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NASA NTRS2018

Hydrovolcanic Astromaterials in the Lab

Zag and Monahans (1998) are H chondrite regolith breccias that contain 4.5 GY old halite crystals which in turn contain abundant inclusions of aqueous fluids, solids and organics. We have previously proposed that these halites originated on a hydrovolcanically-active C class asteroid, probably Ceres, or a trans-neptunian object (TNO - or P- or D-class asteroid) injected into the inner solar system during giant planet migration. We have begun a detailed analysis of organics and other solids trapped within the halite, which we hypothesize sample the mantle of the halite parent object, and are examining a halite-bearing C1 chondrite clast also found in Zag, which is similar to the solids in the halite. These investigations will reveal the water-rock interactions on the hydrovolcanically-active parent world.

Zolensky, M. E.↗
NASA NTRS2020

Use of an Internal Mercury-Argon Lamp for the Calibration of Raman Frequency in Large Raman Images of Astromaterials

Raman imaging is an emerging tool for the analysis of meteorites, as it is capable of describing mineralogy, carbon composition/speciation, and crystal orientation all within a petrographic context. Adequately examining the heterogeneous composition of a meteorite, while maintaining low laser powers needed to prevent damage to meteorite mineralogy and organics, often requires the collection of large Raman images with long collection times on the timescale of days. However, the frequency calibration of the Raman instrument/spectrometer drifts on long timescales resulting in low frequency precision for the Raman spectra comprising a large Raman image. This decrease in frequency precision can compromise the analysis of geological markers that can provide important information on a meteorite sample. We examine, in detail, the change in bandwidth and frequency of the Raman bands and Hg-Ar emission lines in our Raman images as a function of time and laboratory temperature. To overcome the drift in calibration, we utilize a commercial WITec Raman instrument with an internal Hg-Ar calibration lamp to individually calibrate each spectrum in the Raman image. Our instrument, known as “Ratatoskr”, uses a beam splitter in place of the customary mirror to facilitate collection of Hg-Ar calibration lines concurrent with Raman spectra. We show that using the internal calibration we can improve the frequency precision for the spectra in our Raman images from ~±0.15 cm(exp -1) to ~±0.05 cm(exp -1) for Raman spectra collected over multiple days. This is important as it improves measurements of mineral chemistry, latent strain, and other features that are dependent upon accurate peak position determination. We also examine the spectral signal-to-noise ratio needed to minimize the frequency error when fitting bands to Gaussian/Lorentzian profiles. We then use our results to suggest a general method for calibrating the frequency of Raman spectra in large Raman images.

Jakubek, Ryan S.↗
NASA NTRSDate not supplied

Use of an Internal Mercury-Argon Lamp for the Calibration of Raman Frequency in Large Raman Images of Astromaterials

Raman imaging is an emerging tool for the analysis of meteorites, as it is capable of describing the mineralogy and organics within a petrographic context. Adequately examining the heterogeneous composition of a meteorite often requires the collection of large Raman images with long collection times on the time-scale of days. However, the frequency calibration of the Raman instrument/spectrometer drifts on long timescales resulting in low frequency precision for the Raman spectra comprising a large Raman image. Here we utilize a Hg-Ar calibration lamp integrated into our Raman microscope to calibrate the Raman spectra within a Raman image. We characterize this method of calibration in detail.

Ryan S. Jakubek↗
NASA NTRSDate not supplied

Stable Chlorine Isotope Measurements of Astromaterials Using the Cs-Sputter Negative Ion Source of an Accelerator Mass Spectrometer

The volatile element Cl can be lost during the formation and evolution of planetary bodies, leading to fractionation of its two stable isotopes 35Cl and 37Cl. Chlorine isotope variations (reported as δ37Cl in parts per thousand (‰) relative to Standard Mean Ocean Chloride, SMOC) [1] are documented to exceed 80‰ [2] between different lunar rock samples and have been variably interpreted as the fingerprint of degassing during accretion, magma ocean, or volcanic portions of lunar history[3,4].The large intersample and intrasample variations observed by both bulk isotope ratio mass spectrometry (IRMS) and in-situ secondary ion mass spectrometry (SIMS) methods are difficult to interpret in part because of a paucity of bulk Cl isotope measurements (Figure 1).This lack of high-precision bulk data is due to the relative rarity of IRMS laboratories capable of making these high precision measurements on small samples of precious planetary materials such as those returned by human or robotic exploration. Here we present a new method for performing high precision δ37Cl measurements using the Cs-sputter negative ion source of an existing accelerator mass spectrometer. A brief description of the methods used for this work is followed by the results of our δ37Cl measurements and a discussion of the technique’s possible applications.

Chlorine↗
NASA NTRSDate not supplied

A New Coordinated NanoSIMS, Transmission Electron Microscopy and Atom Probe Tomography Approach For the Characterization of Primitive Astromaterials

Presolar grains are remnants of evolved stellar systems preserved within primitive extraterrestrial materials. They are important for studying physical and chemical processing, and formation mechanisms occurring within the interstellar medium, Solar Nebula and their parent stellar environments [1]. Our recent work has shown coordinated nano-scale Secondary Ion Mass Spectrometry (NanoSIMS) and Atom Probe Tomography (APT) can show isotopic and chemical signatures at major to trace levels, morphological signatures, and regional contextual relationships [2,3]. Previous studies have shown Transmission Electron Microscopy (TEM) of Focus Ion Beam (FIB) TEM lamella, can provide localized contextual relationships, crystallographic information and chemical information [1]. Coordinating NanoSIMS, TEM, and APT could gain access to almost all contextual, structural and geochemical signatures within each presolar grain. However, this has proved challenging owing to the preparation requirements for TEM and APT. For example, studying specimen prepared as APT needles in TEM removes the local context, the higher degree of surface exposure can alter the chemistry of beam sensitive materials, and the shank angle of the needle can impact the quality of TEM diffraction images. We designed a new FIB method which takes a 100 nm thick FIB-TEM lamella and sandwiches it between two indium slices (5 μm x ~300 nm x 3 μm). The indium is melted onto the lamella surface using the electron beam (Fig 1). This process adds bulk to the lamella, making it more amenable to APT needle formation (Fig 2). Consequently, samples can be prepared per the optimal requirements for each technique improving data quality, acquisition stability, and access to the signatures and relationships summarised earlier. This technique can be used for measuring multiple phases across a TEM lamella and targeting an individual phase. For example, a presolar grain identified in NanoSIMS could be targeted, studied in TEM and then indium sandwiched with its precise location in the TEM lamella marked using a Pt button for preparation of an APT needle and atomic scale acquisition. [1] A. M. Davis (2014) Meteorites and cosmochemical processes, 1. [2] Nevill N. et al. (2023) LPSC, 54, #1707. [3] Nevill N. et al. (2023) LPSC, 54, #1714.

NanoSIMS↗
NASA NTRSDate not supplied

NASA Johnson Space Center Astromaterials Research Exploration Science Image Science and Analysis Group (ISAG) ISAG Support to the ISS Program

- Primary focus is on maintaining the safety of the crew and vehicle. - ISAG personnel request and screen imagery to: - Monitor changes in the ISS external condition - Anomalous indications - Hardware out of configuration - Detect Micro-Meteoroid or Orbital Debris (MMOD) impacts leading to: - Hardware failure - EVA sharp edges - ISAG personnel derive engineering data from imagery for: - Anomaly investigations - Structural dynamics measurements - Clearance assessments - Verifying ISS configuration against models and requirements - Jettison trajectory calculation - Provide Real-Time Support to the ISS and Anomalies

Dwight Osborne↗
NASA NTRS2014

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↗
NASA NTRSDate not supplied

Microbial Monitoring of New Cleanrooms Used to Curate Astrobiologically Relevant Asteroid Samples from Bennu and Ryugu

Introduction: NASA has constructed two new cleanrooms to house materials from the OSRIS-REx and Hayabusa2 missions to the asteroids Ryugu (162173) and Bennu (101955), respectively. In accordance with standard astromaterials curation practices, these cleanrooms will be monitored for particulate contamination and maintained to ISO 5 equivalent standards1. Since the samples in these collections are expected to contain prebiotic organic compounds that may help explain the origin of life on Earth, these labs will also be monitored for organic and biological contamination2. Samples from Ryugu arrived on Earth in December, 2020. After basic characterization in Japan, NASA received a subset of these samples at the astromaterials curation facility in Houston in December of 2021. OSIRIS-REx is expected to return samples in September, 2023. Here we present preliminary microbial monitoring results from monthly monitoring of these new labs and the connected microtomy and staging areas that support them, as they are being commissioned. We also compare these results to baseline values for other astromaterials curation labs. We will also briefly describe additional cleaning efforts employed to reduce the bioburden in these new cleanrooms. Methods: Microbial samples were collected from surfaces using a dry macrofoam swab (Puritan Brand 2518051PFRNDFD). Swabs were also opened in the lab but not touched to any surfaces to function as negative controls. Samples and controls were processed inside a class II biosafety cabinet to avoid inadvertent cross contamination. The swabs were suspended in 15 ml of PBS (Phosphate Buffered Saline) and vortexed for 20 seconds to remove cells from the swab surface. The PBS was used to inoculate Petri dishes filled with TSA (Tryptic Soy Agar), Blood Agar, or Reasoners 2 agar to check for microbial growth. Each plate was inoculated with 0.1 ml of PBS. The TSA and blood agar plates were incubated at 35˚C and the Reasoners 2 agar plates were incubated at 25˚C for seven days. Petri dishes filled with Potato dextrose agar, Saboraud dextrose agar, or Saboraud dextrose agar with 0.1 mg/ml of chloramphenicol, an antibiotic, were used to check for fungal growth. These plates were inoculated with 0.3 ml of PBS and incubated at 30˚C. The remaining PBS was frozen at -80 ˚C for DNA sequencing. After incubation, isolates were counted and reisolated for identification. Isolates were identified using the VITEK23 system or by sequencing a portion of the 16S rRNA gene for bacteria or the ribosomal internal transcribed spacer (ITS) for fungi. Sequencing was performed with an ABI 3500 Sanger sequencer. Results: During our initial sampling, six of the seven sites sampled (86%) displayed bacterial or fungal growth. Samples collected from the staging areas and microtomy labs are not included in this calculation since those areas are maintained at a lower ISO 7 equivalent cleanliness standard. A month later, only three of the seven sites (43%) displayed bacterial growth. No fungal growth was detected in the second sampling. Since new equipment had been introduced to the Hayabusa2 lab since the first round of sampling, an additional three sampling sites were included in the second round of sampling. None of these sites displayed microbial growth. These sites will be included in all future sampling efforts. Bacterial isolates have been identified from the following genera at multiple time points: Micrococcus, Staphylococcus, and Bacillus. Isolates from the genera: Microbacterium, Nocardioides, Methylocystis, and Microvirga were identified in the initial sampling, but were not present at later time points. Identification of fungal isolates is in progress. Results are summarized in Table 1. Discussion: The recovery rate or percentage of positive samples4 was initially 86%, which is higher than the median recovery rate for comparable ISO 5 equivalent curation labs like Stardust (33%), Hayabusa (33%), and Cosmic Dust (50%). However, after a month of operation, the recovery rate for these same sites decreased to 43%, which is similar to what we observe in comparable curation cleanrooms with no microbial control requirements. Adding in the new sampling sites further decreases the recovery rate to 30%. With the reduction in recovery rate, we also observed a decrease in microbial diversity. At the first time point, we observed at least 10 different bacterial species and at least two different fungi. This is a higher diversity than the median values for comparable ISO 5 equivalent labs (2-4 isolates per sampling event). After the second sampling, we observed at least 4 bacterial species and no fungi, which is more consistent with comparable labs. We expect the recovery rate and diversity in both labs to continue to decrease as routine operation continues. We will use ultrapure hydrogen peroxide to disinfect equipment and work areas prior to opening any sample containers. Most of the bacterial and fungal isolates were detected on samples from the cleanroom floors. This is consistent with baseline results from other curation labs. Organisms from the genera Bacillus, Staphylococcus, and Micrococcus that were repeatedly detected are common in cleanrooms and on human skin5,6. These organisms are generally thought to be introduced when people enter the cleanroom. Microbacterium, Nocardioides, and Microvirga have also previously been identified in astromaterials cleanrooms, but not as frequently as Bacillus, Staphylococcus, and Micrococcus. Methylocystis is a novel genus in the astromaterials cleanrooms, but it was identified with low accuracy (93% match in the sequenced region of the 16S rRNA gene) and further work is needed to confirm this identification. Microbacterium is a diverse genus with isolates identified from terrestrial and aquatic sediments. Some species of Microbacterium are capable of degrading complex organic compounds found in crude oil. The presence of these bacteria in the OSIRIS REx and Hayabusa2 cleanrooms should be closely monitored. Methylocystis is a genus of methanotrophic bacteria capable of oxidizing methane. If this identification proves to be correct and it is detected again, it should be closely monitored as well. Under nominal operating conditions, samples should not ever encounter the cleanroom floor or other high traffic areas. If we observe an increase in the bioburden in sensitive work areas that appears to be influenced by organism transfer from high traffic areas like the floors, we can employ additional hydrogen peroxide treatments to disinfect high traffic areas. Routine microbial monitoring of these labs will ensure that NASA’s astromaterials collections remain pristine and useful for scientific study. Table 1. Sampling Locations and Colony Counts Bacterial CFUa Fungal CFU Bacterial CFU Fungal CFU Lab - Location 11/2/2021 11/2/2021 12/13/2021 12/13/2021 H2b-Floor 4 8 1 0 H2-staging pass through 3 0 0 0 H2-microtomy pass through TNTCc 0 0 0 H2 Microscope 1 NA NA 0 0 H2 Microscope 2 NA NA 0 0 H2-Table NA NA 0 0 OREXd- microtomy pass through 0 0 6 0 OREX – Anteroom pass through 0 0 0 0 OREX – Floor 1 2 0 0 OREX Witness Foil Table 3 0 1 0 Staging-Floor 16 0 15 0 Microtomy-Floor 3 0 2 0 a: CFU = Colony Forming Unit b: H2 = Hayabusa2 Lab c: TNTC = too numerous to count d: OREX = OSIRIS-REx Lab References: 1. ISO 14644-1:2015 - Cleanrooms and associated controlled environments -- Part 1: Classification of air cleanliness by particle concentration. 37 (2015). 2. McCubbin, F. M. et al. Space Sci Rev 215, (2019). 3. Pincus, D. H. Encyclopedia of Rapid Microbiological Methods (2005). 4. The United States Pharmacopeial Convention. USP General Chapter <1116> 17, 784–794 (2013). 5. Sheraba, N. S., Yassin, A. S. & Amin, M. BMC Research Notes 3, 278 (2010). 6. Utescher, C. L. de A., Franzolin, M. R., Trabulsi, L. R. & Gambale, V. Brazilian Journal of Microbiology 38, 710–716 (2007).

A B Regberg↗
NASA NTRS2015

Comprehensive Non-Destructive Conservation Documentation of Lunar Samples Using High-Resolution Image-Based 3D Reconstructions and X-Ray CT Data

Established contemporary conservation methods within the fields of Natural and Cultural Heritage encourage an interdisciplinary approach to preservation of heritage material (both tangible and intangible) that holds "Outstanding Universal Value" for our global community. NASA's lunar samples were acquired from the moon for the primary purpose of intensive scientific investigation. These samples, however, also invoke cultural significance, as evidenced by the millions of people per year that visit lunar displays in museums and heritage centers around the world. Being both scientifically and culturally significant, the lunar samples require a unique conservation approach. Government mandate dictates that NASA's Astromaterials Acquisition and Curation Office develop and maintain protocols for "documentation, preservation, preparation and distribution of samples for research, education and public outreach" for both current and future collections of astromaterials. Documentation, considered the first stage within the conservation methodology, has evolved many new techniques since curation protocols for the lunar samples were first implemented, and the development of new documentation strategies for current and future astromaterials is beneficial to keeping curation protocols up to date. We have developed and tested a comprehensive non-destructive documentation technique using high-resolution image-based 3D reconstruction and X-ray CT (XCT) data in order to create interactive 3D models of lunar samples that would ultimately be served to both researchers and the public. These data enhance preliminary scientific investigations including targeted sample requests, and also provide a new visual platform for the public to experience and interact with the lunar samples. We intend to serve these data as they are acquired on NASA's Astromaterials Acquisistion and Curation website at http://curator.jsc.nasa.gov/. Providing 3D interior and exterior documentation of astromaterial samples addresses the increasing demands for accessability to data and contemporary techniques for documentation, which can be realized for both current collections as well as future sample return missions.

Blumenfeld, E. H.↗
NASA NTRS2015

JSC Advanced Curation: Research and Development for Current Collections and Future Sample Return Mission Demands

Curation of NASA's astromaterials sample collections is a demanding and evolving activity that supports valuable science from NASA missions for generations, long after the samples are returned to Earth. For example, NASA continues to loan hundreds of Apollo program samples to investigators every year and those samples are often analyzed using instruments that did not exist at the time of the Apollo missions themselves. The samples are curated in a manner that minimizes overall contamination, enabling clean, new high-sensitivity measurements and new science results over 40 years after their return to Earth. As our exploration of the Solar System progresses, upcoming and future NASA sample return missions will return new samples with stringent contamination control, sample environmental control, and Planetary Protection requirements. Therefore, an essential element of a healthy astromaterials curation program is a research and development (R&D) effort that characterizes and employs new technologies to maintain current collections and enable new missions - an Advanced Curation effort. JSC's Astromaterials Acquisition & Curation Office is continually performing Advanced Curation research, identifying and defining knowledge gaps about research, development, and validation/verification topics that are critical to support current and future NASA astromaterials sample collections. The following are highlighted knowledge gaps and research opportunities.

Fries, M. D.↗
NASA NTRS2014

GeoLab: A Geological Workstation for Future Missions

The GeoLab glovebox was, until November 2012, fully integrated into NASA's Deep Space Habitat (DSH) Analog Testbed. The conceptual design for GeoLab came from several sources, including current research instruments (Microgravity Science Glovebox) used on the International Space Station, existing Astromaterials Curation Laboratory hardware and clean room procedures, and mission scenarios developed for earlier programs. GeoLab allowed NASA scientists to test science operations related to contained sample examination during simulated exploration missions. The team demonstrated science operations that enhance theThe GeoLab glovebox was, until November 2012, fully integrated into NASA's Deep Space Habitat (DSH) Analog Testbed. The conceptual design for GeoLab came from several sources, including current research instruments (Microgravity Science Glovebox) used on the International Space Station, existing Astromaterials Curation Laboratory hardware and clean room procedures, and mission scenarios developed for earlier programs. GeoLab allowed NASA scientists to test science operations related to contained sample examination during simulated exploration missions. The team demonstrated science operations that enhance the early scientific returns from future missions and ensure that the best samples are selected for Earth return. The facility was also designed to foster the development of instrument technology. Since 2009, when GeoLab design and construction began, the GeoLab team [a group of scientists from the Astromaterials Acquisition and Curation Office within the Astromaterials Research and Exploration Science (ARES) Directorate at JSC] has progressively developed and reconfigured the GeoLab hardware and software interfaces and developed test objectives, which were to 1) determine requirements and strategies for sample handling and prioritization for geological operations on other planetary surfaces, 2) assess the scientific contribution of selective in-situ sample characterization for mission planning, operations, and sample prioritization, 3) evaluate analytical instruments and tools for providing efficient and meaningful data in advance of sample return and 4) identify science operations that leverage human presence with robotic tools. In the first year of tests (2010), GeoLab examined basic glovebox operations performed by one and two crewmembers and science operations performed by a remote science team. The 2010 tests also examined the efficacy of basic sample characterization [descriptions, microscopic imagery, X-ray fluorescence (XRF) analyses] and feedback to the science team. In year 2 (2011), the GeoLab team tested enhanced software and interfaces for the crew and science team (including Web-based and mobile device displays) and demonstrated laboratory configurability with a new diagnostic instrument (the Multispectral Microscopic Imager from the JPL and Arizona State University). In year 3 (2012), the GeoLab team installed and tested a robotic sample manipulator and evaluated robotic-human interfaces for science operations.

Evans, Cynthia↗