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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↗

GeoLab 2011: New Instruments and Operations Tested at Desert RATS

GeoLab is a geological laboratory and testbed designed for supporting geoscience activities during NASA's analog demonstrations. Scientists at NASA's Johnson Space Center built GeoLab as part of a technology project to aid the development of science operational concepts for future planetary surface missions [1, 2, 3]. It is integrated into NASA's Habitat Demonstration Unit, a first generation exploration habitat test article. As a prototype workstation, GeoLab provides a high fidelity working space for analog mission crewmembers to perform in-situ characterization of geologic samples and communicate their findings with supporting scientists. GeoLab analog operations can provide valuable data for assessing the operational and scientific considerations of surface-based geologic analyses such as preliminary examination of samples collected by astronaut crews [4, 5]. Our analog tests also feed into sample handling and advanced curation operational concepts and procedures that will, ultimately, help ensure that the most critical samples are collected during future exploration on a planetary surface, and aid decisions about sample prioritization, sample handling and return. Data from GeoLab operations also supports science planning during a mission by providing additional detailed geologic information to supporting scientists, helping them make informed decisions about strategies for subsequent sample collection opportunities.

Evans, Cindy A.↗

Apollo Next Generation Sample Analysis (ANGSA): A Segue to the Next Era of Lunar Exploration and Sample Return Activities

In the fifty years since the first lunar samples were collected on Apollo 11, significant advancements have taken place in laboratory analysis, planetary science, and astromaterials curation. These advances are now being leveraged for the Apollo Next Generation Sample Analysis (ANGSA) Program, which aims to study specially curated Apollo samples that have never been studied before. Since Apollo 17 in 1972, a great deal has been learned about the Moon, including the unique environments of the poles. Building upon Apollo and remote sensing studies since then, the Artemis Program aims to explore the cold environments near the lunar south pole while achieving the concurrent goals of landing the first woman and the next man on the Moon by 2024. Recent developments for ANGSA have significantly accelerated our readiness for Artemis sample return, particularly in the area of cold sample studies. Four science teams were selected to study cold and/or volatile-bearing samples collected during the Apollo program. These samples have special storage and handling requirements that necessitate their processing in a -20°C environment that meets the Apollo materials and cleanliness requirements. NASA has recently undertaken the development and implementation of a cold sample processing facility to support ANGSA. A similar facility will be needed to process the cold, volatile-bearing samples planned to be returned by Artemis missions; therefore, ANGSA provides excellent preparation for Artemis’ future cold sample processing efforts. We will outline the goals of the ANGSA and Artemis programs, illustrating the complementary nature of the work for both. We will describe the efforts to date in designing, testing, and implementing a cold curation facility that meets the requirements of ANGSA and Apollo curation. We will then outline future work for that facility to reach operational readiness. Finally, we will present the sample collection and curation strategies for Artemis, showing how they overlap and build on ANGSA efforts. The development of cold curation at NASA represents a significant leap in the knowledge, experience, and technologies used in astromaterials curation, opening the door for new investigations of lunar volatiles, impacts, formation processes, prebiotic chemistry, and resource utilization, among many others.

Julie Mitchell↗

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.↗

ARES Biennial Report 2012 Final

Since the return of the first lunar samples, what is now the Astromaterials Research and Exploration Science (ARES) Directorate has had curatorial responsibility for all NASA-held extraterrestrial materials. Originating during the Apollo Program (1960s), this capability at Johnson Space Center (JSC) included scientists who were responsible for the science planning and training of astronauts for lunar surface activities as well as experts in the analysis and preservation of the precious returned samples. Today, ARES conducts research in basic and applied space and planetary science, and its scientific staff represents a broad diversity of expertise in the physical sciences (physics, chemistry, geology, astronomy), mathematics, and engineering organized into three offices (figure 1): Astromaterials Research (KR), Astromaterials Acquisition and Curation (KT), and Human Exploration Science (KX). Scientists within the Astromaterials Acquisition and Curation Office preserve, protect, document, and distribute samples of the current astromaterials collections. Since the return of the first lunar samples, ARES has been assigned curatorial responsibility for all NASA-held extraterrestrial materials (Apollo lunar samples, Antarctic meteorites - some of which have been confirmed to have originated on the Moon and on Mars - cosmic dust, solar wind samples, comet and interstellar dust particles, and space-exposed hardware). The responsibilities of curation consist not only of the longterm care of the samples, but also the support and planning for future sample collection missions and research and technology to enable new sample types. Curation provides the foundation for research into the samples. The Lunar Sample Facility and other curation clean rooms, the data center, laboratories, and associated instrumentation are unique NASA resources that, together with our staff's fundamental understanding of the entire collection, provide a service to the external research community, which relies on access to the samples. The curation efforts are greatly enhanced by a strong group of planetary scientists who conduct peerreviewed astromaterials research. Astromaterials Research Office scientists conduct peer-reviewed research as Principal or Co-Investigators in planetary science (e. g., cosmochemistry, origins of solar systems, Mars fundamental research, planetary geology and geophysics) and participate as Co-Investigators or Participating Scientists in many of NASA's robotic planetary missions. Since the last report, ARES has achieved several noteworthy milestones, some of which are documented in detail in the sections that follow. Within the Human Exploration Science Office, ARES is a world leader in orbital debris research, modeling and monitoring the debris environment, designing debris shielding, and developing policy to control and mitigate the orbital debris population. ARES has aggressively pursued refinements in knowledge of the debris environment and the hazard it presents to spacecraft. Additionally, the ARES Image Science and Analysis Group has been recognized as world class as a result of the high quality of near-real-time analysis of ascent and on-orbit inspection imagery to identify debris shedding, anomalies, and associated potential damage during Space Shuttle missions. ARES Earth scientists manage and continuously update the database of astronaut photography that is predominantly from Shuttle and ISS missions, but also includes the results of 40 years of human spaceflight. The Crew Earth Observations Web site (http://eol.jsc.nasa.gov/Education/ESS/crew.htm) continues to receive several million hits per month. ARES scientists are also influencing decisions in the development of the next generation of human and robotic spacecraft and missions through laboratory tests on the optical qualities of materials for windows, micrometeoroid/orbital debris shielding technology, and analog activities to assess surface science operations. ARES serves as host to numerous students and visiting scientists as part of the services provided to the research community and conducts a robust education and outreach program. ARES scientists are recognized nationally and internationally by virtue of their success in publishing in peer-reviewed journals and winning competitive research proposals. ARES scientists have won every major award presented by the Meteoritical Society, including the Leonard Medal, the most prestigious award in planetary science and cosmochemistry; the Barringer Medal, recognizing outstanding work in the field of impact cratering; the Nier Prize for outstanding research by a young scientist; and several recipients of the Nininger Meteorite Award. One of our scientists received the Department of Defense (DoD) Joint Meritorious Civilian Service Award (the highest civilian honor given by the DoD). ARES has established numerous partnerships with other NASA Centers, universities, and national laboratories. ARES scientists serve as journal editors, members of advisory panels and review committees, and society officers, and several scientists have been elected as Fellows in their professional societies. This biennial report summarizes a subset of the accomplishments made by each of the ARES offices and highlights participation in ongoing human and robotic missions, development of new missions, and planning for future human and robotic exploration of the solar system beyond low Earth orbit.

Stansbery, Eileen↗

Stardust Curation at Johnson Space Center: Photo Documentation and Sample Processing of Submicron Dust Samples from Comet Wild 2 for Meteoritics Science Community

Dust particles released from comet 81P/Wild-2 were captured in silica aerogel on-board the STARDUST spacecraft and successfully returned to the Earth on January 15, 2006. STARDUST recovered thousands of particles ranging in size from 1 to 100 micrometers. The analysis of these samples is complicated by the small total mass collected ( < 1mg), its entrainment in the aerogel collection medium, and the fact that the cometary dust is comprised of submicrometer minerals and carbonaceous material. During the six month Preliminary Examination period, 75 tracks were extracted from the aerogel cells , but only 25 cometary residues were comprehensively studied by an international consortium of 180 scientists who investigated their mineralogy/petrology, organic/inorganic chemistry, optical properties and isotopic compositions. These detailed studies were made possible by sophisticated sample preparation methods developed for the STARDUST mission and by recent major advances in the sensitivity and spatial resolution of analytical instruments.

Nakamura-Messenger, K.↗

Cryogenic Curation: Isolated Technology and Mission Operational Requirements for Sample Return

Future lunar, Mars, asteroid, and comet sample return missions may collect samples that have been preserved at sub-freezing or even cryogenic temperatures. For such samples, the study of volatiles and temperature-sensitive minerals will have high priority. Valuable geochemical and mineralogical information will be lost if such samples are allowed to reach ambient temperatures on Earth. The ability to store, document, subdivide, and transport extraterrestrial geologic samples while maintaining sub-freezing or cryogenic temperatures, possibly as low as 40 K, is required for the complete scientific study of samples from cold environments.

Calaway, Michael J.↗

Geolab in NASA's First Generation Pressurized Excursion Module: Operational Concepts

We are building a prototype laboratory for preliminary examination of geological samples to be integrated into a first generation Habitat Demonstration Unit-1/Pressurized Excursion Module (HDU1-PEM) in 2010. The laboratory GeoLab will be equipped with a glovebox for handling samples, and a suite of instruments for collecting preliminary data to help characterize those samples. The GeoLab and the HDU1-PEM will be tested for the first time as part of the 2010 Desert Research and Technology Studies (DRATS), NASAs annual field exercise designed to test analog mission technologies. The HDU1-PEM and GeoLab will participate in joint operations in northern Arizona with two Lunar Electric Rovers (LER) and the DRATS science team. Historically, science participation in DRATS exercises has supported the technology demonstrations with geological traverse activities that are consistent with preliminary concepts for lunar surface science Extravehicular Activities (EVAs). Next years HDU1-PEM demonstration is a starting point to guide the development of requirements for the Lunar Surface Systems Program and test initial operational concepts for an early lunar excursion habitat that would follow geological traverses along with the LER. For the GeoLab, these objectives are specifically applied to enable future geological surface science activities. The goal of our GeoLab is to enhance geological science returns with the infrastructure that supports preliminary examination, early analytical characterization of key samples, insight into special considerations for curation, and data for prioritization of lunar samples for return to Earth.

Evans, C. A.↗

Advanced Curation Activities at NASA: Preparation for Upcoming Missions

The responsibility for curating NASA's astromaterials collections falls to the NASA Curation Office at Johnson Space Center. Under the governing document, NASA Policy Directive (NPD) 7100.10F and derivative requirements documents, JSC is charged with curation of all extraterrestrial material under NASA control, including future NASA missions to include material returned in Mars Sample Return (MSR) efforts, OSIRIS-REx, NASA's subset of Hayabusa-2 samples, and any other sample return missions. The Directive defines Curation as activities including documentation, preservation, sample preparation, distribution, and tracking of samples for research, education, and public outreach. In this abstract we will describe Curation's research and development efforts to improve the care of existing collections and prepare for future NASA sample return missions. These efforts are collectively referred to as Advanced Curation, a term first coined in 2002.

Fries, M. D.↗

Does Collection Time Bias the Ecology of Cleanroom Air Samples?

Microbial monitoring of astromaterials collections has taken on increased importance with the return of biologically sensitive samples from the asteroids Ryugu and Bennu and the initiation of the Mars Sample Return Program. Terrestrial bacteria and fungi can alter the mineralogy and organic composition of our collections causing irreversible contamination of pristine samples and increasing the risk of false positives for life detection measurements. NASA has conducted routine microbial monitoring of its existing collections since 20181. Initial monitoring focused on surface samples collected with foam swabs. Although, airborne microbiology is often decoupled from surface microbiology in the built environment2 culture-based air sampling techniques like impactors were not compliant with existing contamination control requirements. Bringing organic rich media, gelatin or liquids into curation cleanrooms presents an unacceptable risk to pristine samples. In 2022 NASA purchased a materials complaint air sampler and began collecting air samples from the cleanrooms in addition to surface samples3. The new instrument uses an electret filter to collect samples that are suitable for cultivating organisms or for direct DNA sequencing. Preliminary DNA sequencing results appeared to indicate that longer sampling times biased the microbial community in favor of hearty, spore-forming bacteria3. We present the results of a study comparing overnight sampling (17 hours) to short (1 hour) sampling of unoccupied curation cleanrooms. The results will help us optimize our monitoring protocols and develop a more detailed inventory of the ecology of astromaterials curation cleanrooms. Methods: We analyzed 72 paired air samples from six different cleanrooms including the meteorite processing lab (ISO 7 equivalent, 16 samples), the lunar lab (ISO 6 equivalent, 10 samples), the stardust lab (ISO 5 equivalent 14 samples), the OSIRIS-REx lab (ISO 5 equivalent, 12 samples), the Hayabusa2 lab (ISO 5 equivalent, 14 samples), and the Genesis lab (ISO 4 equivalent, 6 samples). All the samples were collected with an InnovaPrep Bobcat air sampler operating at a sampling rate of 200 L/min. The sampler operates for 5 minutes out of every 20 minute period. Half of the samples were collected by filtering 3,000L (15 min. of active sampling) of air across an electret filter for one hour. The rest of the samples were collected by filtering approximately 51,000 L air across the filter overnight (~17 hours, 255 min. of active sampling). Cells were eluted from the filter using 6-7 ml of pressurized 0.15% tween 20 in PBS (phosphate buffered saline). This liquid was used to cultivate bacteria according to previously published methods1,4,5 and for DNA extraction and next generation sequencing. DNA was extracted with a Qiagen MagAttract PowerMicrobiome kit6. To identify bacteria and archaea, the 16S rRNA gene was amplified using Earth Microbiome primers for the V4 region 7. The amplified DNA was sequenced on an Illumina MiSeq using a V3 reagent kit. The resulting sequences were processed using DADA2 and QIIME2 as implemented on the EDGE bioinformatics platform8–10. Results: Only two of the 72 samples had no amplifiable DNA. Amplified DNA concentrations ranged from 2.67 – 0.272 ng/µl. The median concentration of amplified DNA for the 1 hour samples was 0.770 ± 0.368 ng/µl. The median concentration of amplified DNA for the overnight samples was 0.877 ± 0.434 ng/µl. On average the overnight samples had slightly more sequences (58,960 vs. 59,456) and ASV’s (amplicon sequence variants) (60 vs 64.5) than the one hour samples, but these differences are not statistically significant. The most abundant ASV in every sample mapped to the genus Cupravidus. ASV’s mapping to the genuses Bacillus, Schlegelella, Thermus, and Staphylococcus were also common. Discussion and Future Work: Alpha diversity statistics like Shannon Entropy and Faith Phylogenetic Diversity are used to describe the diversity of organisms in a single sample. If a longer sampling time was biasing the data, we would expect to see a change in these diversity statistics vs. sample time. However, we did not observe this in our data. The median Shannon entropy was slightly higher for the overnight samples (3.773 vs 3.611) as was the Faith Phylogenetic Diversity (4.042 vs 3.596), but both values were within a standard deviation of each other for the two sampling times (Fig. 1). It is unlikely, that the longer sampling time is introducing bias into our data. We do observe a significant decrease in diversity when comparing the air samples by lab. The Genesis lab (ISO 4 equivalent) has a lower median number of ASV’s (45.5) than the other labs (62). Median values for Shannon Entropy (3.717 vs. 3.430) and Faith Phylogenetic Diversity (3.796 vs. 3.548) are also lower for Genesis, but those values are with one standard deviation of each other for the different sampling times. This is consistent with previous culture-based results suggesting that the environment in cleanrooms tends to select for a core group of organisms capable of surviving under dry, low nutrient, conditions. The presence of the ASV’s mapping to Cupravidus and Thermus in our sequencing blanks and controls suggests that several of the most common organisms in our samples represent contaminants from the reagents used to perform the DNA extractions and sequencing. Further work is needed to identify these contaminants, remove them from our data and recalculate the diversity statistics. This is a systematic error. Therefore, we do not expect removing the sequencing contaminants to change our conclusions. Longer air sample collection times appear to result in slightly higher diversity and do not bias the results towards “hardy” bacteria like spore-formers. Based on these preliminary results we conclude that sampling at least 3,000 liters of air is sufficient to capture the microbial diversity of cleanrooms, and that air samples can also be collected overnight without negatively impacting diversity. These results allow us to be flexible when designing microbial monitoring plans so that they do not interfere with routine lab activity. References: 1. Regberg, A. B. et al. 49th Lunar and Planetary Science Conference (2018). 2. The United States Pharmacopeial Convention. USP General Chapter <1116> (2013). 3. Regberg, A. B., et al. 54th Lunar and Planetary Science Conference (2023). 4. Regberg, A. B. et al. 53rd Lunar and Planetary Science Conference ( 2022). 5. Davis, R. E.,et al. 50th Lunar and Planetary Science Conference (2019). 6. Qiagen. MagAttract® PowerMicrobiome® DNA/RNA EP Kit Handbook. (2018). 7. Walters, W. et al. mSystems 1, (2015). 8. Callahan, B. J. et al. Nat. Methods 13, 581–583 (2016). 9. Hall, M. & Beiko, R. G. Microbiome Analysis: Methods and Protocols113–129 (Springer, 2018). 10. Philipson, C. et al. Bio-Protoc. 7, e2622 (2017).

A. B. Regberg↗

Mars Sample Return from Meridiani Planum

The NASA Mars Exploration Program has four main goals: (i) determine if life ever arose there, (ii) understand the processes and history of its climate, (iii) determine the evolution of its surface and interior, and (iv) prepare for human exploration of Mars. These goals are embodied in the NASA Mars exploration strategy Follow the Water. Current Mars exploration tactics for lander missions build on knowledge gained by prior orbital investigations; the science rationale for choosing landing sites is based on the current best interpretation of the geology. A future Mars sample return mission will greatly exceed in cost typical lander missions because of the need to design for return to Earth and the infrastructure needed on Earth to curate and process the samples safely and cleanly. Because of this added cost burden, expectations for science return are higher. There must be some prospect that the returned samples will allow for testing higher level hypotheses relevant to NASA's goals. Site selection must be based on knowledge gained from prior in situ measurements to enhance the prospects for successfully meeting these goals. I will argue that Meridiani Planum should be that site.

Mittlefehldt, David W.↗

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.↗

Hydrogen Peroxide as a Method for Bioburden Reduction in Facilities with Strict Materials Requirements.

The cleanrooms used to curate NASA’s Astromaterials samples are carefully monitored for particulate and inorganic contamination. The clean labs also have a very limited set of acceptable materials and cleaning agents to further minimize the potential for contamination. Labs are cleaned primarily with isopropyl alcohol. Astromaterials samples are handled with tools made of stainless steel (304 or 316), Teflon, or aluminum alloy (6061). Although our current collections are not particularly susceptible to biological alteration or organic contamination, this will not be the case for new collections from the OSIRIS-REx mission, Hayabusa2, and from Mars Sample Return. Therefore, it is necessary to develop and test methods to reduce the bioburden in astromaterials cleanrooms without introducing unwanted contaminants. We will report on the results of three case studies where 7.5 wt% hydrogen peroxide was prepared from a stock solution of ultrapure 30 wt% hydrogen peroxide (JT Baker) using curation-grade ultrapure water. We followed CDC (Center for Disease Control) guidelines for using hydrogen peroxide as a high level disinfectant. This solution was used to clean a glovebox prior to processing Apollo samples, as well as surfaces in the Antarctic meteorite processing lab and Stardust lab after facilities monitoring indicated an unwanted increase in bioburden. In all three instances, the culturable bioburden was significantly reduced after a 30 min. exposure to the 7.5% hydrogen peroxide solution without a corresponding increase in inorganic or organic contamination. We observed 77 to 100% reductions in the bioburden recovery rate. In one case study, we also performed amplicon DNA sequencing on samples collected from the surfaces before and after cleaning. We observed a significant change in microbial community composition after peroxide cleaning. These results suggest that routine cleaning with hydrogen peroxide could be an effective way to control bioburden in astromaterials cleanrooms and other facilities with strict contamination control requirements.

A B Regberg↗

Hydrogen Peroxide as a Method for Bioburden Reduction in Facilities with Strict Materials Requirements

The cleanrooms used to curate NASA’s Astromaterials samples are carefully monitored for particulate and inorganic contamination. The clean labs also have a very limited set of acceptable materials and cleaning agents to further minimize the potential for contamination. Labs are cleaned primarily with isopropyl alcohol. Astromaterials samples are handled with tools made of stainless steel (304 or 316), Teflon, or aluminum alloy (6061). Although our current collections are not particularly susceptible to biological alteration or organic contamination, this will not be the case for new collections from the OSIRIS-REx mission, Hayabusa2, and from Mars Sample Return. Therefore, it is necessary to develop and test methods to reduce the bioburden in astromaterials cleanrooms without introducing unwanted contaminants. We will report on the results of three case studies where 7.5 wt% hydrogen peroxide was prepared from a stock solution of ultrapure 30 wt% hydrogen peroxide (JT Baker) using curation-grade ultrapure water. We followed CDC (Center for Disease Control) guidelines for using hydrogen peroxide as a high level disinfectant. This solution was used to clean a glovebox prior to processing Apollo samples, as well as surfaces in the Antarctic meteorite processing lab and Stardust lab after facilities monitoring indicated an unwanted increase in bioburden. In all three instances, the culturable bioburden was significantly reduced after a 30 min. exposure to the 7.5% hydrogen peroxide solution without a corresponding increase in inorganic or organic contamination. We observed 77 to 100% reductions in the bioburden recovery rate. In one case study, we also performed amplicon DNA sequencing on samples collected from the surfaces before and after cleaning. We observed a significant change in microbial community composition after peroxide cleaning. These results suggest that routine cleaning with hydrogen peroxide could be an effective way to control bioburden in astromaterials cleanrooms and other facilities with strict contamination control requirements.

A B Regberg↗

Collection requirements for trace-element analyses of extraterrestrial samples

Trace-element abundances have proven important in understanding the evolution of and interrelationships between different meteorites. Preliminary investigations of the trace-element contents of interplanetary dust particles indicate that trace-element abundances will prove equally important in distinguishing between micrometeorites of different types, comparing the interplanetary dust to the meteorites, and assessing the degree of thermal alteration experienced either on the parent body or during the collection process. Sample collection, delivery, and curation must be accomplished in a manner to avoid contamination with even trace amounts of the elements to be analyzed. The present SXRF sensitivity for micrometeorite analysis is of order 1 femtogram, but anticipated improvements in sensitivity will require sample contamination substantially below this level. Sample collection and handling equipment should be constructed from materials selected for ultrahigh purity, and serious consideration should be given in selecting the particular set of elements from which the collection apparatus is composed so as not to compromise useful information.

Flynn, George J.↗

Preliminary Examination of Particles Recovered from the Surface of the Asteroid Itokawa by the Hayabusa Mission

The Hayabusa spacecraft arrived at S-type Asteroid 25143 Itokawa in November 2006, and reveal astounding features of the small asteroid (535 x 294 x 209 m). Near-infrared spectral shape indicates that the surface of this body has an olivinerich mineral assemblage potentially similar to that of LL5 or LL6 chondrites with different degrees of space weathering. Based on the surface morphological features observed in high-resolution images of Itokawa s surface, two major types of boulders were distinguished: rounded and angular boulders. Rounded boulders seem to be breccias, while angular boulders seem to have severe impact origin. Although the sample collection did not be made by normal operations, it was considered that some amount of samples, probably small particles of regolith, was collected from MUSES-C regio on the Itokawa s surface. The sample capsule was successfully recovered on the earth on June 13, 2010, and was opened at curation facility of JAXA (Japan Aerospace Exploration Agency), Sagamihara, Japan. A large number of small particles were found in the sample container. Preliminary analysis with SEM/EDX at the curation facility showed that at least more than 1500 grains were identified as rocky particles, and most of them were judged to be of extraterrestrial origin, and definitely from Asteroid Itokawa. Minerals (olivine, low-Ca pyroxene, high-Ca pyroxene, plagioclase, Fe sulfide, Fe-Ni metal, chromite, Ca phosphate), roughly estimated mode the minerals and rough measurement of the chemical compositions of the silicates show that these particles are roughly similar to LL chondrites. Although their size are mostly less than 10 m, some larger particles of about 100 m or larger were also identified. A part of the sample (probably several tens particles) will be selected by Hayabusa sample curation team and examined preliminary in Japan within one year after the sample recovery in prior to detailed analysis phase. Hayabusa Asteroidal Sample Preliminary Examination Team (HASPET) has been preparing for the preliminary examination with close cooperation with the curation team.

Tsuchiyama, A.↗

Application of Long-Path Gas Cell Assisted Infrared Spectroscopy for Detection of Lunar Volatiles and Advanced Curation Efforts

The motivation behind analyzing gaseous samples from the Permanently Shadowed Regions (PSRs) on the lunar surface is built upon the volatiles observed during the LCROSS mission. Advanced curation techniques under cold conditions are essential to the critical scientific analysis of these returned samples. The detection of various volatiles in returned samples by gas-phase infrared (IR) spectroscopy is known to be a powerful tool to understand the resources present in planetary bodies and Astro-materials. The identification and quantification of volatile compounds in returned planetary samples and regolith simulants by advanced and custom-built analytical devices are areas of primary research interest in our group and the Planetary Exploration & Astromaterials Research Laboratory (PEARL) facility. In this context, we discuss recent advancements and experimental results for quick analysis of the major volatiles detected by the LCROSS (water, CO 2 , CH 3 OH, and NH 3 ) by a long-path gas cell/FTIR (Fourier Transform Infrared) spectrometer system. The applicability of this system is demonstrated by qualitative analysis of a series of volatiles measured individually. In addition, the linear dependence of absorption intensity on headspace sample volumes was checked by measuring gas-phase IR absorption spectra of increasing volumes of pure CO 2 gas aliquots. Finally, the instrument performance was evaluated by measuring the relative concentration of NH 3 (g) in methanol solution.

Curation↗