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A Combined XRD/XRF Instrument for Lunar Resource Assessment

Robotic surface missions to the Moon should be capable of measuring mineral as well as chemical abundances in regolith samples. Although much is already known about the lunar regolith, our data are far from comprehensive. Most of the regolith samples returned to Earth for analysis had lost the upper surface, or it was intermixed with deeper regolith. This upper surface is the part of the regolith most recently exposed to the solar wind; as such it will be important to resource assessment. In addition, it may be far easier to mine and process the uppermost few centimeters of regolith over a broad area than to engage in deep excavation of a smaller area. The most direct means of analyzing the regolith surface will be by studies in situ. In addition, the analysis of the impact-origin regolith surfaces, the Fe-rich glasses of mare pyroclastic deposits, are of resource interest, but are inadequately known; none of the extensive surface-exposed pyroclastic deposits of the Moon have been systematically sampled, although we know something about such deposits from the Apollo 17 site. Because of the potential importance of pyroclastic deposits, methods to quantify glass as well as mineral abundances will be important to resource evaluation. Combined x ray diffraction (XRD) and x ray fluorescence (XRF) analysis will address many resource characterization problems on the Moon. XRF methods are valuable for obtaining full major-element abundances with high precision. Such data, collected in parallel with quantitative mineralogy, permit unambiguous determination of both mineral and chemical abundances where concentrations are high enough to be of resource grade. Collection of both XRD and XRF data from a single sample provides simultaneous chemical and mineralogic information. These data can be used to correlate quantitative chemistry and mineralogy as a set of simultaneous linear equations, the solution of which can lead to full characterization of the sample. The use of Rietveld methods for XRD data analysis can provide a powerful tool for quantitative mineralogy and for obtaining crystallographic data on complex minerals.

Vaniman, D. T.

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.

Availability of hydrogen for lunar base activities

Hydrogen will be needed on a lunar base to make water for consumables, to provide fuel, and to serve as reducing agent in the extraction of oxygen from lunar minerals. The abundance and distribution of solar wind implanted hydrogen were studied. Hydrogen was found in all samples studied with concentrations varying widely depending on soil maturity, grain size, and mineral composition. Seven cores returned from the moon were studied. Although hydrogen was implanted in the upper surface layer of the regolith, it was found throughout the cores due to micrometeorite reworking of the soil.

Bustin, Roberta

Lunar nearside magnetic anomalies

Contour maps of the vector components of the lunar crustal magnetic field measured with the Apollo 16 subsatellite magnetometer at low altitudes across the central near side are presented. A solution was obtained for a minimum mean magnetization level of about 700 times the stable magnetization component of the most magnetic returned lunar crustal samples. Attention is given to the Reiner Gamma anomaly that is found to represent macroscopic evidence for a surficial darkening process that is dominantly solar wind-dependent.

Hood, L. L.

Entry, Descent, and Landing Operations Analysis for the Genesis Re-Entry Capsule

On September 8, 2004, the Genesis spacecraft returned to Earth after spending 29 months about the sun-Earth libration point collecting solar wind particles. Four hours prior to Earth arrival, the entry capsule containing the samples was released for entry and subsequent landing at the Utah Test and Training Range. This paper provides an overview of the entry, descent, and landing trajectory analysis that was performed during the Mission Operations Phase leading up to final approach to Earth. The operations effort accurately delivered the entry capsule to the desired landing site. The final landing location was 8.3 km from the target, and was well within the allowable landing area. Preliminary reconstruction analyses indicate that the actual entry trajectory was very close to the pre-entry prediction.

Desai, Prasun N.

Removing Contamination From Genesis Sapphire Collectors By Polishing

The Array Collectors of the Genesis spacecraft collected bulk solar wind (SW), as well as three subsets of SW (fast, slow, and coronal mass ejection) in a variety of materials. In all cases the SW implant peaked within < 0.2 microns of the surface. So, when the sample return capsule crashed on landing, cleaning the surfaces for analysis became an extremely difficult, but imperative, task. One collector material was “sapphire”, commercial single crystal corundum. Only ~7.7% of the Genesis Array collectors were sapphire (SAP) but a much higher percentage survived the crash. In fact, surviving bulk SW sapphire collectors have an average area ~10x that of their silicon counterparts since SAP is physically tough, and hard (MOHS 9, by definition) as well as is chemically inert. So, SAP is a good candidate for analytical techniques for measuring SW that require clean areas larger than a millimeter; e.g., synchrotron TXRF and INAA. It is also possible to measure SW in SAP using laser ablation and secondary ion mass spectrometry (SIMS) and, recently, more researchers are choosing to analyze sapphire. Thus, removing surface contamination from SAP could enable many research projects. This report extends the task presented in Schmeling et al. ([4]) that used polishing compounds to remove contamination from Genesis sapphire. It focuses on how polishing with their two top candidates (colloidal silica and cerium oxide) affects the SW layer in SAP.

Genesis solar wind

Advances in Astromaterials Curation: Supporting Future Sample Return Missions

NASA's Astromaterials, curated at the Johnson Space Center in Houston, are the most extensive, best-documented, and leastcontaminated extraterrestrial samples that are provided to the worldwide research community. These samples include lunar samples from the Apollo missions, meteorites collected over nearly 40 years of expeditions to Antarctica (providing samples of dozens of asteroid bodies, the Moon, and Mars), Genesis solar wind samples, cosmic dust collected by NASA's high altitude airplanes, Comet Wild 2 and interstellar dust samples from the Stardust mission, and asteroid samples from JAXA's Hayabusa mission. A full account of NASA's curation efforts for these collections is provided by Allen, et al [1]. On average, we annually allocate about 1500 individual samples from NASA's astromaterials collections to hundreds of researchers from around the world, including graduate students and post-doctoral scientists; our allocation rate has roughly doubled over the past 10 years. The curation protocols developed for the lunar samples returned from the Apollo missions remain relevant and are adapted to new and future missions. Several lessons from the Apollo missions, including the need for early involvement of curation scientists in mission planning [1], have been applied to all subsequent sample return campaigns. From the 2013 National Academy of Sciences report [2]: "Curation is the critical interface between sample return missions and laboratory research. Proper curation has maintained the scientific integrity and utility of the Apollo, Antarctic meteorite, and cosmic dust collections for decades. Each of these collections continues to yield important new science. In the past decade, new state-of-the-art curatorial facilities for the Genesis and Stardust missions were key to the scientific breakthroughs provided by these missions." The results speak for themselves: research on NASA's astromaterials result in hundreds of papers annually, yield fundamental discoveries about the evolution of the solar system (e.g. [3] and references contained therein), and serve the global scientific community as ground truth for current and planned missions such as NASA's Dawn mission to Vesta and Ceres, and the future OSIRIS REx mission to asteroid Bennu [1,3]

Evans, C. A.

Space Weathering of Olivine: Samples, Experiments and Modeling

Olivine is a major constituent of chondritic bodies and its response to space weathering processes likely dominates the optical properties of asteroid regoliths (e.g. S- and many C-type asteroids). Analyses of olivine in returned samples and laboratory experiments provide details and insights regarding the mechanisms and rates of space weathering. Analyses of olivine grains from lunar soils and asteroid Itokawa reveal that they display solar wind damaged rims that are typically not amorphized despite long surface exposure ages, which are inferred from solar flare track densities (up to 10 (sup 7 y)). The olivine damaged rim width rapidly approaches approximately 120 nm in approximately 10 (sup 6 y) and then reaches steady-state with longer exposure times. The damaged rims are nanocrystalline with high dislocation densities, but crystalline order exists up to the outermost exposed surface. Sparse nanophase Fe metal inclusions occur in the damaged rims and are believed to be produced during irradiation through preferential sputtering of oxygen from the rims. The observed space weathering effects in lunar and Itokawa olivine grains are difficult to reconcile with laboratory irradiation studies and our numerical models that indicate that olivine surfaces should readily blister and amorphize on relatively short time scales (less than 10 (sup 3 y)). These results suggest that it is not just the ion fluence alone, but other variable, the ion flux that controls the type and extent of irradiation damage that develops in olivine. This flux dependence argues for caution in extrapolating between high flux laboratory experiments and the natural case. Additional measurements, experiments, and modeling are required to resolve the discrepancies among the observations and calculations involving solar wind processing of olivine.

Keller, L. P.

Understanding the Activation and Solution Properties of Lunar Dust for Future Lunar Habitation

The decision to return humans to the moon by 2020 makes it imperative to understand the effects of lunar dust on human and mechanical systems.( Bush 2004; Gaier 2005; Mendell 2005) During the Apollo missions, dust was found to cause numerous problems for various instruments and systems. Additionally, the dust may have caused health issues for some of the astronauts.(Gaier 2005; Rowe 2007) It is necessary, therefore, for studies to be carried out in a variety of disciplines in order to mitigate the effects of the dust as completely as possible. Due to the lack of an atmosphere, there is nothing to protect the lunar soil from ultraviolet radiation, solar wind, and meteorite impacts. These processes could all serve to "activate" the soil, or produce reactive surface species. In order to understand the possible toxic effects of the reactive dust, it is necessary to "reactivate" the dust, as samples returned during the Apollo missions were exposed to the atmosphere of the Earth. We have used grinding and exposure to UV radiation in order to mimic some of the processes occurring on the lunar surface. To monitor the reactivity of the dust, we have measured the ability of the dust to produce hydroxyl radicals in solution. These radicals have been measured using a novel fluorescent technique developed in our laboratory,(Wallace et al. 2008) as well as using electron paramagnetic resonance (EPR).

Wallace, William T.

Genesis Concentrator Target Particle Contamination Mapping and Material Identification

The majority of surface particles were found to be < 5 microns in diameter with increasing numbers close to the optical resolution limit of 0.3 microns. Acceleration grid EDS results show that the majority of materials appear to be from the SRC shell and SLA materials which include carbon-carbon fibers and Si-rich microspheres in a possible silicone binder. Other major debris material from the SRC included white paint, kapton, collector array fragments, and Al. Image analysis also revealed that SRC materials were also found mixed with the Utah mud and salt deposits. The EDS analysis of the acceleration grid showed that particles < 1 m where generally carbon based particles. Chemical cleaning techniques with Xylene and HF in an ultrasonic bath are currently being investigated for removal of small particles by the Genesis science team as well as ultra-pure water megasonic cleaning by the JSC team [4]. Removal of organic contamination from target materials is also being investigated by the science team with the use of UV-ozone cleaning devices at JSC and Open University [5]. In preparation for solar wind oxygen analyses at UCLA and Open University [1, 2], surface particle contamination on three Genesis concentrator targets was closely examined to evaluate cleaning strategies. Two silicon carbide (Genesis sample # 60001 and 60003) and one chemical vapor deposited (CVD) 13C concentrator target (60002) were imaged and mosaic mapped with optical microscopes. The resulting full target mosaic images and particle feature maps were subsequently compared with non-flight, but flight-like, concentrator targets and sample return capsule (SRC) materials. Contamination found on the flown concentrator acceleration grid was further examined using a scanning electron microscope (SEM). Energy dispersive X-ray spectroscopy (EDS) for particle identification was subsequently compared with the optical images from the flown targets. Figure 1 show that all three targets imaged in this report are fully intact and do not show any signs of material fractures. However, previous ellipsometry results and overview imaging of both flown SiC targets show a solar wind irradiation gradient from the center focal point to the outer edge [3]. In addition, due to the hard landing, each target has experienced varying degrees of impacts, scratches, and particle debris from the spacecraft and Utah impact site.

Calaway, Michael J.

Investigation of the daytime lunar atmosphere

Lunar atmosphere research has tended to center on gases with predictably large sources and on those which have been identified by Apollo experiments. An early candidate atmospheric constituent was Ar 40 which was noted by Heyman and Yaniv to have a surface correlated component in returned soil samples, and an abundance in excess of what can be explained by potassium decay. The source of the excess argon was attributed to atmospheric argon ions which have been accelerated by solar wind fields and implanted in soil grains.

Hodges, R. R., Jr.

Removing Contamination from Genesis Sapphire Collectors by Polishing

The Genesis Solar Wind Sample Re-turn Mission used a variety of materials as solar wind (SW) collectors. “Sapphire”, which is single crystal corundum, was ~6.7% of the collector material flown. But, a much higher percentage of Genesis sapphire collectors (SAP) survived the crash of the sample-return capsule as SAP is chemically inert, physically tough, and hard (MOHS 9, by definition). In fact, 39 sapphire fragments of bulk SW collector having areas ≥60 sq mm are available in JSC’s Genesis online catalog, whereas only 1 similarly sized silicon fragment is available (accessed 1/1/2020). In spite of the ease of accessing larger fragments, sapphire has not been popular among Genesis re-searchers because it is an electrical insulator (making SIMS more difficult) and its chemical inertness, high melting point and high hardness precludes the use of many mass-spectroscopic techniques. Recently, as alternative techniques for measuring Genesis samples are developed (e.g., synchrotron TXRF, INAA, laser ablation mass spectroscopy), more researchers are choosing to analyze sapphire. Thus, a number of researchers are actively studying how to best remove contamination from the Genesis sapphire surfaces. This report extends the task in Schmeling et al. that used polishing compounds to remove contamination from Genesis sapphire and focuses on contaminants (welded silicon, aluminum) that current chemical methods find recalcitrant.

M. Schmeling

Advanced Curation of Current and Future Extraterrestrial Samples

Curation of extraterrestrial samples is the critical interface between sample return missions and the international research community. Curation includes documentation, preservation, preparation, and distribution of samples. The current collections of extraterrestrial samples include: Lunar rocks / soils collected by the Apollo astronauts Meteorites, including samples of asteroids, the Moon, and Mars "Cosmic dust" (asteroid and comet particles) collected by high-altitude aircraft Solar wind atoms collected by the Genesis spacecraft Comet particles collected by the Stardust spacecraft Interstellar dust collected by the Stardust spacecraft Asteroid particles collected by the Hayabusa spacecraft These samples were formed in environments strikingly different from that on Earth. Terrestrial contamination can destroy much of the scientific significance of many extraterrestrial materials. In order to preserve the research value of these precious samples, contamination must be minimized, understood, and documented. In addition the samples must be preserved - as far as possible - from physical and chemical alteration. In 2011 NASA selected the OSIRIS-REx mission, designed to return samples from the primitive asteroid 1999 RQ36 (Bennu). JAXA will sample C-class asteroid 1999 JU3 with the Hayabusa-2 mission. ESA is considering the near-Earth asteroid sample return mission Marco Polo-R. The Decadal Survey listed the first lander in a Mars sample return campaign as its highest priority flagship-class mission, with sample return from the South Pole-Aitken basin and the surface of a comet among additional top priorities. The latest NASA budget proposal includes a mission to capture a 5-10 m asteroid and return it to the vicinity of the Moon as a target for future sampling. Samples, tools, containers, and contamination witness materials from any of these missions carry unique requirements for acquisition and curation. Some of these requirements represent significant advances over methods currently used. New analytical and screening techniques will increase the value of current sample collections. Improved web-based tools will make information on all samples more accessible to researchers and the public. Advanced curation of current and future extraterrestrial samples includes: Contamination Control - inorganic / organic Temperature of preservation - subfreezing / cryogenic Non-destructive preliminary examination - X-ray tomography / XRF mapping / Raman mapping Microscopic samples - handling / sectioning / transport Special samples - unopened lunar cores Informatics - online catalogs / community-based characterization.

Allen, Carlton C.

Lunar Dust and Lunar Simulant Activation, Monitoring, Solution and Cellular Toxicity Properties

During the Apollo missions, many undesirable situations were encountered that must be mitigated prior to returning humans to the moon. Lunar dust (that part of the lunar regolith less than 20 m in diameter) was found to produce several problems with astronaut s suits and helmets, mechanical seals and equipment, and could have conceivably produced harmful physiological effects for the astronauts. For instance, the abrasive nature of the dust was found to cause malfunctions of various joints and seals of the spacecraft and suits. Additionally, though efforts were made to exclude lunar dust from the cabin of the lunar module, a significant amount of material nonetheless found its way inside. With the loss of gravity correlated with ascent of the lunar module from the lunar surface to rendezvous with the command module, much of the major portions of the contaminating soil and dust began to float, irritating the astronaut s eyes and being inhaled into their lungs. Our goal has been to understand some of the properties of lunar dust that could lead to possible hazards for humans. Due to the lack of an atmosphere, there is nothing to protect the lunar soil from ultraviolet radiation, solar wind, and meteorite impacts. These processes could all serve to activate the soil, or produce reactive surface species. In order to understand the possible toxic effects of the reactive dust, it is necessary to reactivate the dust, as samples returned during the Apollo missions were exposed to the atmosphere of the Earth. We have used grinding and UV exposure to mimic some of the processes occurring on the Moon. The level of activation has been monitored using two methods: fluorescence spectroscopy and electron paramagnetic resonance spectroscopy (EPR). These techniques allow the monitoring of hydroxyl radical production in solution. We have found that grinding of lunar dust produces 2-3 times the concentration of hydroxyl radicals as lunar simulant and 10 times that of quartz. Exposure of the lunar dust to UV radiation under vacuum was also found to lead to hydroxyl radical production. After grinding, we have also monitored loss of reactivity of the dusts by exposing them to conditions of known humidity and temperature. From these tests, it was found that the reactivity half-life of lunar simulant is approximately 3 hours, while that of quartz is approximately 2 hours. Placing lunar dust in solution could lead to effects on mechanical and physiological systems, as well as other biological systems. For instance, while it is known that lunar dust is highly abrasive and caused a variety of problems with suits and equipment during Apollo, it is unknown as to how these properties might be affected in the presence of water or other liquids. It is possible that the dust may release minerals (e.g., metallic nanophase Fe) into solution that could speed corrosion or rust. Also, as lunar dust produces hydroxyl radicals (and possibly other reactive oxygen species) in solution, these radicals could also lead to the breakdown of suit or habitat materials. In the body (i.e., in lung solution), the effects could be two-fold. First, if the lunar dust dissolves, it may release an excess of elements (such as zero-valence metallic Fe) that are necessary for bodily functions but only in certain concentration ranges. For lunar dust, the presence of nanophase iron being released into the body is a concern. Secondly, the hydroxyl radicals or other reactive oxygen species produced by the dust in solution could conceivably interact with cells, leading to various problems. We have studied the dissolution of both ground and unground lunar simulant in buffer solutions of different pH. The concentration of a number of species was determined using mass spectrometry. These studies showed that lowering the pH of the solution causes a dramatic increase in the amount of each element released into solution and that grinding also produces higher concentrations. Finally, we have perfmed initial tests aimed at understanding the effects of lunar simulant on cellular systems. Alveolar epithelial cells were cultured and exposed to different concentrations of dust suspended in cell culture media. After predetermined amounts of time, the media was removed and the concentrations of important inflammatory cytokines (IL6, IL8, and TNF-alpha ) were measured. The results of these tests are being used to develop the correct protocols for tests to be performed using lunar dust samples.

Jeevarajan, A.S.

Isotopic studies in returned lunar samples

Analysis of lunar soil samples returned by Apollo 11 and 12 flights are discussed. Isotopic studies of the rare gases from Apollo 11 flight lunar samples are presented. The lunar soil analyses indicated the following: (1) high concentrations of solar wind rare gases, (2) isotopic match between solar wind gases and gas components in gas-rich meteorites, and (3) rare gases attributable to spallation reactions induced in heavier nuclides by cosmic ray particles.

Alexander, E. C., Jr.

Sampling the Uppermost Surface of Airless Bodies

The uppermost surface of an airless body is a critical source of ground-truth information for the various remote sensing techniques that only penetrate nanometers to micrometers into the surface. Such samples will also be vital for understanding conditions at the surface and acquiring information about how the body interacts with its environment, including solar wind interaction, grain charging and levitation [1]. Sampling the uppermost surface while preserving its structure (e.g. porosity, grain-to-grain contacts) however, is a daunting task that has not been achieved on any sample return mission to date.

Noble, S. K.

Electron Spin Resonance (ESR) studies of returned comet nucleus samples

The most important objective of the Comet Nucleus Sample Returm Mission is to return samples which could reflect formation conditions and evolutionary processes in the early solar nebula. It is expected that the returned samples will consist of fine-grained silicate materials mixed with ices composed of simple molecules such as H2O, NH3, CH4 as well as organics and/or more complex compounds. Because of the exposure to ionizing radiation from cosmic-ray, gamma-ray, and solar wind protons at low temperature, free radicals are expected to be formed and trapped in the solid ice matrices. The kind of trapped radical species together with their concentration and thermal stability can be used as a dosimeter as well as a geothermometer to determine thermal and radiation histories as well as outgassing and other possible alternation effects since the nucleus material was formed. Since free radicals that are known to contain unpaired electrons are all paramagnetic in nature, they can be readily detected and characterized in their native form by the Electron Spin Resonance (ESR) method. In fact, ESR has been shown to be a non-destructive, highly sensitive tool for the detection and characterization of paramagnetic, ferromagnetic, and radiation damage centers in terrestrial and extraterrestrial geological samples. The potential use of ESR as an effective method in the study of returned comet nucleus samples, in particular, in the analysis of fine-grained solid state icy samples is discussed.

Tsay, Fun-Dow

Microbial Ecology of NASA Curation Clean Rooms

Clean room standards like ISO 14644 used for facilities that construct spacecraft and store returned samples do not explicitly account for microbial contamination. While there are associated ISO standards for monitoring and controlling bio-contamination in clean rooms it is not always standard practice to do so. The NASA Astromaterials Acquisition and Curation Office maintains seven separate clean labs for storing extraterrestrial samples from the Moon, meteorites, cosmic dust, asteroids, comets, solar wind particles, and microparticle impact samples. These labs are routinely monitored for particulate and trace metal contamination. However, the sample collections are either non-sterile at the time of collection (e.g., meteorites) or are no longer being used to address scientific questions that could be affected by non-sterile conditions (e.g., Lunar samples). Outside of isolated studies there has not been a systematic, longitudinal characterization of the microbial ecology of NASA curation clean rooms. In accordance with the advanced curation initiative, and to prepare for future sample return missions, we have initiated a routine microbiological monitoring program in the Antarctic Meteorite Lab. This monitoring program will be used to determine what microbes are capable of surviving in these oligotrophic environments and whether or not they are capable of altering the sample collections in any significant manner. Repeat sampling will allow us to understand how routine use of these labs affects the microbial ecology over time.

Regberg, A. B.