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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↗
NASA NTRS2010

Probabilistic Round Trip Contamination Analysis of a Mars Sample Acquisition and Handling Process Using Markovian Decompositions

A method for evaluating the probability of a Viable Earth Microorganism (VEM) contaminating a sample during the sample acquisition and handling (SAH) process of a potential future Mars Sample Return mission is developed. A scenario where multiple core samples would be acquired using a rotary percussive coring tool, deployed from an arm on a MER class rover is analyzed. The analysis is conducted in a structured way by decomposing sample acquisition and handling process into a series of discrete time steps, and breaking the physical system into a set of relevant components. At each discrete time step, two key functions are defined: The probability of a VEM being released from each component, and the transport matrix, which represents the probability of VEM transport from one component to another. By defining the expected the number of VEMs on each component at the start of the sampling process, these decompositions allow the expected number of VEMs on each component at each sampling step to be represented as a Markov chain. This formalism provides a rigorous mathematical framework in which to analyze the probability of a VEM entering the sample chain, as well as making the analysis tractable by breaking the process down into small analyzable steps.

Hudson, Nicolas↗
NASA NTRS2008

Curation of Frozen Samples

NASA's Johnson Space Center (JSC) and the Astromaterials Curator are charged by NPD 7100.10D with the curation of all of NASA s extraterrestrial samples, including those from future missions. This responsibility includes the development of new sample handling and preparation techniques; therefore, the Astromaterials Curator must begin developing procedures to preserve, prepare and ship samples at sub-freezing temperatures in order to enable future sample return missions. Such missions might include the return of future frozen samples from permanently-shadowed lunar craters, the nuclei of comets, the surface of Mars, etc. We are demonstrating the ability to curate samples under cold conditions by designing, installing and testing a cold curation glovebox. This glovebox will allow us to store, document, manipulate and subdivide frozen samples while quantifying and minimizing contamination throughout the curation process.

Fletcher, L. A.↗
NASA NTRS2014

Cellulose Acetate Replica Cleaning Study of Genesis Non-Flight Sample 3CZ00327

The Genesis mission collected solar wind and brought it back to Earth in order to provide precise knowledge of solar isotopic and elemental compositions. The ions in the solar wind were stopped in the collectors at depths on the order of 10 to a few hundred nanometers. This shallow implantation layer is critical for scientific analysis of the composition of the solar wind and must be preserved throughout sample handling, cleaning, processing, distribution, preparation and analysis. We are working interactively with the community of scientists analyzing Genesis samples, using our unique laboratory facilities -- and, where needed, our unique cleaning techniques -- to significantly enhance the science return from the Genesis mission. This work is motivated by the need to understand the submicron contamination on the collectors in the Genesis payload as recovered from the crash site in the Utah desert, and -- perhaps more importantly -- how to remove it. That is, we are evaluating the effectiveness of the wet-chemical "cleaning" steps used by various investigators, to enable them to design improved methods of stripping terrestrial contamination from surfaces while still leaving the solar-wind signal intact.

Kuhlman, K. R.↗
NASA NTRS2016

Small Particulate Contamination Survey Of Genesis Flight Sample 61423

The Genesis mission collected solar wind and brought it back to Earth in order to provide precise knowledge of solar isotopic and elemental compositions. The ions in the solar wind stop in the collectors at depths on the order of 10 to a few hundred nanometers. This shallow implantation layer is critical for scientific analysis of the composition of the solar wind and must be preserved throughout sample handling, cleaning, processing, distribution, preparation and analysis. We continue to work with the community of scientists analyzing Genesis samples using our unique laboratory facilities -- and, where needed, our unique cleaning techniques -- to significantly enhance the science return from the Genesis mission. This work is motivated by the need to understand the submicron contamination on the collectors in the Genesis payload as recovered from the crash site in the Utah desert, and -- perhaps more importantly -- how to remove it. We continue to evaluate the effectiveness of the wet-chemical "cleaning" steps used by various investigators, to enable them to design improved methods of stripping spacecraft and terrestrial contamination from surfaces while still leaving the solar-wind signal intact.

Kuhlman, K. R.↗
NASA NTRS2013

Examples of Optical Assessment of Surface Cleanliness of Genesis Samples

Optical microscope assessment of Genesis solar wind collector surfaces is a coordinated part of the effort to obtain an assessed clean subset of flown wafer material for the scientific community. Microscopic survey is typically done at 50X magnification at selected approximately 1 square millimeter areas on the fragment surface. This survey is performed each time a principle investigator (PI) returns a sample to JSC for documentation as part of the established cleaning plan. The cleaning plan encompasses sample handling and analysis by Genesis science team members, and optical survey is done at each step in the process. Sample surface cleaning is performed at JSC (ultrapure water [1] and UV ozone cleaning [2]) and experimentally by other science team members (acid etch [3], acetate replica peels [4], CO2 snow [5], etc.). The documentation of each cleaning method can potentially be assessed with optical observation utilizing Image Pro Plus software [6]. Differences in particle counts can be studied and discussed within analysis groups. Approximately 25 samples have been identified as part of the cleaning matrix effort to date.

Rodriquez, Melissa C.↗
NASA NTRSDate not supplied

Stratigraphy of the Apollo 17 Landslide Core 73002 From FMR Maturity and VNIR and Mössbauer Spectroscopy

A suite of samples from the Apollo missions to the Moon (1969-1973) were set aside and stored under controlled conditions to have unexamined lunar samples available decades later for analyses that take advantage of evolved sample handling techniques, maturation of then existing instrumentation, and development of new analytical techniques and instrumentation [e.g., 1]. One preserved sample is the Apollo 17 double drive tube core (73001/2) that was driven into the lunar surface on the landslide deposit at Station 3 on the South Massif in the Taurus-Littrow valley [2]. The deeper section (73001) was stored frozen in a Core Sample Vacuum Container (CSVC) to maximize preservation of lunar volatiles. We report here, as a part of the Apollo Next Generation Sample Analysis (ANGSA) Initiative [1,3], stratigraphy for the upper core section (73002) with respect to maturity (ferromagnetic resonance (FMR) maturity index Is/FeO [4-6]), visible-near-IR (VNIR) spectroscopy, and, for representative samples, grain-size analysis and Mössbauer spectroscopy. Stratigraphy provides data to model the dynamics of lunar landslide deposits and their post-emplacement evolution in comparison to impact-driven mixing on an airless body and stratigraphic context for volatile and (if any) organic behavior. Reported by [7] are preliminary results for multispectral imaging and hyperspectral scanning of the first dissection pass of 73002.

R. V. Morris↗
NASA NTRS2014

GeoLab: A Geological Workstation for Future Missions

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

Evans, Cynthia↗
NASA NTRS2016

Drilling Subsurface Ice at the Haughton Crater Analog Site

Over a decade of evolutionary development of integrated automated drilling and sample handling at the terrestrial polar Mars analog site at Haughton Crater has made it possible to propose missions that could sample 1-2m into rocks and ice on Mars. The eventual search for biomarkers and signs of past or extant life in Mars polar regions will require sample acquisition there below the desiccated and irradiated surface. Drilling and drill tests at the Haughton Crater site since 1998 have also shown a retreat downward of the active-layer boundary in annual measurements.

subsurface↗
NASA NTRS2008

Portable Device Analyzes Rocks and Minerals

inXitu Inc., of Mountain View, California, entered into a Phase II SBIR contract with Ames Research Center to develop technologies for the next generation of scientific instruments for materials analysis. The work resulted in a sample handling system that could find a wide range of applications in research and industrial laboratories as a means to load powdered samples for analysis or process control. Potential industries include chemical, cement, inks, pharmaceutical, ceramics, and forensics. Additional applications include characterizing materials that cannot be ground to a fine size, such as explosives and research pharmaceuticals.

Source record↗
NASA NTRSDate not supplied

Characterization Of Early Solar System Aqueous Fluids

The most direct and convincing evidence for the presence of water and organic molecules on protoplanetary bodies is provided by fluid inclusions trapped in secondary minerals. Our research has demonstrated that early solar system fluids have survived as fluid inclusions in a few astromaterials that escaped significant shock, terrestrial alteration, and invasive sample handling. Our long-term goal is to measure bulk molecular and isotopic composition of individual fluid inclusions in meteorites and samples collected directly from asteroids to provide ground truth regarding the nature and evolution of aqueous fluids in the early solar system. Our current protocol is to locate candidate fluid inclusions using X-Ray Computed Tomography, and then make compositional measurements of individual fluid inclusions by coordinated Raman spectrometry, Transmission Electron Microscopy and, most recently, Time of Flight – Secondary Ion Mass Spectrometry.

Michael Zolensky↗
NASA NTRS1988

Fluid inclusions in Martian samples: Clues to early crustal development and the hydrosphere

Major questions about Mars that could be illuminated by examining fluid inclusions in Martian samples include: (1) the nature, extent and timing of development (and decline) of the hydrosphere that existed on the planet; and (2) the evolution of the crust. Fluid inclusion analyses of appropriate samples could provide critical data to use in comparison with data derived from analogous terrestrial studies. For this study, sample handling and return restrictions are unlikely to be as restrictive as the needs of other investigators. The main constraint is that the samples not be subjected to excessively high temperatures. An aqueous fluid inclusion trapped at elevated pressure and temperature will commonly consist of liquid water and water vapor at room temperature. Heating (such as is done in the laboratory to fix P-V-T data for the inclusion) results in moderate pressure increases up to the liquid-vapor homogenization temperature followed by a sharp increase in pressure with continued heating because the inclusion is effectively a fixed volume system. This increased pressure can rupture the inclusion; precise limits are dependent on size, shape, and composition as well as the host material.

Brown, Philip E.↗
NASA NTRS2024

Future of the Search for Life: Workshop Report

The 2-week, virtual Future of the Search for Life science and engineering workshop brought together more than 100 scientists, engineers, and technologists in March and April 2022 to provide their expert opinion on the interconnections between life-detection science and technology. Participants identified the advances in measurement and sampling technologies they believed to be necessary to perform in situ searches for life elsewhere in our Solar System, 20 years or more in the future. Among suggested measurements for these searches, those pertaining to three potential indicators of life termed “dynamic disequilibrium,” “catalysis,” and “informational polymers” were identified as particularly promising avenues for further exploration. For these three indicators, small breakout groups of participants identified measurement needs and knowledge gaps, along with corresponding constraints on sample handling (acquisition and processing) approaches for a variety of environments on Enceladus, Europa, Mars, and Titan. Despite the diversity of these environments, sample processing approaches all tend to be more complex than those that have been implemented on missions or envisioned for mission concepts to date. The approaches considered by workshop breakout groups progress from nondestructive to destructive measurement techniques, and most involve the need for fluid (especially liquid) sample processing. Sample processing needs were identified as technology gaps. These gaps include technology and associated sampling strategies that allow the preservation of the thermal, mechanical, and chemical integrity of the samples upon acquisition; and to optimize the sample information obtained by operating suites of instruments on common samples. Crucially, the interplay between science-driven life-detection strategies and their technological implementation highlights the need for an unprecedented level of payload integration and extensive collaboration between scientists and engineers, starting from concept formulation through mission deployment of life-detection instruments and sample processing systems.

Marc Neveu↗
NASA NTRS2013

Robotic Sample Manipulator for Handling Astromaterials Inside the Geolab Microgravity Glovebox

Future human and robotic sample return missions will require isolation containment systems with strict protocols and procedures for reducing inorganic and organic contamination. Robotic handling and manipulation of astromaterials may be required for preliminary examination inside such an isolation containment system. In addition, examination of astromaterials in microgravity will require constant contact to secure samples during manipulation. The National Space Grant Foundation exploration habitat (XHab) academic innovative challenge 2012 administered through the NASA advanced exploration systems (AES) deep space habitat (DSH) project awarded funding to the University of Bridgeport team to develop an engineering design for tools to facilitate holding and handling geological samples for analysis in a microgravity glovebox environment. The Bridgeport XHab team developed a robotic arm system with a three-finger gripper that could manipulate geologic samples within the existing GeoLab glovebox integrated into NASA's DSH called the GeoLab Robotic Sample Manipulator (see fig. 1 and 2). This hardware was deployed and tested during the 2012 DSH mission operations tests [1].

Bell, Mary S.↗
NASA NTRS1991

Precision metering of microliter volumes of biological fluids in micro-gravity

Concepts were demonstrated and investigated for transferring accurately known and reproducible microliter volumes of biological fluids from sample container onto dry chemistry slides in microgravity environment. Specific liquid transfer tip designs were compared. Information was obtained for design of a liquid sample handling system to enable clinical chemical analysis in microgravity. Disposable pipet tips and pipet devices that were designed to transfer microliter volumes of biological fluid from a (test tube) sample container in 1-G environment were used during microgravity periods of parabolic trajectories of the KC-135 aircraft. The transfer process was recorded using charge coupled device camera and video cassette equipment. Metering behavior of water, a synthetic aqueous protein solution, and anticoagulated human blood was compared. Transfer of these liquids to 2 substrate materials representative of rapidly wettable and slowly wettable dry chemistry slide surface was compared.

Columbus, Richard L.↗
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 NTRS2010

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

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

Evans, C. A.↗