-rial, as well as higher Zr, Y, and Hf content compared to surrounding material, all of which is confirmed by our XRF ele-mental distribution maps (Figure 2.) Conclusions: The new M4 Tornado Plus µXRF within the Astromaterials Acquisition and Curation office at NASA JSC allows for rapid and non-destructive elemental analysis of astromaterials with limited or no sample preparation. µXRF analyses pro-vide crucial compositional knowledge for the prelimi-nary examination and curation of astromaterials. This instrument enhances the advanced curation capabili-ties in the X-FaCT laboratory at JSC by allowing pro-ductive, cohesive, and non-destructive multi-modal x-ray analyses on astromaterial samples, which is neces-sary for the comprehensive curation and study of our current and future astromaterial collections. Addition-ally, µXRF can provide complimentary information to researchers for studies on astromaterials. References: [1] Allen, C. et al., (2011). Chemie De Erde Geochemistry, 71, 1-20. [2] McCubbin, F. M. et al., (2016) 47th LPSC, abstract #2668 [3] Zeigler, R. A. et al., (2017) 48th LPSC, abstract #2772 [4] Bruker User Manual [5] Young et al., (2016) Appl. Geochemistry, 72, 77-87 [6] Mor-ris, R. V. et al., (2023) 54th LPSC.

E W O'Neal↗

An Interdisciplinary Method for the Visualization of Novel High-Resolution Precision Photography and Micro-XCT Data Sets of NASA's Apollo Lunar Samples and Antarctic Meteorite Samples to Create Combined Research-Grade 3D Virtual Samples for the Benefit of Astromaterials Collections Conservation, Curation, Scientific Research and Education

New technologies make possible the advancement of documentation and visualization practices that can enhance conservation and curation protocols for NASA's Astromaterials Collections. With increasing demands for accessibility to updated comprehensive data, and with new sample return missions on the horizon, it is of primary importance to develop new standards for contemporary documentation and visualization methodologies. Our interdisciplinary team has expertise in the fields of heritage conservation practices, professional photography, photogrammetry, imaging science, application engineering, data curation, geoscience, and astromaterials curation. Our objective is to create virtual 3D reconstructions of Apollo Lunar and Antarctic Meteorite samples that are a fusion of two state-of-the-art data sets: the interior view of the sample by collecting Micro-XCT data and the exterior view of the sample by collecting high-resolution precision photography data. These new data provide researchers an information-rich visualization of both compositional and textural information prior to any physical sub-sampling. Since January 2013 we have developed a process that resulted in the successful creation of the first image-based 3D reconstruction of an Apollo Lunar Sample correlated to a 3D reconstruction of the same sample's Micro- XCT data, illustrating that this technique is both operationally possible and functionally beneficial. In May of 2016 we began a 3-year research period during which we aim to produce Virtual Astromaterials Samples for 60 high-priority Apollo Lunar and Antarctic Meteorite samples and serve them on NASA's Astromaterials Acquisition and Curation website. Our research demonstrates that research-grade Virtual Astromaterials Samples are beneficial in preserving for posterity a precise 3D reconstruction of the sample prior to sub-sampling, which greatly improves documentation practices, provides unique and novel visualization of the sample's interior and exterior features, offers scientists a preliminary research tool for targeted sub-sample requests, and additionally is a visually engaging interactive tool for bringing astromaterials science to the public.

Blumenfeld, E. H.↗

Astromaterial Curation and Research at NASA

Astromaterial sample return missions from other planetary bodies (e.g., the Moon, asteroids, the Sun) and astromaterial sample collection missions here on Earth (e.g., Antarctic Meteorites, Cosmic Dust) have been a vital part of NASA’s science vision since nearly its inception. Beginning with the Apollo missions to the Moon and extending to the recent successful sample collection by the OSIRIS-REx asteroid sample return mission, these astromaterials collections have been an invaluable resource to scientists and educators around the world. Sample studies continue to provide fundamental insight into how our solar system and its constituent bodies formed and evolved over the past 4.5 billion years. As evidence of their broad impact, there are over 19,141 samples on loan to 433 Principal Investigators in 24 countries [1]. As we plan for exploration missions through 2050, sample return missions will continue to play a vital role in NASA’s science vision. Returned samples truly are the gift that keeps on giving. Having the samples accessible on Earth allows new generations of scientists and new generations of instrumentation to pursue ever evolving scientific questions. For example, the Apollo samples were collected ~50 years ago, yet our views of how the Earth-Moon system formed, the role of volatiles in the early inner solar system, and even the positions of the gas giants in the outer solar system have changed dramatically as a result of Apollo sample analyses conducted very recently. Vital to the long-term viability of any sample return mission is the careful curation of the samples. Curatorial efforts need to begin early in the project lifecycle, not with the return of the samples, but at mission conception. The Astromaterials Acquisition and Curation Office at NASA Johnson Space Center is responsible for curating all of NASA’s current and future extraterrestrial samples. Looking at possible sample return missions over the next 35+ years [2], many samples would require curation efforts a step beyond current capabilities, e.g., cold or cryogenic curation, organically and biologically clean curation, curation of gases and ices, and curation of samples with extreme pressure, temperature, or redox requirements. During the lecture, we discuss the current curatorial efforts in JSC curation, as well as discoveries from the astromaterial research. [1] Zeigler, R. A. et al. (2017) Planetary Science Vision 2050 Workshop. [2] McCubbin F. M. et al. (2017) Planetary Science Vision 2050 Workshop.

astromaterial↗

Real Time Nitrogen Monitoring and Quality Control System for NASA Astromaterials Collection

The Nitrogen system is a vital utility supporting the curation office within NASA's Astromaterials Re-search and Exploration Science (ARES) Division at the Johnson Space center (JSC). Since the Apollo samples were returned in 1969. It has played an essential role in preserving NASA’s astromaterial collections (now nine collections) by maintaining contamination-free, controlled environments required for long term curation and advanced scientific research. To meet the stringent purity requirements for contamination control, high purity modified Grade C Liquid Nitrogen (LN2) is delivered weekly by an industrial gas vendor to a 15,000-gallon tank located outside at NASA JSC near the ARES facility. This nitrogen is vital for creating an inert atmosphere to store the collection in, ensuring they are continuously shielded from contaminants and alterations through a constant N2purge. For most of the past 65 years deliveries of LN2 have required a CoA (Certificate of Analysis) prior to delivery. If those were not available, then LN2 deliver were sent to third-party laboratories for verification, creating an operational bottleneck and quality gap. To address this challenge and maintain rigorous quality control, NASA JSC Infrastructure and Astromaterials Acquisition & Curation Office initiated the development of an on-site Analytical Gas Sampling (AGS) Laboratory. Designed to streamline quality verification if a CoA unavailable, the AGS lab was constructed by a subcontractor in Newton, NJ. After a successful factory acceptance test conducted by the NASA ARES Infrastructure team, the lab was trans-ported to NASA JSC, where it was anchored and integrated into the site’s nitrogen pressure system using stainless steel, oxygen-cleaned tubing. The ARES nitrogen system was modified to provide parallel flows to the AGS lab for quality control and to the astromaterials collection labs for maintaining an inert environment. The AGS lab features two operational modes: (1)Primary: Gaseous Nitrogen (GN2) Quality Monitoring –The AGS system continuously samples the site’s GN2 supply every 15 minutes to ensure compliance with required purity levels. (2) Secondary: LN2 Quality Verification when a comprehensive CoA is not available, a cryogenic vaporizer converts LN2 to GN2, which is then analyzed for impurities: H₂, Ar, O₂, CO, CO₂, H₂O, and total hydrocarbons (THC). By significantly enhancing on-site analytical capabilities, the AGS lab eliminates reliance on external testing, ensures uninterrupted quality monitoring of the nitrogen pressure system, and reinforces NASA’s commitment to preserving pristine astromaterials under the highest standards of curation and research integrity.

glove box↗

Astromaterials Curation Online Resources for Principal Investigators

The Astromaterials Acquisition and Curation office at NASA Johnson Space Center curates all of NASA's extraterrestrial samples, the most extensive set of astromaterials samples available to the research community worldwide. The office allocates ~1500 individual samples to researchers and students each year and has served the planetary research community for 45+ years. The Astromaterials Curation office provides access to its sample data repository and digital resources to support the research needs of sample investigators and to aid in the selection and request of samples for scientific study. These resources can be found on the Astromaterials Acquisition and Curation website at https://curator.jsc.nasa.gov. To better serve our users, we have engaged in several activities to enhance the data available for astromaterials samples, to improve the accessibility and performance of the website, and to address user feedback. We havealso put plans in place for continuing improvements to our existing data products.

Todd, Nancy S.↗

Advanced Curation of Astromaterials for Planetary Science Over the Next Decade

Advanced curation is a cross-disciplinary field of research and development aiming to improve curation and sample acquisition practices in existing astromaterials collections and to enable future sample return activities.The primary result of advanced curation is to both reduce and quantify contamination to astromaterials and preserve the scientific integrity of all samples from mission inception to scientific analysis. Over the next decade, NASA should support advanced curation research and monitoring efforts as they pertain to improving our current collections and preparing for samples from current and future astromaterials acquisition activities.We highlight here five advanced curation activities of critical importance for the success of sample science supported by NASA over the coming decade, including: 1) supporting efforts to build contamination knowledge collections as part of sample return missions, which requires curation involvement from the earliest stages of sample return mission planning;2) supporting Earth-based astromaterials collection campaigns of meteorites and cosmic dust as they represent relatively inexpensive sample acquisition activities that continue to grow NASA’s astromaterials collections and enable new discoveries;3) preparing to curate and process samples under “cold” conditions to enable return of samples from volatile-rich Solar System targets like permanently shadowed regions on the lunar surface orcomets;4) determining how best to combine clean room technology and biosafety technology into one infrastructure to support curation of samples from bodies designated as Category V:Restricted Earth Return; and 5) supporting real-time monitoring and testing of curation labs to verify that sample processing environments remain clean from the standpoint of inorganic, organic, and biological contamination

Francis M. McCubbin↗

NASA's Astromaterials Database: Enabling Research Through Increased Access to Sample Data, Metadata and Imagery

The Astromaterials Acquisition & Curation Office at NASA's Johnson Space Center (JSC) is the designated facility for curating all of NASA's extraterrestrial samples. Today, the suite of collections includes the lunar samples from the Apollo missions, cosmic dust particles falling into the Earth's atmosphere, meteorites collected in Antarctica, comet and interstellar dust particles from the Stardust mission, asteroid particles from Japan's Hayabusa mission, solar wind atoms collected during the Genesis mission, and space‐exposed hardware from several missions. To support planetary science research on these samples, JSC's Astromaterials Curation Office hosts NASA's Astromaterials Curation digital repository and data access portal [http://curator.jsc.nasa.gov/], providing descriptions of the missions and collections, and critical information about each individual sample. Our office is designing and implementing several informatics initiatives to better serve the planetary research community. First, we are re‐hosting the basic database framework by consolidating legacy databases for individual collections and providing a uniform access point for information (descriptions, imagery, classification) on all of our samples. Second, we continue to upgrade and host digital compendia that summarize and highlight published findings on the samples (e.g., lunar samples, meteorites from Mars). We host high resolution imagery of samples as it becomes available, including newly scanned images of historical prints from the Apollo missions. Finally we are creating plans to collect and provide new data, including 3D imagery, point cloud data, micro CT data, and external links to other data sets on selected samples. Together, these individual efforts will provide unprecedented digital access to NASA's Astromaterials, enabling preservation of the samples through more specific and targeted requests, and supporting new planetary science research and collaborations on the samples.

Evans, Cindy↗

Improving the Discoverability and Availability of Sample Data and Imagery in NASA's Astromaterials Curation Digital Repository Using a New Common Architecture for Sample Databases

The Astromaterials Acquisition and Curation Office at NASA's Johnson Space Center (JSC) is the designated facility for curating all of NASA's extraterrestrial samples. The suite of collections includes the lunar samples from the Apollo missions, cosmic dust particles falling into the Earth's atmosphere, meteorites collected in Antarctica, comet and interstellar dust particles from the Stardust mission, asteroid particles from the Japanese Hayabusa mission, and solar wind atoms collected during the Genesis mission. To support planetary science research on these samples, NASA's Astromaterials Curation Office hosts the Astromaterials Curation Digital Repository, which provides descriptions of the missions and collections, and critical information about each individual sample. Our office is implementing several informatics initiatives with the goal of better serving the planetary research community. One of these initiatives aims to increase the availability and discoverability of sample data and images through the use of a newly designed common architecture for Astromaterials Curation databases.

Todd, N. S.↗

Organic Contamination Baseline Study in NASA Johnson Space Center Astromaterials Curation Laboratories

Future robotic and human spaceflight missions to the Moon, Mars, asteroids, and comets will require curating astromaterial samples with minimal inorganic and organic contamination to preserve the scientific integrity of each sample. 21st century sample return missions will focus on strict protocols for reducing organic contamination that have not been seen since the Apollo manned lunar landing program. To properly curate these materials, the Astromaterials Acquisition and Curation Office under the Astromaterial Research and Exploration Science Directorate at NASA Johnson Space Center houses and protects all extraterrestrial materials brought back to Earth that are controlled by the United States government. During fiscal year 2012, we conducted a year-long project to compile historical documentation and laboratory tests involving organic investigations at these facilities. In addition, we developed a plan to determine the current state of organic cleanliness in curation laboratories housing astromaterials. This was accomplished by focusing on current procedures and protocols for cleaning, sample handling, and storage. While the intention of this report is to give a comprehensive overview of the current state of organic cleanliness in JSC curation laboratories, it also provides a baseline for determining whether our cleaning procedures and sample handling protocols need to be adapted and/or augmented to meet the new requirements for future human spaceflight and robotic sample return missions.

Calaway, Michael J.↗

The Astromaterials X-Ray Computed Tomography Laboratory at Johnson Space Center

The Astromaterials Acquisition and Curation Office at NASA's Johnson Space Center (hereafter JSC curation) is the past, present, and future home of all of NASA's astromaterials sample collections. JSC curation currently houses all or part of nine different sample collections: (1) Apollo samples (1969), (2) Lunar samples (1972), (3) Antarctic meteorites (1976), (4) Cosmic Dust particles (1981), (5) Microparticle Impact Collection (1985), (6) Genesis solar wind atoms (2004); (7) Stardust comet Wild-2 particles (2006), (8) Stardust interstellar particles (2006), and (9) Hayabusa asteroid Itokawa particles (2010). Each sample collection is housed in a dedicated clean room, or suite of clean rooms, that is tailored to the requirements of that sample collection. Our primary goals are to maintain the long-term integrity of the samples and ensure that the samples are distributed for scientific study in a fair, timely, and responsible manner, thus maximizing the return on each sample. Part of the curation process is planning for the future, and we also perform fundamental research in advanced curation initiatives. Advanced Curation is tasked with developing procedures, technology, and data sets necessary for curating new types of sample collections, or getting new results from existing sample collections [2]. We are (and have been) planning for future curation, including cold curation, extended curation of ices and volatiles, curation of samples with special chemical considerations such as perchlorate-rich samples, and curation of organically- and biologically-sensitive samples. As part of these advanced curation efforts we are augmenting our analytical facilities as well. A micro X-Ray computed tomography (micro-XCT) laboratory dedicated to the study of astromaterials will be coming online this spring within the JSC Curation office, and we plan to add additional facilities that will enable nondestructive (or minimally-destructive) analyses of astromaterials in the near future (micro-XRF, confocal imaging Raman Spectroscopy). These facilities will be available to: (1) develop sample handling and storage techniques for future sample return missions; (2) be utilized by PET for future sample return missions; (3) be used for retroactive PET (Positron Emission Tomography)-style analyses of our existing collections; and (4) for periodic assessments of the existing sample collections. Here we describe the new micro-XCT system, as well as some of the ongoing or anticipated applications of the instrument.

Zeigler, R. A.↗

The Astromaterials X-Ray Computed Tomography Laboratory at Johnson Space Center

The Astromaterials Acquisition and Curation Office at NASA's Johnson Space Center (hereafter JSC curation) is the past, present, and future home of all of NASA's astromaterials sample collections. JSC curation currently houses all or part of nine different sample collections: (1) Apollo samples (1969), (2) Lunar samples (1972), (3) Antarctic meteorites (1976), (4) Cosmic Dust particles (1981), (5) Microparticle Impact Collection (1985), (6) Genesis solar wind atoms (2004); (7) Stardust comet Wild-2 particles (2006), (8) Stardust interstellar particles (2006), and (9) Hayabusa asteroid Itokawa particles (2010). Each sample collection is housed in a dedicated clean room, or suite of clean rooms, that is tailored to the requirements of that sample collection. Our primary goals are to maintain the long-term integrity of the samples and ensure that the samples are distributed for scientific study in a fair, timely, and responsible manner, thus maximizing the return on each sample. Part of the curation process is planning for the future, and we also perform fundamental research in advanced curation initiatives. Advanced Curation is tasked with developing procedures, technology, and data sets necessary for curating new types of sample collections, or getting new results from existing sample collections [2]. We are (and have been) planning for future curation, including cold curation, extended curation of ices and volatiles, curation of samples with special chemical considerations such as perchlorate-rich samples, and curation of organically- and biologically-sensitive samples. As part of these advanced curation efforts we are augmenting our analytical facilities as well. A micro X-Ray computed tomography (micro-XCT) laboratory dedicated to the study of astromaterials will be coming online this spring within the JSC Curation office, and we plan to add additional facilities that will enable nondestructive (or minimally-destructive) analyses of astromaterials in the near future (micro-XRF, confocal imaging Raman Spectroscopy). These facilities will be available to: (1) develop sample handling and storage techniques for future sample return missions; (2) be utilized by PET for future sample return missions; (3) be used for retroactive PET (Positron Emission Tomography)-style analyses of our existing collections; and (4) for periodic assessments of the existing sample collections. Here we describe the new micro-XCT system, as well as some of the ongoing or anticipated applications of the instrument.

Zeigler, R. A.↗

Investigating Astromaterials Curation Applications for Dexterous Robotic Arms

The Astromaterials Acquisition and Curation office at NASA Johnson Space Center is currently investigating tools and methods that will enable the curation of future astromaterials collections. Size and temperature constraints for astromaterials to be collected by current and future proposed missions will require the development of new robotic sample and tool handling capabilities. NASA Curation has investigated the application of robot arms in the past, and robotic 3-axis micromanipulators are currently in use for small particle curation in the Stardust and Cosmic Dust laboratories. While 3-axis micromanipulators have been extremely successful for activities involving the transfer of isolated particles in the 5-20 micron range (e.g. from microscope slide to epoxy bullet tip, beryllium SEM disk), their limited ranges of motion and lack of yaw, pitch, and roll degrees of freedom restrict their utility in other applications. For instance, curators removing particles from cosmic dust collectors by hand often employ scooping and rotating motions to successfully free trapped particles from the silicone oil coatings. Similar scooping and rotating motions are also employed when isolating a specific particle of interest from an aliquot of crushed meteorite. While cosmic dust curators have been remarkably successful with these kinds of particle manipulations using handheld tools, operator fatigue limits the number of particles that can be removed during a given extraction session. The challenges for curation of small particles will be exacerbated by mission requirements that samples be processed in N2 sample cabinets (i.e. gloveboxes). We have been investigating the use of compact robot arms to facilitate sample handling within gloveboxes. Six-axis robot arms potentially have applications beyond small particle manipulation. For instance, future sample return missions may involve biologically sensitive astromaterials that can be easily compromised by physical interaction with a curator; other potential future returned samples may require cryogenic curation. Robot arms may be combined with high resolution cameras within a sample cabinet and controlled remotely by curator. Sophisticated robot arm and hand combination systems can be programmed to mimic the movements of a curator wearing a data glove; successful implementation of such a system may ultimately allow a curator to virtually operate in a nitrogen, cryogenic, or biologically sensitive environment with dexterity comparable to that of a curator physically handling samples in a glove box.

Snead, C. J.↗

Advances in Small Particle Handling of Astromaterials in Preparation for OSIRIS-REx and Hayabusa2: Initial Developments

The Astromaterials Acquisition and Curation office at NASA Johnson Space Center has established an Advanced Curation program that is tasked with developing procedures, technologies, and data sets necessary for the curation of future astromaterials collections as envisioned by NASA exploration goals. One particular objective of the Advanced Curation program is the development of new methods for the collection, storage, handling and characterization of small (less than 100 micrometer) particles. Astromaterials Curation currently maintains four small particle collections: Cosmic Dust that has been collected in Earth's stratosphere by ER2 and WB-57 aircraft, Comet 81P/Wild 2 dust returned by NASA's Stardust spacecraft, interstellar dust that was returned by Stardust, and asteroid Itokawa particles that were returned by the JAXA's Hayabusa spacecraft. NASA Curation is currently preparing for the anticipated return of two new astromaterials collections - asteroid Ryugu regolith to be collected by Hayabusa2 spacecraft in 2021 (samples will be provided by JAXA as part of an international agreement), and asteroid Bennu regolith to be collected by the OSIRIS-REx spacecraft and returned in 2023. A substantial portion of these returned samples are expected to consist of small particle components, and mission requirements necessitate the development of new processing tools and methods in order to maximize the scientific yield from these valuable acquisitions. Here we describe initial progress towards the development of applicable sample handling methods for the successful curation of future small particle collections.

Snead, C. J.↗

Applicability and Utility of the Astromaterials X-Ray Computed Tomography Laboratory at Johnson Space Center

The Astromaterials Acquisition and Curation Office at NASA’s Johnson Space Center is responsible for curating all of NASA’s astromaterial sample collections (i.e. Apollo samples, Luna Samples, Antarctic Meteorites, Cosmic Dust Particles, Microparticle Impact Collection, Genesis solar wind atoms, Stardust comet Wild-2 particles, Stardust interstellar particles, and Hayabusa asteroid Itokawa particles) [1-3]. To assist in sample curation and distribution, JSC Curation has recently installed an X-ray computed tomography (XCT) scanner to visualize and characterize samples in 3D. [3] describes the instrumental set-up and the utility of XCT to astromaterials curation. Here we describe some of the current and future projects and illustrate the usefulness of XCT in studying astromaterials.

Eckley, S. A.↗

Development of Machine Learning Algorithms to Segment and Study Images of Astromaterial Samples

Introduction: Micrometer-scale chemical analyses of chondritic meteorites and mission-returned asteroid samples can reveal details of the physical and chemical processes operating in the early solar system, including processes that gave rise to planets, moons, and minor bodies. These primitive astromaterials are comprised of chondrules, calcium- and aluminum-rich inclusions (CAI), and many other silicates, oxides, metals, sulfides, and fine-grained materials. The chemical and mineralogical complexity of these samples, vast populations of different components, and heterogeneity across mm to km scales, all limit our understanding of the origin and evolution of these materials. Here, we describe recent efforts to use machine learning techniques to automate the segmentation of chemical maps of chondritic meteorites, designed to aid studies of asteroid samples returned by spacecraft. By automating the task of segmentation it will become possible to rapidly analyze and interpret the sizes, shapes, mineralogy, chemistry, and other properties of every chondrule, calcium- and aluminum-rich inclusion (CAI) and other clast within and between asteroid samples. Sample return missions significantly accelerate and heighten the need to develop such new data analysis techniques, and associated data repositories. Techniques: Neural networks require abundant training data, i.e. images which have been segmented by a human user. We have manually segmented data available from previous petrologic and chemical work at NASA Johnson Space Center and the American Museum of Natural History [1-4]. These data were derived from energy- and wavelength-dispersive X-ray spectroscopy (EDS, WDS) mapping of samples from many chondrite groups. The Deeplabv3+ [5] neural network architecture was trained on human-labeled masks and used to create machine-labeled masks. Several different algorithms were investigated, with inputs ranging from common RGB image formats through to hyperspectral datasets, with raw data comprising greyscale maps of Mg, Ca, and Al, with or without Si, Fe, Ti for both EDS and WDS data, and extending to other elements in EDS only. Each greyscale image was paired with a binary mask for each labelled particle type. Results: The trained algorithms can segment (Fig 1), classify, and measure the dimensions of thousands of particles in chemical maps of a standard 1-inch round petrographic section in seconds to minutes, rather than many hours needed by a human. Accuracy of the algorithms varied from chondrite to chondrite and across particle types. Further results and details of the algorithms will be presented at the workshop. Future directions: Machine learning has the potential to revolutionize our understanding of complex particle populations contained within primitive astromaterial, with segmentation being a critical first step. Example applications include better understanding of particle transport, nebular reservoirs, parent body accretion, and a deeper understanding of the relationships between particle populations and bulk rock elemental and isotopic compositions. In addition to benefits that machine learning can bring to individual researchers, building a community data repository of thousands to millions of particles across hundreds of samples will open up many other possibilities. For example, with a large enough dataset it will be possible to search for exceptionally closely matching particles across disparate samples. Such a capability would enable a single CAI from OSIRISREx or Hayabusa/II samples to be matched to chondritic CAIs that exhibit near-identical size, texture, and mineralogy, down to the level of similar core phenocrysts, zonation, and rim sequences. Such comparative analyses will help to disentangle precursor chemistry, chronology, gas/dust reservoirs during heating, and accretion. Such an endeavor would be impossible without machine learning and a large community data repository of astromaterial chemical/mineralogic maps.

Machine Learning↗

Ultrapure Water System at JSC for High Purity Cleaning of Flight Hardware, Astromaterial Handling Tools and Solar Wind Samples

Use of Ultrapure Water (UPW) for cleaning of astromaterial sample handling tools and containers was driven by the discontinuation of Freon 113 as a cleaning solvent, due to environmental concerns. Freon 113, recycled using distillation, was very effective at removing organic residues from sample handling hardware. The initial switch to high purity water for astromaterial tool cleaning was modeled after efforts at White Sands Test Facility (WSTF) and current semiconductor UPW production practices in the early 1990s. JSC curation’s first system was comprised of ion exchange polishing cylinders, 55 gallon PVDF-lined storage tank, a few tens of feet of PVDF piping, UV and particle filtration, and this system supported cleaning for lunar, meteorite and Cosmic Dust collectors lab operations. By 2000 a major expansion and upgrade was providing UPW of quality E-1 (ASTM D5127-90) or better at 10 gpm for cleaning of the Genesis solar wind payload for flight, in addition to sample handling tools for other astromaterials. This expansion included a 1000 gallon storage tank and several hundred feet of PVDF piping located in B. 31 and 31N. An extra reverse osmosis process unit was added to incoming water in 2005. Subsequently several major components were replaced, and in anticipation of adding new labs, an enlarged UPW system was designed in 2018 and completed in 2019. This system produces grade E1.1 UPW at 15 gpm in a continuous 1100 ft. loop with 5000 gal. storage tank, supplying 8 laboratories.

Ultrapure water↗

Organic Contamination Baseline Study on NASA JSC Astromaterial Curation Gloveboxes

Future planned sample return missions to carbon-rich asteroids and Mars in the next two decades will require strict handling and curation protocols as well as new procedures for reducing organic contamination. After the Apollo program, astromaterial collections have mainly been concerned with inorganic contamination [1-4]. However, future isolation containment systems for astromaterials, possibly nitrogen enriched gloveboxes, must be able to reduce organic and inorganic cross-contamination. In 2012, a baseline study was orchestrated to establish the current state of organic cleanliness in gloveboxes used by NASA JSC astromaterials curation labs that could be used as a benchmark for future mission designs.

Calaway, Michael J.↗

Reducing Organic Contamination in NASA JSC Astromaterial Curation Facility

Future robotic and human spaceflight missions to the Moon, Mars, asteroids and comets will require handling and storing astromaterial samples with minimal inorganic and organic contamination to preserve the scientific integrity of each sample. Much was learned from the rigorous attempts to minimize and monitor organic contamination during Apollo, but it was not adequate for current analytical requirements; thus [1]. OSIRIS-REx, Hayabusa-2, and future Mars sample return will require better protocols for reducing organic contamination. Future isolation con-tainment systems for astromaterials, possibly nitrogen enriched gloveboxes, must be able to reduce organic and inorganic cross-contamination. In 2012, a baseline study established the current state of organic cleanliness in gloveboxes used by NASA JSC astromaterials curation labs that could be used as a benchmark for future mission designs [2, 3]. After standard ultra-pure water (UPW) cleaning, the majority of organic contaminates found were hydrocarbons, plasticizers, silicones, and solvents. Hydro-carbons loads (> C7) ranged from 1.9 to 11.8 ng/cm2 for TD-GC-MS wafer exposure analyses and 5.0 to 19.5 ng/L for TD-GC-MS adsorbent tube exposure. Plasticizers included < 0.6 ng/cm2 of DBP, DEP, TXIB, and DIBP. Silicones included < 0.5 ng/cm2 of cyclo(Me2SiO)x (x = 6, 8, 9, 10) and siloxane. Solvents included < 1.0 ng/cm2 of 2-cyclohexen-1-one, 3,5,5-trimethyl- (Isopho-rone), N-formylpiperidine, and 2-(2-butoxyethoxy) ethanol. In addition, DBF, rubber/polymer additive was found at < 0.2 ng/cm2 and caprolactam, nylon-6 at < 0.6 ng/cm2. Reducing Organics: The Apollo program was the last sam-ple return mission to place high-level organic requirements and biological containment protocols on a curation facility. The high vacuum complex F-201 glovebox in the Lunar Receiving Labora-tory used ethyl alcohol (190 proof), 3:1 benzene/methanol (nano grade solution), and heat sterilization at 130degC for 48 hours to reduce organic contamination. In addition, both heat sterilization and peracetic acid sterilization were used in the atmospheric de-contamination (R) cabinets. Later, Lunar curation gloveboxes were degreased with a pressurized Freon 113 wash. Today, UPW has replaced Freon as the standard cleaning procedure, but does not have the degreasing solvency power of Freon. Future Cleaning Studies: Cleaning experiments are cur-rently being orchestrated to study how to degrease and reduce organics in a JSC curation glovebox lower than the established baseline. Several new chemicals in the industry have replaced traditional degreasing solvents such as Freon and others that are now federally restricted. However, these new suites of chemicals remain untested for lowering organics in curation gloveboxes. 3M's HFE-7100DL and DuPont's Vertrel XF are currently being tested as a replacement for Freon 113 as a degreaser at JSC cura-tion facilities. In addition, the use of UPW as a final rinse is be-ing tested, which presumably can maintain a lower total organic carbon load than the filtered purity of chemical solutions. References: [1] Allton J.H. et al. (2012) LPS XLIII, 2439; [2] Calaway M.

Calaway, M. J.↗