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Sample Return Container Opening Process Concept for Potential Mars Sample Return
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Sampling By the NASA Perserverance Rover for Mars Sample Return
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Mars Sample Return: Preparing for Biologically Sensitive Samples
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Pre-Mission Input Requirements to Enable Successful Sample Collection by a Remote Field/EVA Team
This paper is intended to evaluate the sample collection process with respect to sample characterization and decision making. In some cases, it may be sufficient to know whether a given outcrop or hand sample is the same as or different from previous sampling localities or samples. In other cases, it may be important to have more in-depth characterization of the sample, such as basic composition, mineralogy, and petrology, in order to effectively identify the best sample. Contextual field observations, in situ/handheld analysis, and backroom evaluation may all play a role in understanding field lithologies and their importance for return. For example, whether a rock is a breccia or a clast-laden impact melt may be difficult based on a single sample, but becomes clear as exploration of a field site puts it into context. The FINESSE (Field Investigations to Enable Solar System Science and Exploration) team is a new activity focused on a science and exploration field based research program aimed at generating strategic knowledge in preparation for the human and robotic exploration of the Moon, near-Earth asteroids (NEAs) and Phobos and Deimos. We used the FINESSE field excursion to the West Clearwater Lake Impact structure (WCIS) as an opportunity to test factors related to sampling decisions. In contract to other technology-driven NASA analog studies, The FINESSE WCIS activity is science-focused, and moreover, is sampling-focused, with the explicit intent to return the best samples for geochronology studies in the laboratory. This specific objective effectively reduces the number of variables in the goals of the field test and enables a more controlled investigation of the role of the crewmember in selecting samples. We formulated one hypothesis to test: that providing details regarding the analytical fate of the samples (e.g. geochronology, XRF/XRD, etc.) to the crew prior to their traverse will result in samples that are more likely to meet specific analytical objectives than samples collected in the absence of this premission information. We conducted three tests of this hypothesis. Our investigation was designed to document processes, tools and procedures for crew sampling of planetary targets. This is not meant to be a blind, controlled test of crew efficacy, but rather an effort to recognize the relevant variables that enter into sampling protocol and to develop recommendations for crew and backroom training in future endeavors. Methods: One of the primary FINESSE field deployment objectives was to collect impact melt rocks and impact melt-bearing breccias from a number of locations around the WCIS structure to enable high precision geochronology of the crater to be performed [1]. We conducted three tests at WCIS after two full days of team participation in field site activities, including using remote sensing data and geologic maps, hiking overland to become familiar with the terrain, and examining previously-collected samples from other islands. In addition, the team members shared their projects and techniques with the entire team. We chose our "crew members" as volunteers from the team, all of whom had had moderate training in geologic fieldwork and became familiar with the general field setting. The first two tests were short, focused tests of our hypothesis. Test A was to obtain hydrothermal vugs; Test B was to obtain impact melt and intrusive rock as well as the contact between the two to check for contact metamorphism and age differences. In both cases, the test director had prior knowledge of the site geology and had developed a study-specific objective for sampling prior to deployment. Prior to the field deployment, the crewmember was briefed on the sampling objective and the laboratory techniques that would be used on the samples. At the field sites (Fig. 2), the crewmember was given 30 minutes to survey a small section of outcrop (10-15 m) and acquire a suite of three samples. The crewmember talked through his process and the test director kept track of the timeline in verbal cues to the crewmember. At the conclusion, the team member conducting the scientific study appraised the samples and train of thought. Test C was a 90-minute EVA simulation using two crewmembers working out of line-of-sight in communication with a science backroom. The science objectives were determined by the science backroom team in advance using a Gigapan image of the outcrop (Fig. 1). The science team formulated hypotheses for the outcrop units and created sampling objectives for impact-melt lithologies; the science team turned these into a science plan, which they communicated to the crew in camp prior to crew deployment. As part of the science plan, the science team also discussed their sample needs in depth with the crewmembers, including laboratory methods, objectives, and samples sizes needed. During the deployment, the two crewmembers relayed real-time information to the science backroom by radio with no time delay. Both the crew and science team re-evaluated their hypotheses and science plans in real-time. Discussion: Upon evaluation, we found that the focused tests (Tests A and B) were successful in meeting their scientific objectives. The crewmember used their knowledge of how the samples were to be used in further study (technique, sample size, and scientific need) to focus on the sampling task. The crewmember was comfortable spending minimal time describing and mapping the outcrop. The crewmember used all available time to get a good sample. The larger test was unsuccessful in meeting the sampling objectives. When the crewmembers began describing the lithologies, it was quickly apparent that the lithologies were not as the backroom expected and had communicated to the crew. When the outcrop wasn't as expected, the crew members instinctively switched to field characterization mode, taking significant time to characterize and map the outcrop. One crew member admitted that he "kind of lost track" of the sampling strategy as he focused on the basic outcrop characterization. This is the logical first step in a field geology campaign, that a significant amount of time must be spent by the crew and backroom to understand the outcrop and its significance. Basic field characterization of an outcrop is a focused activity that takes significant time and training [2, 3]. Sampling of representational lithologies can be added to this activity for little cost [4]. However, we have shown that identification of unusual or specific samples for laboratory study also takes significant time and knowledge. We suggest that sampling of this type be considered a separate activity from field characterization, and that crewmembers be trained in sampling needs for different kinds of studies (representative lithologies vs. specialized samples) to acquire a mindset for sampling similar to field mapping. Sampling activities should be given a significant amount of specifically allocated time in scheduling EVA activities; and in the better case, that sampling be done as a second activity to a previously studied outcrop where both crew and backroom are comfortable with its context and characteristics. Our hypothesis posited that crewmember knowledge of how the samples would be used upon return would aid them in choosing relevant samples. Our testing bore this hypothesis out to some extent. We therefore recommend that crewmember training should include exposure to the laboratory techniques and analyses that will be used on the samples to foster this knowledge. There is also the potential for increasing crewmember contextual knowledge real-time in the field through the introduction of in situ geochemical technologies such as field portable XRF. The presence of field portable geochemical technology could enable the astronauts to interrogate the samples for K abundance real-time, ensuring they could collect valuable and dateable samples [5]. Though simulations such as these can teach us a fair bit about decision making processes and timeline building, one EVA participant noted that when he wasn't collecting "real" samples, he wasn't at his best. This effect suggests that higher-fidelity studies involving truly remote participants conducting actual scientific studies merit further attention to capture lessons for application to future crew situations.
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).
Assessing Risk Due to Small Sample Size in Probability of Detection Analysis Using Tolerance Intervals
Small sample size (e.g.6-30) poses risk in results of probability of detection (POD) analysis using tolerance intervals. This method is also called as the limited sample or LS POD. The analysis is performed either during NDE procedure qualification or for assessment of reliability of an NDE procedure. The risk is primarily due to sampling error. Smaller samples are not likely to be random to the population or representative of the population. The small samples are likely to be biased. Biased samples have smaller standard deviation compared to the population. POD analysis with small biased sample can lead to overestimation of POD. Many sampling schemes are available in statistics to mitigate sampling risk. Primary objective of POD analysis is to determine a decision threshold from signal response measurements of a sample such that it is less than or equal to population decision threshold for 90% POD. Sampling error implies that this NDE reliability condition is violated. One of sampling types is called a representative sample. Representative samples reduce variance in POD estimates but also reduce magnitude of the error. Sampling sensitivity analysis for some sampling types is performed here using repetitive random sampling or Monte Carlo method. Six sampling types are considered for comparison. Some of the sampling types are similar to drawing a representative sample. LS POD model assumes random sampling. Therefore, random sampling is used as a basis for comparison with each sampling type. The sampling types used in the analysis are, A. Nominal and worst-case sampling, B. Worst-case sampling, C. Nominal case sampling, D. Random sampling, E. Random target, and sub-target sampling. F. Nominal target and sub-target sampling. Results of Monte Carlo simulation indicate that type F sampling can mitigate sampling risk and is also more practical to implement. Type A sampling may also mitigate the sampling risk, but it may be less practical to implement.
The Importance of Contamination Knowledge - Insights into Mars Sample Return
The Astromaterials Acquisition and Curation Office at NASA Johnson Space Center (JSC), in Houston, TX (henceforth Curation Office) manages the curation of all past, present, and future extraterrestrial samples returned by NASA missions and shared collections from international partners, preserving their integrity for future scientific study while providing the samples to the international community in a fair and unbiased way. The Curation Office also curates all reference and witness materials for each mission (e.g., flight and non-flight hardware coupons; lubricants; non-flight, flight-like, and flown witness plates). These reference and witness materials provide the scientific community with the fundamental ability to reconstruct the contamination/alteration history of the sample collection through the course of the mission, with the overall goal of strengthening the scientific conclusions drawn from the study of returned materials. The information gained from characterizing the physical, biological, inorganic, and organic chemical properties of reference and witness materials is defined as the Contamination Knowledge (CK) of the sample collection. Unlike the data collected for Contamination Control (CC) and Planetary Protection (PP), CK is exclusively concerned with preserving reference and witness materials for study by future scientists upon sample return. Although CC and PP data collected for sample integrity and forward contamination purposes can be complementary to CK, they are two separate data sets with distinct objectives. A robust collection of samples for CK is necessary to allow the extraterrestrial material in a returned sample to be distinguished from terrestrial contamination. Traditionally CK is utilized by sample scientists in order to accomplish the mission’s scientific objectives, however this information can also be utilized by the Office of Planetary Protection to help evaluate the presence of any back contamination. Mars 2020, the first phase of a potential multipart Mars Sample Return (MSR) campaign, is expected to contribute to NASA’s Mars Exploration Program Science Goals by filling in knowledge gaps concerning: 1) the existence of past or present life on Mars, 2) the past and present climate of Mars, 3) the geology of Mars, and 4) hazards associated with human exploration of Mars. Although there is debate concerning which samples will best answer these questions, the necessity for proper sample blanks is well-understood. The CC and PP requirements, driven by the restricted Class V mission designation, are the most stringent of any sample return mission in recent history. The extremely low levels of allowable terrestrial contamination on the spacecraft and rover can complicate these analyses given the detection limits of current analytical instrumentation, especially in the case of biological contamination. By collecting and curating unanalyzed samples specifically for CK, future sample scientists will not be relegated to: 1) relying on data collected using possibly obsolete tools and techniques for return sample blanks, or 2) using remnants of extracted and/or cultured samples from ATLO (Assembly, Test, and Launch Operations), which could be incompatible with the desired experimental endpoints or state-of-the-art techniques available at the time of sample return.The addition of biological experimental endpoints to a sample return campaign’s objectives broadens the requisite range in preservation environments (e.g. inert ultra-pure nitrogen gaseous environment at 18 degrees Centigrade versus less than or equal to minus 80 degrees Centigrade) and types of CK samples. As a result, the Curation Office will also curate the following CK samples at less than or equal to minus 80 degrees Centigrade for the Mars 2020 mission: 1) unanalyzed swabs and wipes in sterile containers, 2) all recirculation filters from the clean rooms used for sample and caching subsystem assembly and all filters from the laminar flow benches used to assemble sample intimate hardware, and 3) witness plates collecting airborne contamination within the assembly clean rooms. It has been Curation Office policy since the Apollo missions to preserve as many pristine samples as possible for future scientific research. Although CK is required to be collected for all stages of the MSR campaign, the CK for the Mars 2020 mission is the most critical for understanding contamination in the returned samples given the intimacy between the Martian samples and the Mars 2020 flight hardware. This presentation highlights the importance of CK for sample return missions as well as the traditional and novel types of CK samples required for a successful MSR campaign.
The Effect of Temperature on the Preservation of Volatile-Rich Lunar Samples
Introduction. The Moon’s south pole is a high-priority target for human exploration and scientific study. This interest is, in part, due to the presence of Permanently Shadowed Regions (PSRs), which could contain high concentrations of unique volatiles at cryogenic temperatures [1]. Returned samples from PSRs may include a unique combination of rocks, regolith, and volatile species, providing unprecedented insights into the history of the Solar System and the potential for resource utilization on the Moon. However, because PSR samples are cryogenic up-on collection, lunar polar sample return will eventually require cold stowage for the journey from the Moon to Earth. Without cold stowage, PSR sample return will likely result in phase changes and chemical reactions within the volatile component of the sample, which would negatively impact the resulting scientific studies of those samples. This abstract summarizes the initial results from an ongoing characterization of analog PSR samples at a range of temperatures, with the goal of defining the temperatures needed for a flight cold stowage freezer. Background. Based on remote sensing observations of the Moon [2], south polar PSRs range in temperature from ~120K for small and/or shallow PSRs to ~20K at the most extreme locations in large, deep PSRs. A range of volatiles have been hypothesized to exist at the surface or subsurface of the lunar poles [3-5 and others]. This hypothesis was verified when the LCROSS mission impacted the <50-K PSR in the crater Cabeus, detecting a range of volatiles from water to low condensation temperature species such as H2S and methane [6]. Species such as H2S and ammonia (also detected by LCROSS) are also highly reactive, and increase the likelihood of chemical reactions at elevated (non-cryogenic) temperatures. At the Johnson Space Center’s Planetary Exploration and Astromaterials Research Laboratory (JSC-PEARL), we have developed a volatile-bearing lunar simulant that incorporates several of the species detected by LCROSS [Table 1] mixed cryogenically with the USGS Lunar Highlands Type (LHT) regolith simulant. The new volatile-regolith simulant will be used to assess the degree of sample alteration at room temperature, -20°C, -80°C, and -196°C (liquid nitro-gen), over a two-week period. Room temperature samples represent those likely to be returned during initial missions without cold stowage, -20°C provides an analog to Apollo cold curated samples, -80°C is the temperature of multiple flight payload freezers (e.g., MELFI), and -196°C is analogous to lunar PSRs. Two weeks is an approximation of the time between sample collection and Earth return for initial Artemis missions. Over this period of time, sample head-space gases will be analyzed using a Universal Gas Analyzer (UGA, a type of mass spectrometer) coupled with a Baratron pressure sensor. After testing, the regolith component of the simulant will be purged of volatiles and preserved for future electron beam and/or FTIR analysis. Experimental Procedure. Volatile-regolith simulants will be produced as an initial homogenous batch; this batch will then be distributed into aliquots (gas chromatography/GC vials or cryo vials), ensuring that each sample has the same starting composition and conditions [Fig. 1]. In addition to the “full” simulant shown in Table 1, less complex simulant compositions will be used as baseline and control samples [Table 2]. Aliquots will be produced in triplicate for each simulant composition, storage temperature, and date of sampling. Headspace gases in all Day 0 samples will be analyzed by the UGA immediately. Cold storage samples for future analytical days will be placed in freezers appropriate to their target temperatures (-20°C, -80°C, -196°C). For ambient-temperature samples, regolith and regolith-water samples will be stored in a fume hood, while the full simulant will be stored in a sealed Parr vessel for safety; no other simulants (RWCM/ RWCM+) will be stored at ambient temperature for this test. Samples will be analyzed by UGA in this manner on each Analysis Day outlined in Table 2. Analytical Data. The UGA measures the partial pressures in a single sample aliquot over a set mass range of 0-105 atomic mass units (AMU) [Figure 2]; this set range was selected to slightly exceed the mass of the highest-mass expected reaction product (H2SO4). The Baratron complements the UGA by measuring the total pressure in the headspace of a sample vial. Coupled together, the quantitative abundances of gases will be monitored throughout the test. UGA analyses of the triplicate samples for each storage temperature, day, and simulant composition will be averaged, and standard deviations for each will be calculated. The compositions of starting species (shown in Table 1) will be characterized as a function of time, and the presence of any new compounds (reaction products) will be monitored as well. Total pressures will be recorded for each sample analysis, and any samples that show signs of leakage (e.g., a significant reduction in pressure or simulant volatiles) will be discarded. Anticipated Results. Testing is planned to begin in January 2022. The resulting data will allow compositional and phase changes in the volatile component of the simulants to be determined. Both the reduction in initial compounds and the addition of reaction products are expected to be observed. In addition, the relative efficacy of the different temperatures at pre-serving the initial composition of the simulants will be quantified. Finally, the regolith component of each sample will be argon-purged and stored in a controlled environment for future laboratory analysis. Compositional and morphological changes in the regolith are expected for samples above 0°C. This test will be repeated three times over the course of 2022. Understanding the effect of temperature on both the volatile and regolith components of analog lunar materials will allow requirements for a cold stowage freezer to be developed. The implementation of cold stowage for lunar polar missions will maximize the preservation of returned samples, enabling ground-breaking lunar and Solar System volatiles science for decades to come.
EVA Swab Kit: Tools and Techniques for Collecting Aseptic Samples from Crewed Space Missions
Introduction: When we send humans to search for life on other planets, we'll need to know what we brought with us versus what may already be there. To ensure our crewed spacecraft meet planetary protection requirements—and to protect our science from human contamination—we'll need to assess and verify whether micro-organisms may be leaking/venting from our spacesuits. This requires collecting samples under Extravehicular Activity (EVA) conditions. Detailed, systematic research on forward contamination from robotic spacecraft has been steadily progressing since the Viking missions, but systematic studies of contamination from space suits has not been conducted in many years. The modern EMU (Extravehicular Mobility Unit) suit used by NASA is designed to leak at rates as high as 100 cc/min. Before humans land on Mars there is a critical need to understand the types and quantities of microbes that could be introduced via space suits. The Human Forward Contamination Assessment team at NASA’s Johnson Space Center (JSC) has developed a prototype EVA swab tool [1,2,3,4] designed for use in space to sample cleaned and uncleaned space suits to determine the present day microbial load and eventually the rate of leakage. The ability to assess microbial leakage early in advanced space suit and life support system design cycles will help avoid costly hardware redesign later. Test Objectives: The primary objective of EMU testing was to characterize the type of micro-organisms typically found on or near selected suit pressure joints under suit differential pressure conditions. Most human-borne microbes can fit through a 0.5 to 1.0 µm gap. Knowing which joints are more likely to leak will inform hardware design decisions. Knowing which types of micro-organisms may leak from EVA suits provides a basis for subsequent studies to characterize the viability of those organisms under destination conditions, as well as how far they might spread through natural or human-influenced processes. That data, in turn, will inform exploration mission operations and hardware design. The secondary objective of testing was to evaluate the interface between a fully suited test subject and the EVA swab tool at vacuum. Bulky EVA suits can restrict movement and limit visibility through the helmet visor. Fully suited testing is important for identifying tool design issues prior to flight. At exploration destinations, such as Mars, suited crew may be required to periodically sample their suits as part of an environmental monitoring protocol. Suit Microbial Sampling Results: This report details results of microbial swabs collected from current flight suit configurations worn by crew members assigned to upcoming ISS expedition missions as well as swabs collected from prototype suits intended for use on the Orion spacecraft. These tests were intended to characterize the types of contaminants found on flight suits under current, typical handling conditions. No attempt was made to change suit handling procedures, provide additional sterilization, or to limit typical potential contaminant sources. Using culture based techniques, we cultivated 235 CFU (colony forming units) comprised of 26 bacterial species and one fungal species on the outside of the suits. The fungal species and 14 of the bacterial species were unique to the suit surfaces and were not detected in any of the background samples collected within the chambers. We sequenced 755,434 ribosomal fragments on all of the suit surfaces from swab samples. 557,016 of these sequences represent DNA that survived at least 4 hours at vacuum. These sequences formed 2,464 OTU's (Operational Taxonomic Units, 97% similarity) showing low diversity in the samples. The most abundant sequences that survived vacuum belong to the genera Staphyloccocus, Ralstona, Bacillus and Rhodobacter all of which are common to the human microbiome. [5] See Danko et al., (2021) for more complete details of these first analyses. Further analysis of EVA suit materials with respect to the efficacy of various cleaning protocols and engineered containment solutions is planned to inform suit design for NASA’s Artemis Moon to Mars program crew testing. Swab Tool Function Results: The kit was demonstrated for fit and function in suited subject vacuum tests to determine how well the tool worked as an aseptic microbial sampling device as well as to identify any design elements that could be upgraded for EVA task specific improvement. It was found that sample acquisition efficacy could be enhanced by redesign of the sample canister to end-effector interface. Several modifications of the sample caddy assemblies to optimize EVA safety and functionality were also identified. Consequently, fabrication of the redesigned sample canister to end-effector assembly interfaces and and the sample caddy assemblies are required. Fabrication of sixteen flight sample canister assemblies (8 per each of two EVA Swab Kits) and two sample caddy assemblies are in process to be followed by hardware testing and certification to produce two flight-certified EVA Swab Kits for transport to ISS no earlier than summer of 2022. Sampling Strategy: The International Space Station is an ideal testbed for systematic studies of contamination from crewed vehicles since it has been continuously occupied for 20 years and exposed to non-terrestrial conditions. We will sample the exterior of the ISS during EVA using a purpose-built swab tool capable of maintaining sterility while undergoing temperature changes from -151 to +121°C under hard vacuum. Prior to each EVA, the project team will work with ISS mission managers to identify precise sampling locations, which will vary by EVA based on the translation paths and worksites scheduled for that particular EVA. Ideally, translation path handrails and areas near ECLSS (Environmental Control and Life Support System) external vent openings on a spacecraft would be assessed. There are currently more than a dozen ECLSS external vents on the ISS. Some are connected to systems that vent waste products, while others are intended to equalize cabin pressure. As EVA opportunity allows, microbial samples from any of these external vents would provide a valuable data point, though some will be more useful than others. Four criteria have been identified to help prioritize sampling sites near vents: • EVA Accessibility: To minimize cost, it is desired to piggy-back onto a planned EVA. Therefore, the sampling location must be readily accessible by an EVA crew • Type of Vented Products: Vent products that have been in direct contact with crew, such as cabin air, are more likely to contain microorganisms than vent products associated with isolated systems, such as experiment module combustion products. • Mass of Vented Products: Higher-flow vents are more likely to contain detectible levels of microbial contaminants than lower-flow vents. • Local Environment: Sample locations with relatively benign local conditions, such as warm surfaces shielded from direct ultraviolet (UV) radiation exposure, may be more likely to support microbial growth than locations with harsher local environmental conditions. Because EVA accessibility is the most important criteria, the proposal team worked with an astronaut and flight controllers using the Dynamic Onboard Ubiquitous Graphics (DOUG) tool. The DOUG virtual environment allows an operator to “fly” around the current ISS vehicle configuration to assess EVA translation paths, attach points, and keep-out zones. While analysis on station or rapid return to Earth would be preferable, samples collected from the exterior of the ISS have already been exposed to temperature variations between -157 and +121 °C as well as hard vacuum. Therefore, they should be fairly stable and robust. We hypothesize that samples collected from the ISS exterior could be stored for up to 6 months at -80°C without degradation. Sample canisters will be returned to Earth while frozen at -80°C for analysis, and sterilized canisters can be re-flown back to ISS to support additional sampling opportunities Relevance to NASA Exploration Objectives: These data will allow us to identify new or improved methods, technologies, and procedures for spacecraft sterilization and leakage mitigation to minimize the amount of contamination introduced to the environment by human explorers. This work is funded by NASA research grant: NNH18ZDA001N-PPR References: [1] Bell, M.S. et al. (2015) LPS XLVI, Abst. #1832 [2] Rucker et al. (2018) 42nd COSPAR (PPP.3) [3] Bell, M.S. et al. (2019) Mars Extant Life Conference, Abst. #5096.[4] Bell, M.S. et al., (2020) 43rd COSPAR (BO.2).[5] Danko D, et.al.,(2021)Front.Microbiol.12:608478.
The Collection, Usage, and Preliminary Examination of the Apollo Sample Suite: Lessons for Artemis
Apollo Sample Collection and Usage: From 1969 to 1972 there were six Apollo missions to the surface of the Moon during which the astronauts collected 382 kg of rock and regolith (~2200 samples). The samples collected fall into these general categories: rocks (~66% by mass), rake samples (~4%), bulk regolith (~24%), and specialty regolith (deep drill cores, drive tubes, sealed bulk regolith) samples (~6%). In each category there are a variety of different subtypes available for study, e.g., among the bulk regolith samples there are also skim, trench, and (partially) shaded regolith samples each sampling unique types or depths of regolith. This variety of subsamples has enabled a multitude of different studies over the past 55 years (>3400 individual requests). We are still averaging ~50 unique requests and have allocated >500 individual Apollo samples annually for the past 10 years (2020 excepted). Looking at the 4,675 non-ANGSA (Apollo Next Generation Sample Analysis) samples allocated over the past 10 years, the proportions of allocated samples do not precisely align with the abundance (by mass) of those samples withing the collection: Rock (69.4 %); Rake (10.8 %); Bulk Regolith (15.5 %); Drive Tube (3.3 %); Core/Specialty (1.0 %). Apollo Preliminary Examination (PE): The PE process differs significantly for the various sample types enumerated above; we focus on regolith and rock samples here. During the Apollo mission era, the PE process evolved over the course of the missions; below is what was done for the Apollo 17 mission. For regolith samples, the PE process was: (1) documented bags containing regolith are opened, photographed, and described; (2) large rocks are removed and treated separately; (3) 25% to 33% of the bulk soil is scooped out, weighed, and stored in reserve; (4) the remaining sample is sieved to produce the size fractions <1, 1- 2, 2-4, and 4-10 mm, all of which are weighed. For rock samples, the process is: (1) removing rocks from the container(s) it came back from the Moon in; (2) rematching any materials that spalled off the rock to their original location; (3) numbering, weighing, and basic photographic documentation; (4) dusting with a gentle N2 gas jet; (5) Orthogonal photography; (6) detailed description of the textures and features of the rock; (7) rock modelling and measurement; (8) stereophotography; (9) determination of the orientation of the rock on the lunar surface. Drive tubes and deep drill cores were not characterized during PE beyond an initial weight and a sketch of the interior tube materials derived from 2D medical X-ray images. Catalogs: The ongoing utility of the Apollo samples is enabled by the robust cataloguing process for the samples [3-5], which allows the scientific community to accurately request samples uniquely suited to their proposed studies. A common misconception, however, is the amount of detail that goes into the initial catalog (e.g., [6]) for a collection from the preliminary examination (PE) period, versus what goes into the catalogs that come later in the life cycle of the samples from that mission (e.g., [7]). The only required data for a PE catalog is a weight, a basic photograph, and a description of the nature of the sample. Artemis PE: Over the past few years, the ongoing ANGSA project studied previously unopened Apollo 17 double drive tube samples 73001/2 [1], and a PE of the drive tubes was done. The PE took the existing core dissection process (developed during PE of Apollo cores in the 1970s, 1980s), and modernized it [7]. The main lesson from the ANGSA PE relative to future missions was that the physical work done during PE of lunar samples has not changed much over the past 5 decades. The use of “modern” technology during PE (e.g., XCT; multispectral analyses) resulted in an enhanced initial understanding of the 73001 and 73002 drive tubes, but greatly increased the time required. The lessons learned from recent astromaterial PEs (e.g., ANGSA and OREx) are important to consider when planning for Artemis, but the unique nature of the Artemis Campaign means many lessons learned from these mission will not be applicable. Given the time constraints (6 months) and likely number of samples that will be returned by Artemis (>200), the Artemis PE catalog will necessarily look much more like [4] than [6].
OSIRIS-REx Curation: The First Year with Bennu Samples on Earth
The OSIRIS-REx (Origins, Spectral Interpretation, Resource Identification, and Security – Regolith Explorer) sample return capsule landed on the Utah Test and Training Range (UTTR) on September 24, 2023. Preparations for the curation of the sample from asteroid Bennu inside of this capsule spanned more than a decade. On the morning of landing, the sample return capsule was brought to a temporary cleanroom at UTTR for initial de-integration and connection of the sample canister to a nitrogen gas purge to protect the sample from modification by the terrestrial atmosphere. In the week following landing, the sample canister was flown to Houston while on nitrogen purge, transferred to a nitrogen atmosphere glovebox at NASA Johnson Space Center in which the canister lid was removed revealing small amounts of sample on the inside of the canister lid and avionics deck, some of this sample was allocated rapidly to the mission sample analysis team as “quick look” samples. Next, the Touch-and-Go sample acquisition mechanism (TAGSAM) head was disassembled inside of a specially designed glovebox. A challenge arose during one of the last stages of disassembly when two fasteners resisted being loosened. The curation team was able to remove 70.3 grams of asteroid sample from the TAGSAM head with those fasteners in-place and began initial sample processing which supported long-term curation of hermetically sealed and frozen samples, transfer of some samples to remote storage, and allocation of aggregate samples to the mission sample analysis team. Meanwhile, curation engineers developed a tool to remove the stubborn fasteners without contaminating the remaining sample, enabling the remaining bulk sample to be transferred to long-term storage trays in January 2024. With this second part of the bulk sample, the returned bulk asteroid sample reached 121.6 grams. During disassembly and prior to sealing the bulk sample trays into long-term storage containers, archival photographs were collected. Select particles are gradually being XCT scanned while inside of containers that hold a nitrogen atmosphere. The initial OSIRIS-REx sample catalog was released in spring 2024 with an update in fall 2024. The curation team will be busy working to allocate samples to scientists around the world for the foreseeable future.
The Genesis Non-flight Implant Sample Archive
Introduction: For the past 20 years the Genesis science community has been analyzing solar wind captured in sample collectors now curated at Johnson Space Center (JSC). Non-flown flight like collector materials (non-flight) considered reference material was always allocated by the JSC Genesis team for testing experimental procedures. However, to expedite Genesis science, distribution of non-flown reference materials were also provided by, D. S. Burnett (Genesis PI, Caltech) and A. J. G. Jurewicz (ASU) who were funded to aid all Genesis PIs by providing engineering test materials archived at Caltech pre-flight as well as ion implants into these materials [1]. Implanted materials (non-flight reference, flight-like semiconductor materials, and NIST SRM glass) received from the Caltech collection during a pilot project are being used to develop an accession procedure for the purpose of making these materials available to researchers in the future. These implant samples are important because they can be utilized as measurement standards [2]. This is a work in progress and this work reports progress in documentation and imaging. The pilot program received 63 implanted reference materials with known implanted ions. Genesis Non-Flight Database: The existing non-flight material database was modified to allow for the description of implant sessions and to allow correlation of the implant information to individual specimens. An implant session has three main components: a known ion, a known dose (ion/cm2), and a known energy (keV). Procedure: Laboratory Procedure. Upon receiving non-flight analytical standards (independently calibrated implants), or implant samples (nominally calibrated implants), they will be imaged in their current containers to capture any information written before being brought into the Genesis Sample Laboratory. Documentation is provided by the donor and used for correlating the data between the implant sessions and implant samples. This information is not verified by Genesis Curation. The microscope used to image samples in the laboratory has an automated stage with a stainless-steel plate to hold samples and a camera that utilizes the software Surveyor to take photomosaic images of the implant samples. The camera attached to the microscope is a QICAM High Performance IEEE 1394 FireWire Digital CCD Camera. This setup, shown in Fig. 1, allows for photomosaics of small-scale samples with a 10x objective or 25x objective. Examples of images taken with this microscope setup are shown in Fig.2 and Fig. 3. After imaging, samples get stored in a clean fluoroware container or polypropylene vial depending on sample size for long term storage. Database Procedure. The Genesis Non-Flight Database currently allows for the addition of implant sessions. The required fields for adding an implant session are the implant session ion, the implant session dose, and the implant session energy. There are also fields for the date and vendor of the sessions as well as a field for if the session was calibrated or not. Once an implant session has been inserted into the database, additional documentation from the session can be attached. The database will automatically assign an Implant Session Number. After inserting an implant session, the implanted samples can be inserted. The fields required for an implant sample are the material of the sample and the size of the sample. The Generic name for the implant sample with be automatically generated by the database once it has been inserted. Implant sample numbers begin with 3X to distinguish from flown Genesis sample numbers. There are also fields for processors to add the location (room, cabinet, tray) and container type (fluoroware, polypropylene vial). Once an implant session and an associated sample(s) have been inserted into the database the sample can be then tied to all associated implant sessions. An implant sample can be tied to multiple implant sessions. Future work: For curation, future work consists of creating an online catalogue for implant samples as well as updating the database with more samples as we receive them. For the scientific community these implant samples have many potential uses. For Genesis research, they are directly applicable for testing and, in some cases, as analytical standards. For non-Genesis research, implants (especially calibrated implants) could be used for calibrating other, unique planetary materials [1].
Initial analysis of “stone” size Ryugu samples: current status
As a part of the initial analysis of the Ryugu samples, we perform a variety of analyses of millimeter-sized "stones". Our goals are to elucidate the entire formation process of C-type asteroid Ryugu from the viewpoint of petrology and mineralogy ande obtain necessary information by sample analysis, and then simulate the formation of Ryugu based on the evidencef obtained rom sample analysis. Eighteen stones (8 from Room A and 10 from Room C) were received from the ISAS curation facility on June 1, 2021, and brought into a fully nitrogen-displaced glove box at Tohoku University. At the same time, we also received the powder samples from Room A and Room C. To completely block the atmosphere from leaking into the container, all samples were put in the sample transport containers prepared by ISAS, transferred from the main chamber to the glovebox at ISAS, and then all containers were completely sealed in plastic bags with moisture and oxygen absorbers. No moisture or oxygen was detected when the bags were opened in the glove box at Tohoku University, so it was confirmed that there was no exposure to the atmosphere during transport. To date, a number of analyses have been carried out successfully and almost on schedule. The analysis started with the measurement of reflectance spectra, which are sensitive to atmospheric oxidation, hydroxylation, and adsorbed water. The visible, near-infrared, and mid-infrared reflectance spectra were measured while the samples were kept airtight. The spectra of powder samples and stone samples (as aggregates and as single stone) were successfully obtained. A major feature of the stone team's analysis is the use of synchrotron radiation facilities around the world. Since this analysis is non-destructive, stone samples whose reflectance spectra were measured were sent to KEK, SPring-8, ESRF (France), SOLEIL (France), DESY (Germany), and APS (USA). Using these synchrotron radiation facilities, high spatial resolution and sensitivity XRD, STXM, XANES, CT [1], IR-CT, FT-IR [2, 3], XRF, and Mössbauer analyses were performed. Most of the analyses were carried out under air-tight conditions on the stone samples and the particulates separated from the stone samples. These analyses allowed us to determine the three-dimensional distribution of minerals and elements, redox state, density and porosity of the stone samples. Furthermore, as a characteristic analysis of the stone team, light elemental analysis using negative Muon was performed at the MLF facility of J-PARC with an exceptionally long allocation of machine time. This is the only non-destructive method to measure the concentration of light elements in the whole (not the surface) of stone samples. Because the characteristic X-rays produced by muon irradiation are much higher in energy than the fluorescent X-rays produced by X-ray irradiation, there is little effect of self-absorption by the sample, and therefore, the concentration of light elements such as carbon, oxygen, and Na in the entire "stone" sample can be determined. Some stone samples are currently being measured for heat and strength physical properties in order to understand the physical properties of asteroid Ryugu. The data obtained from these measurements are useful for interpreting the remote-sensing data data taken from the surface layer of the asteroid Ryugu [4-7]. It is also important for understanding the behavior of the Ryugu material during impact events. The surfaces of many stone samples were observed by electron microscopy and other techniques, especially on natural “flat” surfaces formed on 5 stomes. As a result, characteristric mineral aggregates formed by the reactions with water and characteiristic impact features were observed on some of the samples. Based on the observations of surfaces and the synchrotron measurements of the whole stones, important objects such as characteristic structures and specific crystal aggregates for understanding the formation history of the asteroid were identified, and these parts were separated from the stone samples using an Xe beam (pFIB) and analyzed by various methods including transmission electron microscopy and synchrotron radiation analysis. Many stone samples, from which important objects have been separated, are embedded in epoxy resin and cut to produce many polished sections. Electron microscopy and spectroscopic measurements of the polished surfaces are being carried out to reveal the detailed mineralogical properties and elemental distribution inside the stone samples. In the fall, machine time for synchrotron radiation will begin, and we plan to analyze single crystals and characteristic objects separated from the stone samples.