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Organic and inorganic contamination control approaches for return sample investigation on Mars 2020

The Mars 2020 Rover mission will have the capability to collect and cache samples for potential Mars sample return. Specifically, the sample caching system (SCS) is designed for coring Mars samples and acquiring regolith samples as well as handling, sealing and caching on Mars. As the potential first Martian samples that could be returned to Earth, assuring low levels of terrestrial contamination is of the utmost concern. In developing the SCS, the project prioritizes limiting sample contamination in organic, inorganic and biological areas. The focus of this paper is on the strategies being implemented to limit terrestrial organic and inorganic contamination in the samples.

Steltzner, Adam↗

Robotic Mars Sample Return and Earth entry vehicle concept development

NASA has studied potential Mars Sample Return over many decades, and the most recent Planetary Science Decadal Survey recommended making significant progress on this topic one of its highest priority goals. Recent inter-agency discussions and scientific support are lending credence to current Mars Sample Return planning activities, which notionally target launch of Sample Retrieval Lander and Earth Return Orbiter flight elements in 2026, and return of Martian samples to Earth in 2031. As part of the Mars Sample Return architecture under consideration, an Earth Entry Vehicle would perform the final phase by protecting the samples through severe entry environments using a 60-deg. sphere-cone flying on a passive/ballistic trajectory. The Earth Entry Vehicle design activities in particular are considering a variety of potential challenges, including: minimizing vehicle mass due to the need to travel to Mars and back to Earth, vehicle robustness to Micrometeroid and Orbital Debris impacts, capability to withstand severe entry environments while minimizing landing ellipse size, and providing impact load attenuation during a high-speed landing to meet Martian sample tube load limits and ensure sample containment in off-nominal scenarios. The present work provides a snapshot of current study work in progress, and highlights paths being taken to address these various design challenges for the conceptual Earth Entry Vehicle.

Corliss, James↗

Extensibility of PICA TPS for Future Sample Return Missions

Stardust was the first successful robotic sample return mission delivering samples of the Comet Wild 2 to Earth in 2006. Genesis followed Stardust, in the era of “faster, better, cheaper,” collecting samples of solar wind. The Genesis sample return capsule (SRC) was larger and the program did not have the time nor funding to scale up the Stardust PICA heatshield and so, utilized an alternate heatshield. The successful Stardust mission led to future mission concepts baselining Stardust EDL, especially the entry heatshield. OSIRIS REx, was one such concept and the mission was designed to include build-to-print elements of the Stardust design. The primary scale-up limitation beyond Stardust and OSIRIS REx is the single-piece net cast PICA heatshield. In the past three years, FMI working with NASA Ames, expanded the manufacturing capability of PICA and demonstrated a 1.3 m PICA single piece TPS. This was done in anticipation of the Mars Sample Return mission as well as future Sample Return missions requiring larger-scale SRCs. This effort also identified a sustainable domestic replacement precursor for the PICA preform as the heritage precursor was discontinued in 2016 and FMI has gone through multiple rayon replacements since Stardust. As part of the effort, PICA was also tested at conditions higher than the Stardust or OSIRIS REx entry envelope to establish an expanded performance envelope and enable future sample return missions at higher entry speeds. The poster will highlight PICA sustainability and extensibility as part of the Sample Return to Earth session.

PICA thermal protection↗

Quantitation of Trace Water in ISS Atmosphere Samples Recovered from CO2-Removal Systems

As crewed spaceflight continues to push the limits of exploration, instruments and hardware used to maintain and monitor crew and vehicle health must become more integrated, reliable, and efficient. By combining a carbon dioxide (CO2) removal system with a resource recovery system like a Sabatier or Bosch reactor, the waste gas from the removal system can be converted into valuable resources that help reduce reliance on ground resupply. Due to the high-pressure nature of the Sabatier and Bosch reactions, the vent gas from most CO2 removal systems will need to be compressed before it can be processed. In order to prevent condensation in the compressor of the recovery system, it is critical to ensure that the vent stream from the CO2 removal system does not contain an excess of water. There are currently three different CO2 removal systems that are being developed as candidates for exploration missions. Each of these systems will be evaluated as a technology demonstration on ISS, and vent gas samples will be collected in Summa sampling canisters fitted with Entech valves. Due to the need to measure low levels of water in these samples, it was not possible to use the current ISS miniature grab sample containers (GSCs) to collect these samples. The Summa containers, which were used to collect archive samples during Shuttle missions, have a different surface treatment that makes it possible to measure the low levels of water in samples collected in these containers. This paper will provide some background on the CO2 removal systems being evaluated for exploration missions as well as results from ground-based testing of the current miniature GSCs and Summa canisters. Details on the development of the analytical method and the plan for preparing the canisters that will be used for in-flight sampling are also discussed.

Steven W Beck↗

Mars Sample Return Mission Concept Status

This paper will provide an overview of current concepts and options for the architecture and design of a Mars Sample Return Mission, including the Sample Retrieval Lander (SRL) (developed by NASA) and the Earth Return Orbiter (ERO) (developed by ESA) . Key mission objectives and the overall campaign will be described, including the mission’s concept of operations and a notional timeline from launch to entry, through surface operations, to delivery of the samples to Mars orbit and return to Earth. The overall SRL lander vehicle concept will be described, including current options being evaluated. Key lander element options that have been studied will be discussed, including the Mars Ascent Vehicle (MAV), Sample Fetch Rover (provided by ESA), Orbiting Sample container (OS), and sample tube transfer robotics systems. For the ERO the vehicle concept will be described including key interfaces with the Capture/Containment and Return System (CCRS). Specific challenges and approaches for addressing those challenges will be discussed, including key technical margins and backward planetary protection. The information provided about possible Mars sample return architectures is for planning and discussion purposes only. NASA has made no official decision to implement Mars sample return.

Muirhead, Brian K↗

Assessing the Sampleability of Bennu’s Surface for the OSIRIS-REx Asteroid Sample Return Mission

NASA’s first asteroid sample return mission, OSIRIS-REx, collected a sample from the surface of near-Earth asteroid Bennu in October 2020 and will deliver it to Earth in September 2023. Selecting a sample collection site on Bennu’s surface was challenging due to the surprising lack of large ponded deposits of regolith particles exclusively fine enough (≤ 2 cm diameter) to be ingested by the spacecraft’s Touch-and-Go Sample Acquisition Mechanism (TAGSAM). Here we describe the Sampleability Map of Bennu, which was constructed to aid in the selection of candidate sampling sites and to estimate the probability of collecting sufficient sample. “Sampleability” is a numeric score that expresses the compatibility of a given area’s surface properties with the sampling mechanism. The algorithm that determines sampleability is a best fit functional form to an extensive suite of laboratory testing outcomes tracking the TAGSAM performance as a function of four observable properties of the target asteroid. The algorithm and testing were designed to measure and subsequently predict TAGSAM collection amounts as a function of the minimum particle size, maximum particle size, particle size frequency distribution, and the tilt of the TAGSAM head off the surface. The sampleability algorithm operated at two general scales, consistent with the resolution and coverage of data collected during the mission. The first scale was global and evaluated nearly the full surface. Due to Bennu’s unexpected boulder coverage and lack of ponded regolith deposits, the global sampleability efforts relied heavily on additional strategies to find and characterize regions of interest based on quantifying and avoiding areas heavily covered by material too large to be collected. The second scale was site-specific and used higher-resolution data to predict collected mass at a given contact location. The rigorous sampleability assessments gave the mission confidence to select the best possible sample collection site and directly enabled successful collection of hundreds of grams of material.

Asteroid exploration↗

Quantitation of Trace Water in ISS Atmosphere Samples Recovered from CO2-Removal Systems

As crewed spaceflight continues to push the limits of exploration, instruments and hardware used to maintain and monitor crew and vehicle health, must become more integrated, reliable, and efficient. By combining a carbon dioxide (CO2) removal system with a resource recovery system like a Sabatier or Bosch reactor, the waste gas from the removal system can be converted into valuable resources that help reduce reliance on ground resupply. Due to the high-pressure nature of the Sabatier and Bosch reactions, the vent gas from most CO2 removal systems will need to be compressed before it can be processed. In order to prevent condensation in the compressor of the recovery system, it is critical to ensure that the vent stream from the CO2 removal system does not contain an excess of water. There are currently two different CO2 removal systems that are being developed as candidates for exploration missions. Each of these systems will be evaluated as a technology demonstration on ISS, and vent gas samples will be collected in Summa sampling canisters fitted with Entech valves for ground analysis. Due to the need to measure low levels of water in these samples, it was not possible to use the current ISS mini-grab sample containers (m-GSC) to collect these samples. The Summa containers, which were used to collect archive samples during Shuttle missions, have a different surface treatment that makes it possible to measure the low levels of water in samples collected in these containers. This paper will provide some background on the CO2 removal systems being evaluated for exploration missions as well as results from ground-based testing of the Summa canisters. Details on the development of the analytical method and the plan for preparing the canisters that will be used for in-flight sampling are also discussed.

William M. King↗

Processing Frozen Apollo Samples in a Nitrogen Environment

A few weeks after their return to Earth, several Apollo 17 regolith sample splits and one Apollo 17 basalt were frozen at -20˚C (under dry gaseous N2 like all other pristine Apollo samples), and have remained essentially unstudied within the Apollo sample collection at NASA’s Johnson Space Center (JSC). As part of the Apollo Next Generation Sample Analysis (ANGSA) project, these frozen samples were selected for consortium study in 2019. Although the samples themselves were kept at -20˚C for nearly 50 years, the JSC Curation office has lacked a facility for processing frozen samples under pristine Apollo processing conditions. A temporary lab for this work was designed, built, and tested. Procedures were then developed for working in this unique environment, and the facility was sucessfully used to process the frozen Apollo samples for scientific allocation.

ANGSA↗

Sampling Functions from Gaussian Processes and Structured Covariance Gaussian Networks

When learning aerodynamic models from data, it is critical to incorporate estimates of model uncertainty. This motivates the design of probabilistic aerodynamic databases which can be sampled to generate physically and statistically plausible aerodynamic models. In this talk we discuss how to sample deterministic functions from two different kinds of probabilistic models and demonstrate their use. First, Gaussian Process Regressors (GPRs) are a widely used probabilistic kernel-based model which can be thought of as Gaussian distributions over functions. GPRs are generally trained by maximizing the marginal likelihood of seeing the training data over the kernel parameter space. Sample functions are easily generated by drawing points from the Gaussian distribution at desired input points. However, when the points are not known ahead of time, the classical sampling approach is not possible since successive function samples will generate different function realizations. We present an approach for sampling consistent function evaluations from a GPR over multiple samples. Second, we describe a neural network architecture which learns a conditional Gaussian distribution by maximizing the marginal likelihood at each point in the input space. We then discuss and compare several options for generating sample functions which match this distribution. Finally, we demonstrate the use of these probabilistic aerodynamic models in an atmospheric reentry simulation.

Gaussian process regression↗

Evolved Gas Analyses of Sedimentary Rocks from the Glen Torridon Clay-Bearing Unit, Gale Crater, Mars: Results From the Mars Science Laboratory Sample Analysis at Mars Instrument Suite

Evolved gas analysis (EGA) data from the Sample Analysis at Mars (SAM) instrument suite indicated Fe-rich smectite, carbonate, oxidized organics, Fe/Mg sulfate, and chloride in sedimentary rocks from the Glen Torridon (GT) region of Gale crater that displayed phyllosilicate spectral signatures from orbit. SAM evolved H2O data indicated that the primary phyllosilicate in all GT samples was an Fe-rich dioctahedral smectite (e.g., nontronite) with lesser amounts of a phyllosilicate such as mixed layer talc-serpentine or greenalite-minnesotaite. CO(2) data supported the identification of siderite in several samples, and CO(2) and CO data was also consistent with trace oxidized organic compounds such as oxalate salts. SO(2) data indicated trace and/or amorphous Fe sulfates in all samples and one sample may contain Fe sulfides. SO(2) data points to significant Mg sulfates in two samples, and lesser amounts in several other samples. A lack of evolved O(2) indicated the absence of oxychlorine salts and Mn3+/Mn4+ oxides. The lack of, or very minor, evolved NO revealed absent or very trace nitrate/nitrite salts. HCl data suggested chloride salts in GT samples. Constraints from EGA data on mineralogy and chemistry indicated that the environmental history of GT involved alteration with fluids of variable redox potential, chemistry and pH under a range of fluid-to-rock ratio conditions. Several of the fluid episodes could have provided habitable environmental conditions and carbon would have been available to any past microbes though the lack of significant N could have been a limiting factor for microbial habitability in the GT region.

A. C. McAdam↗

Optimizing Single Nuclei Sequencing of Brain Samples From Space Flown Mice Across Age and Strain

The NASA GeneLab Sample Processing Laboratory offers high-throughput sequencing services to NASA-funded space biology researchers. Space biology studies have specific challenges such as low sample numbers, introducing susceptibility to batch effects from sample handling. These issues are compounded by complex protocols such as single-nuclei isolation and sequencing, which has recently become an attractive methodology for assessing the cellular diversity within spaceflight samples. High quality single-nuclei sequencing requires reproducible protocols to dissociate tissue and generate clean suspension of intact single nuclei. Producing single-nuclei suspension from brain tissue is particularly challenging due to cell type heterogeneity and the myelin sheath that carries over into the nuclei suspension as debris. Current procedures tend to be time consuming and sometimes include steps that can alter gene expression and create cell-type bias. Commercially available nuclei isolation kits, such as the 10X Genomics nuclei isolation kit, offers a streamlined way to process samples for nuclei isolation, thereby minimizing batch effects and enabling reproducibility. In this study, we report on the performance of the 10X Genomics nuclei isolation kit and Chromium Next GEM Single Cell Multiome ATAC + Gene Expression kit to generate sequencing libraries from space-flown mouse brain samples. Single nuclei sequencing was performed on frozen mouse brain tissue from two spaceflight missions, Rodent Research-10 (RR-10) and RR Reference Mission-2 (RRRM-2). RR-10 mice were female B6129SF2/J, euthanized at 18-19 weeks whereas RRRM-2 mice were female C57BL/6NTac, euthanized at 20 or 37 weeks. Sequencing data was processed using standard GeneLab data processing pipelines. We report evaluation of the performance of the 10X Genomics nuclei isolation kit for spaceflight samples from mouse brain, and evaluation of reproducibility across different mouse strains and age groups. We also report preliminary scientific results including cell type inference, cell clustering, and differentially expressed genes and pathways between spaceflight and ground control samples.

RR-10↗

Investigating the Impact of X-Ray Computed Tomography Imaging on Soluble Organic Matter in the Murchison Meteorite: Implications for Bennu Sample Analyses

X-ray computed tomography (XCT) is a valuable reconnaissance tool for three-dimensional imaging and identification of distinct lithologies in extraterrestrial samples. It will be used as part of the preliminary examination of samples returned from asteroid (101955) Bennu by the Origins, Spectral Interpretation, Resource Identification, and Security–Regolith Explorer (OSIRIS-REx) mission. However, it must first be established whether x-rays generated during XCT could degrade or alter the organic composition of the returned samples by radiolysis. To test this, we split a crushed sample of the Murchison CM2 meteorite, kept one portion as a control, and irradiated the other portion up to the maximum x-ray dosage (~180 Gy) that a Bennu sample would experience during an XCT imaging experiment. We then extracted organic compounds from both splits and conducted (i) nontargeted soluble organic analyses to compare the chemical distributions of C-, H-, O-, N-, and S-bearing species and (ii) targeted measurements to quantify the abundances of 96 individual soluble organic molecules that included protein amino acids, amines, carboxylic acids, hydroxy acids, carbonyl compounds, polycyclic aromatic hydrocarbons, alcohols, sugars, and N-heterocycles. We found that XCT imaging of the Murchison meteorite had no measurable impact on the relative abundances or enantiomeric compositions of most of the soluble organic compounds targeted in this study. Elevated total abundances of several soluble organic compound classes were observed in the XCT-scanned Murchison sample relative to the control. This is likely related to particle size heterogeneity and specific surface area differences between the sample aliquots used for the extractions, rather than a result of the x-ray exposure. Assuming the samples returned from asteroid Bennu by OSIRIS-REx have a similar composition to carbonaceous chondrites, these data provide confidence that XCT will not significantly alter their soluble organic compositions.

Daniel P Glavin↗

Identification of Presolar Grains in Quick Look Samples of Asteroid Bennu Returned By the OSIRIS-REx Mission

The OSIRIS-REx spacecraft returned regolith sample from the B-type asteroid Bennu on September 24, 2023. The first samples to be analyzed, termed the Quick Look samples, are comprised of material collected from the avionics deck of the OSIRIS-REx sample canister. Initial mineralogical analysis of the Quick Look sample revealed a diversity of components, including hydrated and anhydrous silicates, sulfides, magnetite, phosphates, and abundant organic matter. Each constituent has their own origin and history, and their study can inform us of the history of Bennu and its parent asteroid. The analysis plan for asteroid Bennu samples is guided by hypotheses that address specific periods of Bennu’s history, from the pre-accretionary epoch to the OSIRIS-REx epoch. The pre-accretionary epoch studies aim to characterize materials that predate the formation of the solar system. One hypothesis that falls under this epoch is that Bennu contains presolar materials derived from diverse sources. These presolar materials include stardust grains that condensed from the outflows of evolved stars or the ejecta of novae and supernovae (SN), as well as organic matter that formed in the interstellar medium. Here we report the identification of C-rich presolar stardust grains in the Bennu Quick Look sample. Isotopically anomalous organic matter in this sample is reported in.

A N Nguyen↗

Summary of Apollo Next Generation Sample Analysis (ANGSA) and Insights for Artemis Preliminary Examination Activities

Analyses of Apollo samples have provided fundamental insights into the origin and history of the Earth-Moon system and the solar system broadly. With great foresight, a subset of samples from Apollo were left unprocessed so that they could be studied by future generations with their modern technology. To prepare for the return of samples from the Moon by the Artemis Program, NASA initiated the Apollo Next Generation Sample Analysis Program (ANGSA) to analyze a subset of the previously unprocessed Apollo samples. The ANGSA consortium consisted of 9 original teams funded by NASA that combined into a single science team referred to as the ANGSA Science Team. ANGSA was designed to function like the sample analysis phase of a sample return mission with a goal to investigate the lower portion of a double drive tube previously sealed on the lunar surface (73001), the upper portion of that drive tube that had remained unopened (73002), and a variety of Apollo 17 samples that had remained stored at -20 ºC for approximately 50 years.

Francis M. McCubbin↗

Trace Oxygen Measurements of Asteroid Sample Storage Desiccators

The Astromaterials Curation facility at the NASA Johnson Space Center is currently curating more than 120 g of carbonaceous asteroid Bennu material as well as over 500 mg of asteroid Ryugu [1 and 2]. These astromaterials are stored in isolating desiccators and gloveboxes under a continuous purge of pure (<1 ppm O 2 ) gaseous nitrogen. The oxygen and moisture concentrations in our OSIRIS-REx sample processing gloveboxes are continuously monitored via integrated sensors; however, our sample storage desiccators lack integrated oxygen and humidity sensors. In previous studies, we used PreSens Fibox 4 trace oxygen meters and optochemical PSt9 spot sensors to measure the oxygen concentrations in candidate asteroid sample containers that had been sealed in nitrogen; we determined that Eagle stainless steel containers inhibit the ingress of external oxygen for several weeks [3]. This optochemical sensor technology allowed us to take precise, contactless measurements within a trace range of 0 to 200 ppmv O 2 . The effectiveness of the trace oxygen sensors in our container experiments inspired us to utilize them to assess the performance of our desiccators that previously lacked trace oxygen monitoring. In this study, our goal was to determine the quality of the nitrogen purge in the isolating desiccator under normal operating conditions by measuring the trace oxygen content. Utilizing optochemical sensor technology, we determined how long the oxygen concentration takes to reach an equilibrium in the desiccator; that is, determine the rate at which the oxygen diffusion into the desiccator equals the rate at which oxygen diffuses out of the desiccator via N2 purge. Additionally, we wanted to determine the oxygen concentration at this equilibrium, the state in which our desiccators are in during normal operating conditions. We tested a custom three chamber desiccator manufactured by Germfree using a PSt9 trace oxygen sensor spot that was mounted into a ¼” National Pipe Tapered (NPT) metal flow-through cell and attached it to the desiccator exhaust. The desiccator consists of top, middle, and bottom isolating chambers. The top chamber door was opened for several minutes to simulate a sample exchange, it was sealed, and then purged ~15 Standard Cubic Feet per Hour (SCFH). Oxygen measurements were automatically recorded via the Fibox 4 trace oxygen meter in 5-minute intervals over the course of a 24-hour period. Our results indicate the desiccator reached an equilibrium value of 10-15 ppm O 2 after ~5 hours (Fig. 1). This data allows us to explore standards for purging and exchange protocols that can be applied to similar types of desiccators in Hayabusa2, OSIRIS-REx, and for sample return collections. The assessment of the internal gaseous compositions of desiccators also allows us to share with the community the N 2 environment in which many of our asteroid samples and hardware are securely curated. Future measurements will include other nitrogen flow rates and measuring the trace oxygen concentration as a function of time for the levels of the previous commercial desiccator in which the Hayabusa2 sample collection was stored. We will also analyze how long the desiccators hold N2 after being disconnected from their N2 source, an extended measurement for sample security reassurance.

Curation↗

Proteomic Sample Preparation Techniques: Towards Forensic Proteomic Applications

Proteomic sample preparation techniques rely on dynamic multi-step processes that are sample type dependent. Forensic proteomic applications comprise diverse sample types and therefore require numerous sample preparation workflows. A sample may need pre-treatment steps to solubilize proteins from a solid surface, for example - from clothing, from a swab, or off of a filter. A sample may need to be disrupted or homogenized to liberate proteins trapped in cells. Or a sample may need additional processing steps, such as organic extraction, to isolate proteins from small molecule contaminants which interfere with mass spectrometry (MS) measurements. Following these pre-treatment steps, proteins are reduced, denatured, alkylated, and enzymatically digested. The resulting peptide mixture can be desalted by solid phase extraction or fractionated prior to liquid chromatography MS-based proteomic characterization. Here we detail each step of this multi-stage sample type dependent processing.

Nicora, Carrie D.↗

Sampling synchronization through GPS signals

A method uses a distributed data acquisition system with multiple, physically unconnected, data acquisition units, that can be in wireless communication with a remote host, to timestamp measurement data with sub-microsecond time base accuracy of sampling clock relative to an absolute timeframe. A current absolute time is derived from messages received from a satellite radio beacon positioning system (GPS). Measurement data is sampled by each unit at a specified sampling rate. Using hardware logic, batches of sampled data are associated with corresponding timestamps representing the absolute time at which the data was sampled. Data and timestamps may be transmitted to the host. A time offset bias is compensated by comparing timestamps against a nominal time based on start time and nominal sampling rate. The sampling clock rate may be disciplined using time pulses from the GPS receiver. An initial start of data sampling by all units can also be synchronized.

Zhuge, James Q.↗

Sample mount for electron backscatter diffraction

A sample mount having a bottom surface, a front surface, and a second portion is disclosed. The first portion is perpendicular to the bottom surface. The second portion has an external surface and an internal surface and extends from the first portion to form a 70-degree angle relative to the bottom surface. The sample mount may also have a top surface, an opening extending through the second portion of the front surface, and a receiving area configured to receive a sample, wherein the top surface presents an unimpeded path between the sample and an SEM pole piece. The sample mount may include a spring-loaded handle configured to push the sample against the internal surface of the second portion of the front surface, wherein pushing the sample against the internal surface places the sample at the 70-degree angle relative to the bottom surface.

Wieliczka, David M.↗