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All sourcesNASA NTRSDOE OSTI
NASA NTRS2017

Sample Curation in Support of the OSIRIS-REx Asteroid Sample Return Mission

The OSIRIS-REx asteroid sample return mission launched to asteroid Bennu Sept. 8, 2016. The spacecraft will arrive at Bennu in late 2019, orbit and map the asteroid, and perform a touch and go (TAG) sampling maneuver in July 2020. After sample is stowed and confirmed the spacecraft will return to Earth, and the sample return capsule (SRC) will land in Utah in September 2023. Samples will be recovered from Utah [2] and then transported and stored in a new sample cleanroom at NASA Johnson Space Center in Houston [3]. The materials curated for the mission are described here. a) Materials Archive and Witness Plate Collection: The SRC and TAGSAM were built between March 2014 and Summer of 2015, and instruments (OTES,OVIRS, OLA, OCAMS, REXIS) were integrated from Summer 2015 until May 2016. A total of 395 items were received for the materials archive at NASA-JSC, with archiving finishing ~30 days after launch (with the final archived items being related to launch operations)[4]. The materials fall into several general categories including metals (stainless steel, aluminum, titanium alloys, brass and BeCu alloy), epoxies, paints, polymers, lubricants, non-volatile-residue samples (NVR), sapphire, and various miscellaneous materials. All through the ATLO process (from March 2015 until late August 2016) contamination knowledge witness plates (Si wafer and Al foil) were deployed in the various cleanrooms in Denver and KSC to provide an additional record of particle counts and volatiles that is archived for current and future scientific studies. These plates were deployed in roughly monthly increments with each unit containing 4 Si wafers and 4 Al foils. We archived 128 individual witness plates (64 Si wafers and 64 Al foils); one of each witness plate (Si and Al) was analyzed immediately by the science team after archiving, while the remaining 3 of each are archived indefinitely. Information about each material archived is stored in an extensive database at NASA-JSC, and key summary information for each will be presented in an online catalog. b) Bulk Asteroid sample: The Touch and Go Sampling Mechanism (TAGSAM) head will contain up to 1.5 kg of asteroid material. Upon return to Earth, the TAGSAM head with the sample canister will be subjected to a nitrogen purge and then opened in a nitrogen cabinet in Houston. Once the TAGSAM head is removed from the canister, it will be dis-assembled slowly and carefully under nitrogen until the sample can be removed for processing in a dedicated nitrogen glovebox. Bennu surface samples are expected to be sub-cm sized, based on thermal infrared and radar polarization ratio measurements [1]. The upper limit on material collected by the TAGSAM head is ~2 cm. Therefore, we will be prepared to handle, subdivide, and characterize materials of a wide grain size (from ~10 m to 2 cm), and for both organic (UV fluorescence) and inorganic (SEM, FTIR, optical) properties. Representative portions of the bulk sample will be prepared for JAXA (0.5 %; see also [5]) and Canadian Space Agency (4%), with the remaining divided between the science team (<25%) and archived for future studies (NASA) (>75%). c) Contact Pad samples: The base of the TAGSAM head contains 24 contact pads that are designed to trap the upper surface layer of material and thus offer an opportunity to study asteroid samples that have resided at the very top surface of the regolith. Asteroid material is trapped on the pads in spring steel Velcro hooks, and material will have to be removed from these pads by curation specialists in the lab. d) Hardware: Some canister and SRC hardware items will contain information that will be important to understanding the collected samples, including the canister gas filter, temperature strips, flight witness plates, and the TAGSAM and canister parts that might have adhering dust grains. Some challenges remaining for both bulk sample and contact pad samples include: i) working with intermediate size range (200 to 500 micron) samples - a size range NASA has not previously worked in such detail; ii) techniques for removal of contact pad material from the spring steel hooks, iii) static electrical effects of dust sized particles during sample handling and curation is likely to be significant, and iv) the TAGSAM head and associated canister hardware will undoubtedly be coated with fine adhering dust grains from Bennu. In the case of collection of a large bulk sample mass, the adhering dust grains may be of lower priority. If a small sample mass is returned, the adhering dust may attain a higher priority, so recovery of adhering dust grains is an additional challenge to consider. In the year leading up to sample return we plan a variety of sample handling rehearsals that will enables the curation team to be prepared for many new aspects posed by this sample suite.

Righter, Kevin↗
NASA NTRS2022

Sample Materials Considerations for Curating and Processing Pristine MSR Samples

The perseverance rover is collecting and caching samples of Mars as part of the Mars 2020 mission, which represents the first leg of a multi-mission Mars Sample Return Campaign. The MSR Campaign is an international partnership that will result in delivery of the first martian samples to Earth that were not delivered through meteoritic infall. All meteorites, regardless of how they were handled from recovery to curation, have experienced uncontrolled entry and exposure to the terrestrial environment. Whilst meteorite deliveries are serendipitous, they are also unplanned events that require reactionary responses for recovery and curation. However, with the direct return of pristine astromaterials from another body, we are afforded the ability to design a facility in advance of sample delivery to keep those samples in a pristine (i.e., as returned) state for an indefinite period of time. Given that the curation and processing infrastructure needs to be made out of something, it is important to choose materials for the pristine curation environment that will optimize between the need to effectively process samples and the need to minimize contamination of the samples. The Johnson Space Center (JSC) has an optimized list of materials that have been used in previous sample return missions that includes 304/316 Stainless Steel, Teflon, and T6061 Aluminum (1). This set of materials are compatible with inorganic, organic, and biological cleanliness requirements and protocols. Furthermore, only these materials are permitted to come in contact with pristine samples. We note that JSC uses Neoprene and Hypalon for the gloves on their gloveboxes, but the glove material never comes in direct contact with the samples, only the approved materials. The MSR sample tubes will be made of Ti, so Ti may be an acceptable material for making tools, but the minor and trace element abundances of 304 and 316 stainless steel are well known and do not inhibit scientific investigations of metals, including HSE (2). More work is needed to determine whether the same is true for Ti alloys. In addition to defining the materials in the pristine environment, one must also choose whether the pristine environment will be under vacuum or under a specific atmospheric composition and pressure. Although JAXA has successfully implemented pristine curation vacuum chambers for their Hayabusa and Hayabusa2 samples (3), a vacuum environment is not appropriate for martian samples because it may drive deliquescence of mineral phases in the samples that are sensitive to pressure and relative humidity (4). Consequently, the pristine environment for the martian samples should be under an inert gas. It will be crucial to minimize the number of gases that come into direct contact with samples and these gases will need to be high purity and consistent throughout the pristine isolators. Samples at JSC are stored under high purity gaseous nitrogen (1). Dry N2 gas has not been a problem for N isotope studies for high-T release phases, but an additional inert atmosphere like Ar may be needed for samples where there is a particular concern about low-T release of N from bulk sample analysis. References: (1) McCubbin FM, et al. (2019) Space Science Reviews, 215, 1-81. (2) Day JMD, et al. (2018) Meteorit. Planet. Sci. 53:1283-1291. (3) Yada, T., et al., (2014). Meteorit. Planet. Sci. 49, 135-153. (4) Tosca NJ, et al. (2021). Astrobiology, in press, doi:10.1089/ast.2021.0115.

F M McCubbin↗
DOE OSTI2026

SPRUCE: Peat Core Sample Collection Metadata, Marcell Experimental Forest, Minnesota, August 2024

This data set contains metadata associated with peat core samples collected from the Spruce and Peatland Responses Under Changing Environments (SPRUCE) experiment in August 2024. This sample metadata contains no analytical results and is a reference for analytical datasets. To ensure accessibility and discoverability, each sample was assigned an International Generic Sample Number (IGSN), a persistent identifier, using System for Earth and Extraterrestrial Sample Registration (SESAR). These samples were used for downstream analysis by multiple teams of researchers the results of which will be reported separately. This dataset contains one data file in comma separate (.csv) format. Additional metadata are provided: one data dictionary and a file-level metadata file in comma separate (.csv) format and a user guide in PDF (*.pdf) format. An aliquot of most samples is stored at Oak Ridge National Laboratory and may be available for further analysis. Access this collection event on SESAR https://doi.org/10.58052/IEJ9B00VQ. To inquire about obtaining archived samples for analysis, reach out using the Contact Sample Owner form located on the bottom of the landing page in SESAR. Note: Only dried and ground material from C Cores are available for new analysis.

Birkebak, Joshua [ORNL] (ORCID:0009000955611494)↗
NASA NTRSDate not supplied

From Apollo to Artemis: How Processing ANGSA Core Samples 73001/2 Can Help to Prepare for Future Sample Return Missions to the Moon and Beyond.

Introduction: Apollo Sample 73001/2 is a ~71cm long double drive tube consisting of an upper part (73002) and a lower part (73001) that contains regolith collected near Lara Crater at the Apollo 17 site, Station 3. The double drive tube is believed to have penetrated a lunar landslide deposit that was transported from the slope of the South Massif into the Taurus-Littrow Valley [1]. As part of the ANGSA (Apollo Next Generation Sample Analyses) initiative, preparing a preliminary examination (PE) catalog of 73001/2 is a crucial first step for the early identification of material types such as rock fragments and potential stratigraphy within the core. Many new curation and scientific tools such as X-ray computed tomography (XCT) [3], multi-spectral imaging [4], and gas extraction manifold with piercing tool [5-7], have been applied to the ANGSA core to benefit curation strategy, PE efforts, sample allocation to the planetary science community, and ultimately help to prepare for future sample return missions like Artemis. 73001/2 Preliminary Examination and Processing: Sample 73002 was successfully opened and extruded in Nov. 2019 and fully dissected at the end of 2021. Sample 73001 (Fig. 1) was successfully extruded in March 2022 after careful planning before opening the Core Sample Vacuum Container (CSVC) that was holding the drive tube of 73001. XCT, as part of PE, was used to scan the bottom and top part of the 73001 core tube within the CSVC prior to opening it to 1) facilitate non-destructive, rapid detection of any contamination potentials due to piercing of the CSVC during gas extraction [7]; and 2) to aid in the Artemis sample tool development and provide data on the knife edge seal of the CSVC. This knowledge will help us connect the mechanics of the implemented design (i.e., XCT data) to the performance of the seal (i.e., data on the gas samples will tell us how well the seal preserved the volatile record of lunar samples). Both type of information will feed forward into Artemis tool and storage strategies for future samples. Results and Lessons learned: The XCT data of the CSVC and core tube within showed that the bottom Teflon cap was not pierced during gas extraction (Fig. 1c) and thus, the sample integrity remained guaranteed during piercing and subsequent gas extraction. However, the XCT scan of the top of the core (Fig. 1b) revealed that the drive tube was overfilled with lunar soil and the tool that keeps the soil constrained within the drive tube was not fully deployed. These preliminary data allowed us to implement the necessary steps to prevent loss of sample integrity, including any potential stratigraphy shifts during extrusion. Processing Apollo core 73001/2, creating an informative PE catalog, and applying new and refined tools and technologies for sample analyses are invaluable activities that will assist in circumventing any potential pitfalls, aid in the characterization of samples, and help in the assessment of how well any lunar material has been collected and preserved in the past. This will aid in designing future sample collections and curation procedures and help to prepare for future human exploration and sampling missions such as Artemis. References: [1] Schmitt H. (2017) Icarus 298, 2-33. [3] Zeigler et al. (2021) LPSC 52nd, #2632; [4] Sun et al. (2021), LPSC 52nd, #1789; [5] Parai et al. (2021), LPSC 52nd #2665; [6] Schild et al. (2021) LPSC 52nd #1888; [7] McDonald (2022) ESL 2022.

ANGSA↗
NASA NTRS2011

Hayabusa Recovery, Curation and Preliminary Sample Analysis: Lessons Learned from Recent Sample Return Mission

I describe lessons learned from my participation on the Hayabusa Mission, which returned regolith grains from asteroid Itokawa in 2010 [1], comparing this with the recently returned Stardust Spacecraft, which sampled the Jupiter Family comet Wild 2. Spacecraft Recovery Operations: The mission Science and Curation teams must actively participate in planning, testing and implementing spacecraft recovery operations. The crash of the Genesis spacecraft underscored the importance of thinking through multiple contingency scenarios and practicing field recovery for these potential circumstances. Having the contingency supplies on-hand was critical, and at least one full year of planning for Stardust and Hayabusa recovery operations was necessary. Care must be taken to coordinate recovery operations with local organizations and inform relevant government bodies well in advance. Recovery plans for both Stardust and Hayabusa had to be adjusted for unexpectedly wet landing site conditions. Documentation of every step of spacecraft recovery and deintegration was necessary, and collection and analysis of launch and landing site soils was critical. We found the operation of the Woomera Text Range (South Australia) to be excellent in the case of Hayabusa, and in many respects this site is superior to the Utah Test and Training Range (used for Stardust) in the USA. Recovery operations for all recovered spacecraft suffered from the lack of a hermetic seal for the samples. Mission engineers should be pushed to provide hermetic seals for returned samples. Sample Curation Issues: More than two full years were required to prepare curation facilities for Stardust and Hayabusa. Despite this seemingly adequate lead time, major changes to curation procedures were required once the actual state of the returned samples became apparent. Sample databases must be fully implemented before sample return for Stardust we did not adequately think through all of the possible sub sampling and analytical activities before settling on a database design - Hayabusa has done a better job of this. Also, analysis teams must not be permitted to devise their own sample naming schemes. The sample handling and storage facilities for Hayabusa are the finest that exist, and we are now modifying Stardust curation to take advantage of the Hayabusa facilities. Remote storage of a sample subset is desirable. Preliminary Examination (PE) of Samples: There must be some determination of the state and quantity of the returned samples, to provide a necessary guide to persons requesting samples and oversight committees tasked with sample curation oversight. Hayabusa s sample PE, which is called HASPET, was designed so that late additions to the analysis protocols were possible, as new analytical techniques became available. A small but representative number of recovered grains are being subjected to in-depth characterization. The bulk of the recovered samples are being left untouched, to limit contamination. The HASPET plan takes maximum advantage of the unique strengths of sample return missions

Zolensky, Michael E.↗
NASA NTRS2022

Scientific Value of Including an Atmospheric Sample as Part of Mars Sample Return (MSR)

The Perseverance rover is meant to collect samples of the martian surface for eventual return to Earth. The headspace gas present over the solid samples within the sample tubes will be of significant scientific interest for what it reveals about the interactions of the solid samples with the trapped atmosphere and for what it will reveal about the martian atmosphere itself. However, establishing the composition of the martian atmosphere will require other dedicated samples. The headspace gas as the sole atmospheric sample is problematic for many reasons. The quantity of gas present within the sample tube volume is insufficient for many investigations, and there will be exchange between solid samples, headspace gas, and tube walls. Importantly, the sample tube materials and preparation were not designed for optimal Mars atmospheric gas collection and storage as they were not sent to Mars in a degassed evacuated state and have been exposed to both Earth's and Mars' atmospheres. Additionally, there is a risk of unconstrained seal leakage in transit back to Earth, which would allow fractionation of the sample (leak-out) and contamination (leak-in). The science return can be improved significantly (and, in some cases, dramatically) by adding one or more of several strategies listed here in increasing order of effectiveness and difficulty of implementation: (1) Having Perseverance collect a gas sample in an empty sample tube, (2) Collecting gas in a newly-designed, valved, sample-tube-sized vessel that is flown on either the Sample Fetch Rover (SFR) or the Sample Retrieval Lander (SRL), (3) Adding a larger (50-100 cc) dedicated gas sampling volume to the Orbiting Sample container (OS), (4) Adding a larger (50-100 cc) dedicated gas sampling volume to the OS that can be filled with compressed martian atmosphere.

Timothy D. Swindle↗
NASA NTRSDate not supplied

Mars Sample Receiving Facility Research and Development to Enable Preservation, Safe Containment, and Scientific Research of Martian Samples on Earth

NASA and ESA are working together to plan a joint campaign to potentially bring back the first Martian samples to Earth in the early 2030s. On the surface of Mars, the Mars 2020Perseverance Rover is selecting and packaging samples that could be returned to Earth for careful examination by an international team of scientists. In preparation for this historic sample return, advance planning is underway to design and build a Mars Sample Receiving Facility (SRF) in the mid-2020s. In 2022, a Mars Sample Receiving Facility Assessment Study(MSAS) will be conducted to further define construction modality and capability options for a facility in the conterminous United States. Since Mars Sample Return (MSR) is currently categorized as a planetary protection restricted Earth return, this new facility would feature biosafety level 4 (BSL-4)-like high containment to protect Earth’s biosphere from any potential hazard. In addition, the facility also requires integration of cleanroom technologies to mitigate against terrestrial contamination and preserve sample integrity for science investigations. The integration of both clean handling and high containment requires significant technology research and development (R&D) by the mid-2020s to support the definition and planning of a SRF before commencing the site specific design phase. The SRF project will need to solidify the inorganic, organic, and biological contamination control (CC) requirements for the facility. This could entail a translation of Mars 2020 mission CC requirements for geologic material to engineering requirements for surfaces and airborne molecular contamination inside isolators and cleanrooms. In tandem, the project will need to determine precision cleaning and sterilization approaches for cleanrooms, isolators, equipment, and tools. Initial material selections for the facility construction materials, cleanrooms, isolators, and BSL-4 suits/garments are an important activity. The recent construction of the OSIRIS-REx and Hayabusa2 curation cleanroom laboratories greatly benefited from early materials testing, before the design phase, to reduced organic outgassing and particulate shedding inside the laboratory. While the early biohazard investigations in the SRF may deem the samples safe to release to laboratories throughout the world, sterilization methods need to be defined to safely release Martian samples. One key aspect of enabling simultaneous sample containment and cleanliness is the concept of a Double-Walled Isolator (DWI) that ESA has been pursuing. Further R&D is needed about DWIs, sample handling, and instrumentation interfaces before beginning the SRF site specific design phase. A working isolator/DWI engineering model should be developed and fabricated. Isolator sizes, connections, pass-through antechambers, and configurations and basic interfaces with instruments and tools as well as the use of robotic, mechanical, and/or human manipulation need to be considered. Inert high purity gas supply (one-pass or recirculation) and other isolator utilities must be determined. Special accommodations for large instruments (e.g., XCT,SEM, etc.) need to be developed. Techniques for opening the sample tubes packaged by M2020and extracting the headspace gas while keeping samples pristine will be challenging, requiring additional R&D, and engagement of the M2020 project. In addition, careful micromanipulation for subdivision and packaging of samples will also need to be included. These combined R&D activities are important before commencing the SRF design phase to ensure safe biohazard containment, sample preservation, and science integrity for the samples that would be studied in the SRF and in laboratories around the world.

mars sample return↗
NASA NTRS2018

Maximum Sample Temperature for Mars Sample Return: A Historical Perspective

Since the first Mars Sample Return (MSR) report published by the Jet Propulsion Laboratory (JPL) in 1974 [1], a series of panels, reports, and white papers have recognized the importance of sample temperature and offered an informed sample maximum temperature (henceforth SMT) limit for returning martian samples to Earth. The Mars Sample Handling and Requirements Panel (MSHARP, 1999) stated that "[t]he main issue in sample preservation is temperature" [2]. More recently, the Mars Exploration Program Analysis Group (MEPAG)'s "Science Priorities for Mars Sample Return" report (2008), declared that "[s]ignificant loss, particularly to biological studies, occurs if samples reach +50C for three hours", whereby "scientific objectives related to life goals could be seriously compromised" [3]. By contrast, the Mars 2020 mission has adopted a SMT of +60C as spelled out in Beaty et al., 2016 [4]. Samples will be collected and then deposited on the surface in sealed tubes for possible retrieval and return to Earth. Beaty et al. [4] calculates that the samples will experience maximum temperatures of ~+30 to +60C, depending on latitude. At present, there is no mission requirement for the measurement/data logging of sample temperature during this period. We will explore the history of martian SMTs, as they have been recorded since 1974 [1], effectively representing input across multiple generations of Mars scientists. Ten separate publications present SMTs for MSR samples [1-10]. One report [10] is for a mission concept specifically designed to exclude life detection investigations, and recommended an SMT of 50C. Another did not specify a temperature, recommending "Mars ambient temperature" [5]. Of the remaining eight, SMTs are given as: -30C [1], -20C [3], 60C [4], -73 to 41C depending on sample type [6], -40C [7], -43 to 13C depending on type [2,8], and -33C [9]. If we restrict the temperatures to samples highlighted in the Mars 2020 mission goals, i.e. organics-bearing and sedimentary rocks, then the average SMT is -28+/-39C (n=8). Applying a Dixon's Q Test at P=0.05 (two-tailed), the 60C SMT [4] fails with Q=0.602 versus Qcrit=0.526. Excluding the outlier produces an average SMT of -40+/-17C (n=7). Therefore, the average SMT expressed by the Mars science community over the past 44 years (two generations) is a sample temperature no greater than -40C. The difference in chemical reaction rates between this average SMT and Beaty et al [4] can be estimated using the Arrhenius equation. Assuming a generic chemical reaction with an activation energy of 50 kJ/mol and a pre-exponential factor invariant with temperature, this reaction will proceed 2300x faster at 60C than at -40C. To illustrate the effects of the increased reaction rate, consider 10 ppb of alanine in a Mars 2020 cache, and assume that it becomes unmeasurable if it degrades to 1 ppb, as per the Mars 2020 Organic Contamination Panel contamination limits [11]. If we illustrate the effect with an arbitrary degradation rate such that the alanine will become undetectable in ten years at -40C, then the same 10 ppb alanine degrades beyond detectability in only 38 days at 60C. Further research is required to quantify expected analyte losses in the cached samples due to thermal processing.

Fries, Marc↗
NASA NTRS2024

Will MSR Samples Cached on the Martian Surface Experience Significantly Greater Thermal Degradation than Samples Retained in the Rover?

Since the first Mars Sample Return (MSR)-related report published by the Jet Propulsion Laboratory (JPL) in 1974, a series of panels, reports, and white papers have recognized the importance of sample temperature in meeting mission goals and defined a sample maximum temperature (henceforth SMT) limit. The Mars Sample Handling and Requirements Panel (MSHARP, 1999) flatly stated that “[t]he main issue in sample preservation is temperature”. The Mars Exploration Program Analysis Group (MEPAG)’s “Science Priorities for Mars Sample Return” report (2008), declared that “[s]ignificant loss, particularly to biological studies, occurs if samples reach +50°C for three hours ” whereby “scientific objectives related to life goals could be seriously compromised”. Overall, a total of seven panels, white papers, and conference reports adopted a SMT of -40±17°C to preserve samples sufficiently to confidently achieve success in studies of past or present Martian life (see more detail in [5]). In contrast, the Mars 2020 rover (M2020) mission adopted a SMT of +60°C for samples stored on the Martian surface and +50°C for samples retained inside the rover, as stated in a conference poster presented by Beaty et al., 2016. M2020 is currently collecting samples for MSR in tubes. Half of those tubes will be retained within the M2020 rover body (hereafter rover samples, or RS) and half will be deposited on the Martian surface (cached samples or CS), with a currently undetermined number of each collected up to ten years later for return to Earth. CS samples can be expected to experience significantly higher temperatures than RS samples based on their exposed location in sunlight. This work will explore differences in deleterious chemical reaction rates due to thermal environment of both tube types. The findings here should be debated openly and considered when deciding which samples to return to Earth.

M Fries↗
DOE OSTI2024

Apollo Next Generation Sample Analysis (ANGSA): an Apollo Participating Scientist Program to Prepare the Lunar Sample Community for Artemis

As a first step in preparing for the return of samples from the Moon by the Artemis Program, NASA initiated the Apollo Next Generation Sample Analysis Program (ANGSA). ANGSA was designed to function as a low-cost sample return mission and involved the curation and analysis of samples previously returned by the Apollo 17 mission that remained unopened or stored under unique conditions for 50 years. These samples include the lower portion of a double drive tube previously sealed on the lunar surface, the upper portion of that drive tube that had remained unopened, and a variety of Apollo 17 samples that had remained stored at -27 °C for approximately 50 years. ANGSA constitutes the first preliminary examination phase of a lunar “sample return mission” in over 50 years. It also mimics that same phase of an Artemis surface exploration mission, its design included placing samples within the context of local and regional geology through new orbital observations collected since Apollo and additional new “boots-on-the-ground” observations, data synthesis, and interpretations provided by Apollo 17 astronaut Harrison Schmitt. ANGSA used new curation techniques to prepare, document, and allocate these new lunar samples, developed new tools to open and extract gases from their containers, and applied new analytical instrumentation previously unavailable during the Apollo Program to reveal new information about these samples. Most of the 90 scientists, engineers, and curators involved in this mission were not alive during the Apollo Program, and it had been 30 years since the last Apollo core sample was processed in the Apollo curation facility at NASA JSC. There are many firsts associated with ANGSA that have direct relevance to Artemis. ANGSA is the first to open a core sample previously sealed on the surface of the Moon, the first to extract and analyze lunar gases collected in situ, the first to examine a core that penetrated a lunar landslide deposit, and the first to process pristine Apollo samples in a glovebox at -20 °C. All the ANGSA activities have helped to prepare the Artemis generation for what is to come. The timing of this program, the composition of the team, and the preservation of unopened Apollo samples facilitated this generational handoff from Apollo to Artemis that sets up Artemis and the lunar sample science community for additional successes.

79 ASTRONOMY AND ASTROPHYSICS↗
NASA NTRS2020

Analysis of Volatile Organic Compounds in the Apollo Next Generation Sample Analysis (ANGSA) 73002 Core Sample

Understanding the organic content of lunar regolith was an early priority upon the return of Apollo samples, with amino acids being of special interest because of their importance to life on Earth and their astrobiological relevance. Many initial studies focused on the detection of amino acids in these samples and attempts to determine the origin of those compounds. Although no consensus on the origin of the amino acids was reached in those early studies, more recent work determined that the detected amino acids originated from both terrestrial contamination and meteoritic or cometary in fall to the lunar surface. A majority of the amino acids in the Apollo samples studied originated from precursor molecules, either indigenous to the lunar samples or contaminants, that reacted during the water extraction and acid hydrolysis process for analysis in the laboratory, but the identities of the amino acid precursors still remain poorly understood. Such precursors could include hydrogen cyanide (HCN) and other volatile organic compounds such as amines, carboxylic acids, or aldehydes and ketones. The identities of these compounds, as well as the effects of years of curation on their abundances in lunar regolith samples stored at ambient temperature under nitrogen gas purge, are not clear. The specially curated samples available through the Apollo Next Generation Sample Analysis (ANGSA) program provide a unique opportunity to use state-of- the-art analytical techniques to examine previously unstudied lunar materials. The ANGSA samples include three types of samples: 1) samples stored frozen since <1 month after Earth arrival; 2) samples stored under helium; and 3) a double drive tube collected by Apollo 17 astronauts, with the bottom portion of the drive tube sealed under vacuum on the Moon and never opened. In contrast to the typically curated Apollo samples that have been kept for decades at room temperature under flowing nitrogen purge that may have significantly reduced the abundance of volatiles, the vacuum-sealed and frozen samples may have enhanced preservation of these volatiles. Our initial investigation examines amino acids and their potential volatile precursors, including hydrogen cyanide (HCN), aldehydes, ketones, amines, and mono-carboxylic acids, in a sample from the top portion of the Apollo 17 double drive tube. These results will aid in understanding the lunar abundances of these molecules and will also be compared to future analyses of other drive tube and frozen ANGSA samples.

Elsila, J. E.↗
NASA NTRS2004

Microgravity Testing of a Surface Sampling System for Sample Return from Small Solar System Bodies

The return of samples from solar system bodies is becoming an essential element of solar system exploration. The recent National Research Council Solar System Exploration Decadal Survey identified six sample return missions as high priority missions: South-Aitken Basin Sample Return, Comet Surface Sample Return, Comet Surface Sample Return-sample from selected surface sites, Asteroid Lander/Rover/Sample Return, Comet Nucleus Sample Return-cold samples from depth, and Mars Sample Return [1] and the NASA Roadmap also includes sample return missions [2] . Sample collection methods that have been flown on robotic spacecraft to date return subgram quantities, but many scientific issues (like bulk composition, particle size distributions, petrology, chronology) require tens to hundreds of grams of sample. Many complex sample collection devices have been proposed, however, small robotic missions require simplicity. We present here the results of experiments done with a simple but innovative collection system for sample return from small solar system bodies.

Franzen, M. A.↗
NASA NTRS2011

MEPAG Recommendations for a 2018 Mars Sample Return Caching Lander - Sample Types, Number, and Sizes

The return to Earth of geological and atmospheric samples from the surface of Mars is among the highest priority objectives of planetary science. The MEPAG Mars Sample Return (MSR) End-to-End International Science Analysis Group (MEPAG E2E-iSAG) was chartered to propose scientific objectives and priorities for returned sample science, and to map out the implications of these priorities, including for the proposed joint ESA-NASA 2018 mission that would be tasked with the crucial job of collecting and caching the samples. The E2E-iSAG identified four overarching scientific aims that relate to understanding: (A) the potential for life and its pre-biotic context, (B) the geologic processes that have affected the martian surface, (C) planetary evolution of Mars and its atmosphere, (D) potential for future human exploration. The types of samples deemed most likely to achieve the science objectives are, in priority order: (1A). Subaqueous or hydrothermal sediments (1B). Hydrothermally altered rocks or low temperature fluid-altered rocks (equal priority) (2). Unaltered igneous rocks (3). Regolith, including airfall dust (4). Present-day atmosphere and samples of sedimentary-igneous rocks containing ancient trapped atmosphere Collection of geologically well-characterized sample suites would add considerable value to interpretations of all collected rocks. To achieve this, the total number of rock samples should be about 30-40. In order to evaluate the size of individual samples required to meet the science objectives, the E2E-iSAG reviewed the analytical methods that would likely be applied to the returned samples by preliminary examination teams, for planetary protection (i.e., life detection, biohazard assessment) and, after distribution, by individual investigators. It was concluded that sample size should be sufficient to perform all high-priority analyses in triplicate. In keeping with long-established curatorial practice of extraterrestrial material, at least 40% by mass of each sample should be preserved to support future scientific investigations. Samples of 15-16 grams are considered optimal. The total mass of returned rocks, soils, blanks and standards should be approximately 500 grams. Atmospheric gas samples should be the equivalent of 50 cubic cm at 20 times Mars ambient atmospheric pressure.

Allen, Carlton C.↗
NASA NTRS2024

Volatiles in melt inclusions from lunar mare basalts: Bridging the gap in the H 2 O/Ce ratio between melt Inclusions in lunar pyroclastic sample 74220 and other mare samples

The H2O concentration and H 2 O/Ce ratio in olivine-hosted melt inclusions are high in lunar pyroclastic sample 74220 (H 2 O up to 1410 ppmw; H 2 O/Ce up to 77) but lower (H2O 10 to 430 ppmw; H 2 O/Ce 0.3 to 9.4) in all other lunar samples studied before this work. The difference in H 2 O concentration and in H 2 O/Ce ratio is absent for other volatile elements (F, S, and Cl) in melt inclusions in 74220 and other lunar samples. Because H 2 O (or H) is a critical volatile component with significant ramifications on the origin and evolution of the Moon, it is important to understand what causes such a large gap in H 2 O/Ce ratio between 74220 and other lunar samples. Two explanations have been advanced. One is that volcanic product in sample 74220 has the highest cooling rate and thus best preserved H 2 O in melt inclusions compared to melt inclusions in other samples. The other explanation is that sample 74220 comes from a localized heterogeneity enriched in some volatiles. To distinguish these two possibilities, here we present new data from two rapidly cooled lunar samples with glassy melt inclusions: olivine-hosted melt inclusions (OHMIs) in 79135 regolith breccia (unknown cooling rate but with glassy MIs similar in texture with those in 74220), and pyroxene-hosted melt inclusions (PHMIs) in 15597 pigeonite basalts (known high cooling rate, second only to 74220 and 15421). In addition, we also investigated new OHMIs in sample 74220. If the gap is due to the difference in cooling rates, samples with cooling rates between those of 74220 and other studied lunar samples should have preserved intermediate H2O concentrations and H 2 O/Ce ratios. Our results show that melt inclusions in 79135 and 15597 contain high H 2 O concentrations (up to 969 ppmw in 79135 and up to 793 ppmw in 15597) and high H 2 O/Ce ratios (up to 21 in 79135 and up to 13 in 15997), bridging the big gap in H 2 O/Ce ratio among 74220 and other lunar samples. Combined with literature data, we confirm that H 2 O/Ce ratios of different lunar samples are positively correlated to the cooling rates and independent of the type of mare basalts. We hence reinforce the interpretation that the lunar sample with the highest cooling rate best represents pre-eruptive volatiles in lunar basalts due to the least degassing. Based on Ce concentration in the primitive lunar mantle, we estimate that H 2 O concentration in the primitive lunar mantle (meaning bulk silicate Moon) is 121 ± 15 ppmw. Our new data also further constrain F/P, S/Dy and Cl/Ba ratios in lunar basalts and the lunar mantle. Estimated F, P, and S concentrations in the lunar primitive mantle are 4.4 ± 1.1 ppmw, 22 ± 8 ppmw, and 67 +67 −33 ppmw, respectively.

Xue Su↗
NASA NTRS2006

Small Body GN and C Research Report: G-SAMPLE - An In-Flight Dynamical Method for Identifying Sample Mass [External Release Version]

G-SAMPLE is an in-flight dynamical method for use by sample collection missions to identify the presence and quantity of collected sample material. The G-SAMPLE method implements a maximum-likelihood estimator to identify the collected sample mass, based on onboard force sensor measurements, thruster firings, and a dynamics model of the spacecraft. With G-SAMPLE, sample mass identification becomes a computation rather than an extra hardware requirement; the added cost of cameras or other sensors for sample mass detection is avoided. Realistic simulation examples are provided for a spacecraft configuration with a sample collection device mounted on the end of an extended boom. In one representative example, a 1000 gram sample mass is estimated to within 110 grams (95% confidence) under realistic assumptions of thruster profile error, spacecraft parameter uncertainty, and sensor noise. For convenience to future mission design, an overall sample-mass estimation error budget is developed to approximate the effect of model uncertainty, sensor noise, data rate, and thrust profile error on the expected estimate of collected sample mass.

in-flight sample-mass identification↗
NASA NTRS2009

Lunar Samples: Apollo Collection Tools, Curation Handling, Surveyor III and Soviet Luna Samples

The 6 Apollo missions that landed on the lunar surface returned 2196 samples comprised of 382 kg. The 58 samples weighing 21.5 kg collected on Apollo 11 expanded to 741 samples weighing 110.5 kg by the time of Apollo 17. The main goal on Apollo 11 was to obtain some material and return it safely to Earth. As we gained experience, the sampling tools and a more specific sampling strategy evolved. A summary of the sample types returned is shown in Table 1. By year 1989, some statistics on allocation by sample type were compiled [2]. The "scientific interest index" is based on the assumption that the more allocations per gram of sample, the higher the scientific interest. It is basically a reflection of the amount of diversity within a given sample type. Samples were also set aside for biohazard testing. The samples set aside and used for biohazard testing were represen-tative, as opposed to diverse. They tended to be larger and be comprised of less scientifically valuable mate-rial, such as dust and debris in the bottom of sample containers.

Allton, J.H.↗
NASA NTRS2013

Dynamic Acquisition and Retrieval Tool (DART) for Comet Sample Return : Session: 2.06.Robotic Mobility and Sample Acquisition Systems

The 2011 Decadal Survey for planetary science released by the National Research Council of the National Academies identified Comet Surface Sample Return (CSSR) as one of five high priority potential New Frontiers-class missions in the next decade. The main objectives of the research described in this publication are: develop a concept for an end-to-end system for collecting and storing a comet sample to be returned to Earth; design, fabricate and test a prototype Dynamic Acquisition and Retrieval Tool (DART) capable of collecting 500 cc sample in a canister and eject the canister with a predetermined speed; identify a set of simulants with physical properties at room temperature that suitably match the physical properties of the comet surface as it would be sampled. We propose the use of a dart that would be launched from the spacecraft to impact and penetrate the comet surface. After collecting the sample, the sample canister would be ejected at a speed greater than the comet's escape velocity and captured by the spacecraft, packaged into a return capsule and returned to Earth. The dart would be composed of an inner tube or sample canister, an outer tube, a decelerator, a means of capturing and retaining the sample, and a mechanism to eject the canister with the sample for later rendezvous with the spacecraft. One of the significant unknowns is the physical properties of the comet surface. Based on new findings from the recent Deep Impact comet encounter mission, we have limited our search of solutions for sampling materials to materials with 10 to 100 kPa shear strength in loose or consolidated form. As the possible range of values for the comet surface temperature is also significantly different than room temperature and testing at conditions other than the room temperature can become resource intensive, we sought sample simulants with physical properties at room temperature similar to the expected physical properties of the comet surface material. The chosen DART configuration, the efforts to identify a test simulant and the properties of these simulants, and the results of the preliminary testing will be described in this paper.

Dynamic Acquisition and Retrieval Tool (DART)↗
NASA NTRS2024

Sampling the Margin Unit of Jezero Crater, Mars for Future Mars Sample Return

Mars 2020 Perseverance rover is currently exploring Jezero crater, which contains an ancient lake-delta system with a high potential for past habitability. One of Perseverance’s primary science goals is to collect a set of scientifically return-worthy samples for return to Earth (Mars Sample Return; MSR). Between February 2021 and December 2023, Perseverance has sealed 23 tubes containing 20 rock cores, 2 regolith samples and one atmosphere sample. All rock and regolith samples are accompanied by a set of observations (Sample Threshold Observation Protocol, the STOP List) performed on abrasion patches or regolith near each sample collection site. These observations are documented in the Initial Reports and the Sample Dossier (https://pds-geosciences.wustl.edu/missions/mars2020/returned_sample_science.htm). Here we provide an overview of the samples collected during the Margin campaign. The Margin unit is situated interior and adjacent to the western crater rim and exhibits a strong carbonate signal from orbital reflectance spectroscopy. Stratigraphically the unit lies beneath the previously explored curvilinear and blocky units of the fan top and is therefore older than those units. Based on its position near the crater rim and the strong carbonate detections it has been proposed to be a shoreline deposit with possible lacustrine carbonates. Alternative hypotheses include pyroclastic, fluviolacustrine and aeolian deposits. Based on rover observations a lacustrine shoreline deposit seems most likely. The planning of the Margin campaign took place during the summer of 2023, and 3-5 samples were baselined to be collected. Exploration of the Margin unit began in September 2023 and so far, two samples have been collected: the Pelican Point core at the Hans Amundsen Memorial Workspace in the Mandu Wall region , and the Lefroy Bay core at Lake Newell in the Turquoise Bay region (Fig. 1). The associated abrasion patches are Amherst Point (Pelican Point) and Bills Bay (Lefroy Bay) . Mandu Wall is interpreted to be stratigraphically lower than Turquoise Bay based on topography.

Mars sample return↗