Nondestructive Analysis of Apollo Samples by Micro-CT and Micro-XRF Analysis: A PET Style Examination

An integral part of any sample return mission is the initial description and classification of returned samples by the preliminary examination team (PET). The goal of a PET is to characterize and classify the returned samples, making this information available to the general research community who can then conduct more in-depth studies on the samples. A PET strives to minimize the impact their work has on the sample suite, which often limits the PET work to largely visual measurements and observations like optical microscopy. More modern techniques can also be utilized by future PET to nondestructively characterize astromaterials in a more rigorous way. Here we present our recent analyses of Apollo samples 14321 and 14305 by micro-CT and micro-XRF (respectively), assess the potential for discovery of "new" Apollo samples for scientific study, and evaluate the usefulness of these techniques in future PET efforts

Characterization of Apollo Regolith by X-Ray and Electron Microbeam Techniques: An Analog for Future Sample Return Missions

The Apollo missions collected 382 kg of rock and regolith from the Moon; approximately 1/3 of the sample mass collected was regolith. Lunar regolith consists of well mixed rocks, minerals, and glasses less than 1-centimeter n size. The majority of most surface regolith samples were sieved into less than 1, 1-2, 2-4, and 4-10- millimiter size fractions; a portion of most samples was re-served unsieved. The initial characterization and classification of most Apollo regolith particles was done primarily by binocular microscopy. Optical classification of regolith is difficult because (1) the finest fraction of the regolith coats and obscures the textures of the larger particles, and (b) not all lithologies or minerals are uniquely identifiable optically. In recent years, we have begun to use more modern x-ray beam techniques [1-3], coupled with high resolution 3D optical imaging techniques [4] to characterize Apollo and meteorite samples as part of the curation process. These techniques, particularly in concert with SEM imaging of less than 1-millimeter regolith grain mounts, allow for the rapid characterization of the components within a regolith

Lunar Glovebox Balance with Wireless Technology

The most important equipment required for processing lunar samples is a high-quality mass balance for maintaining accurate weight inventory, security, and scientific study. After careful review, a Curation Office memo by Michael Duke in 1978 chose the Mettler PL200 to be used for sample weight measurements inside the gloveboxes (Fig. 3). These commercial off-the-shelf (COTS) balances did not meet the strict accepted material requirements in the Lunar lab. As a result, each balance housing, weighing pan, and wiring was custom retrofitted to meet Lunar Operating Procedure (LOP) 54 requirements [for material construction restrictions]. The original design drawings for the custom housings, readout support stands, and wiring were done by the JSC engineering directorate. The 1977- 1978 schematics, drawings, and files are now housed in the curation Data Center. Per the design specifications, the housing was fabricated from aluminum grade 6061 T6, seamless welds, and anodized per MIL-A-8625 type I, class I. The balance feet were TFE Teflon and any required joints were sealed with Viton A gaskets. The readout display and support stands outside the glovebox were fabricated from 300 series stainless steel with #4 finish and mounted to the glovebox with welded bolts. Wire harnesses that linked the balance with the outside display and power were encapsulated with TFE Teflon and transported through custom Deutsch wire bulk head pass-through systems from inside to outside the glovebox. These Deutsch connectors were custom fabricated with 316L stainless steel bodies, Viton A O-rings, aluminum 6061 with electroless nickel plating, Teflon (replacing the silicone), and gold crimp connectors (no soldering). Many of the Deutsch connectors may have been used in the Apollo program high vacuum complex in building 37 and date to about 1968 to 1970

Advanced Curation Activities at NASA: Preparing to Receive, Process, and Distribute Samples Returned from Future Missions

The Astromaterials Acquisition and Curation Office (henceforth referred to herein as NASA Curation Office) at NASA Johnson Space Center (JSC) is responsible for curating all of NASA's extraterrestrial samples. Under the governing document, NASA Policy Directive (NPD) 7100.10F JSC is charged with curation of all extraterrestrial material under NASA control, including future NASA missions. The Directive goes on to define Curation as including documentation, preservation, preparation, and distribution of samples for research, education, and public outreach. Here we briefly describe NASA's astromaterials collections and our ongoing efforts related to enhancing the utility of our current collections as well as our efforts to prepare for future sample return missions. We collectively refer to these efforts as advanced curation

Curating NASA's Past, Present, and Future Extraterrestrial Sample Collections

As codified in NASA Policy Directive 7100.10F, the Astromaterials Acquisition and Curation Office at NASA Johnson Space Center (hereafter JSC Curation) is charged with curation of all extraterrestrial material under NASA control, including future NASA missions. JSC Curation curates all or part of nine astromaterial collections in seven clean room suites: (1) Apollo Samples (1969; ISO 6-7), (2) Luna Samples (from USSR; 1972; ISO 7), (3) Antarctic Meteorites (1976; ISO 7), (4) Cosmic Dust (1981; ISO 5), (5) Microparticle Impact Collection (formerly called Space Exposed Hardware; 1985; ISO 5), (6) Genesis Solar Wind Atoms (2004; ISO 4); (7) Stardust Comet Particles (2006; ISO 5), (8) Stardust Interstellar Particles (2006; ISO 5), (9) Hayabusa Asteroid Particles (from JAXA; 2010; ISO 5). In addition to the labs that house the samples, we have installed and maintained a wide variety of facilities and infrastructure required to support the clean-rooms: more than 10 different HEPA-filtered air-handling systems, ultrapure dry gaseous nitrogen systems, an ultrapure water system (UPW) and cleaning facilities to provide clean tools and equipment for the labs. We also have sample preparation facilities for making thin sections, microtome sections, and even focused ion-beam (FIB) sections to meet the research requirements of scientists. To ensure that we are keeping the samples as pristine as possible, we routinely monitor the cleanliness of our clean rooms and infrastructure systems. This monitoring includes: daily monitoring of the quality of our UPW, weekly airborne particle counts in the labs, monthly monitoring of the stable isotope composition of the gaseous N2 system, and annual measurements of inorganic or organic contamination in processing cabinets. We track within our databases the current and ever-changing characteristics of more than 250,000 individual samples across our various collections (including the 19,141 samples on loan to 433 Principal Investigators in 24 countries). The next sample return missions that NASA will participate in are Hayabusa2 and OSIRIS-REx (Origins Spectral Interpretation Resource Identification Security - Regolith Explorer). The designs for a new state-of-the-art suite of clean rooms to house these samples at JSC have been finalized. This includes separate ISO class 5 clean rooms to house each collection, a common ISO class 7 area for general use, an ISO class 7 microtome laboratory, and a separate thin section lab. Additionally, a new cleaning facility is being designed and procedures developed that will allow for enhanced cleaning of cabinets and tools in an inorganically, organically, and biologically clean manner. We are also designing a large multi-purpose Advanced Curation laboratory that will allow us to develop the techniques necessary to fully support the Hayabusa2 and OSIRIS-REx missions, as well as future possible sample return missions (e.g., Lunar Polar Volatiles, Mars, Comet Surface). A micro-CT (micro Computed Tomography) laboratory dedicated to the study of astromaterials has come online within JSC Curation, and we plan to add additional facilities that will enable non-destructive (or minimally-destructive) analyses of astromaterials in the near future (e.g., micro-XRF (micro X-Ray Fluorescence), confocal imaging Raman Spectroscopy). These facilities will be available to: (1) develop sample handling and storage techniques for future sample return missions, (2) be utilized by PET (Positron Emission Tomography) for future sample return missions, (3) for retroactive PET-style analyses of our existing collections, and (4) for periodic assessments of the existing sample collections

Astromaterials Curation Online Resources for Principal Investigators

The Astromaterials Acquisition and Curation office at NASA Johnson Space Center curates all of NASA's extraterrestrial samples, the most extensive set of astromaterials samples available to the research community worldwide. The office allocates ~1500 individual samples to researchers and students each year and has served the planetary research community for 45+ years. The Astromaterials Curation office provides access to its sample data repository and digital resources to support the research needs of sample investigators and to aid in the selection and request of samples for scientific study. These resources can be found on the Astromaterials Acquisition and Curation website at https://curator.jsc.nasa.gov. To better serve our users, we have engaged in several activities to enhance the data available for astromaterials samples, to improve the accessibility and performance of the website, and to address user feedback. We havealso put plans in place for continuing improvements to our existing data products

Fieldpath Lunar Meteorite Graves Nunataks 06157, a Magnesian Piece of the Lunar Highlands Crust

To date, 49 feldspathic lunar meteorites (FLMs) have been recovered, likely representing a minimum of 35 different sample locations in the lunar highlands. The compositional variability among FLMs far exceeds the variability observed among highland samples in the Apollo and Luna sample suites. Here we will discuss in detail one of the compositional end members of the FLM suite, Graves Nunataks (GRA) 06157, which was collected by the 2006-2007 ANSMET field team. At 0.79 g, GRA 06157 is the smallest lunar meteorite so far recovered. Despite its small size, its highly feldspathic and highly magnesian composition are intriguing. Although preliminary bulk compositions have been reported, thus far no petrographic descriptions are in the literature. Here we expand upon the bulk compositional data, including major-element compositions, and provide a detailed petrographic description of GRA 06157

Compositional constraints on the launch pairing of three brecciated lunar meteorites of basaltic composition

Lunar meteorite EET 87/96 (paired stones Elephant Moraine 87521 and 96008) is a breccia consisting of fragments of a solidified, differentiated magma of basaltic composition. Small splits of the meteorite vary considerably in composition because they are heterogeneous mixtures of (1) a low-FeO differentiate with high Mg/Fe, high Cr/Sc, high Ca/Na, and low concentrations of incompatible elements and (2) a high-FeO differentiate with complimentary geochemical characteristics. Y79/98 (paired stones 793274 and 981031) and QUE (Queen Alexandra Range) 94281 are regolith breccias consisting of subequal proportions of material from the feldspathic highlands and fragments of mafic volcanic rock of mare-basalt-like composition. Previous studies have shown that (1) QUE 94281 and Y79/98 are very similar to each other and likely derive from the same source crater, (2) the texture and mineralogy of the volcanic components of all three meteorites are similar to each other yet distinct from mare basalts of the Apollo collection, and (3) all three meteorites were launched from the Moon at about the same time. We show that the volcanic component of Y79/98 and QUE 94281 are compositionally indistinguishable from a point on the EET 87/96 mixing line. Thus, there is no compositional impediment to the hypothesis that all three meteorites originate from the same place on the Moon and were launched by a single impact

Identification of New Lithic Clasts in Lunar Breccia 14305 by Micro-CT and Micro-XRF Analysis

From 1969 to 1972, Apollo astronauts collected 382 kg of rocks, soils, and core samples from six locations on the surface of the Moon. The samples were initially characterized, largely by binocular examination, in a custom-built facility at Johnson Space Center (JSC), and the samples have been curated at JSC ever since. Despite over 40 years of study, demand for samples remains high (~500 subsamples per year are allocated to scientists around the world), particularly for plutonic (e.g., anorthosites, norites, etc.) and evolved (e.g., granites, KREEP basalts) lithologies. The reason for the prolonged interest is that as new scientists and new techniques examine the samples, our understanding of how the Moon, Earth, and other inner Solar System bodies formed and evolved continues to grow. Scientists continually clamor for new samples to test their emerging hypotheses. Although all of the large Apollo samples that are igneous rocks have been classified, many Apollo samples are complex polymict breccias that have previously yielded large (cm-sized) igneous clasts. In this work we present the initial efforts to use the non-destructive techniques of micro-computed tomography (micro-CT) and micro x-ray fluorescence (micro-XRF) to identify large lithic clasts in Apollo 14 polymict breccia sample 14305. The sample in this study is 14305,483, a 150 g slab of regolith breccia 14305 measuring 10x6x2 cm (Figure 1a). The sample was scanned at the University of Texas High-Resolution X-ray CT Facility on an Xradia MicroXCT scanner. Two adjacent overlapping volumes were acquired at 49.2 micrometer resolution and stitched together, resulting in 1766 slices. Each volume was acquired at 100 kV accelerating voltage and 98 mA beam current with a 1 mm CaF2 filter, with 2161 views gathered over 360deg at 3 seconds acquisition time per view. Micro-XRF analyses were done at Washington University in St. Louis, Missouri on an EDAX Orbis PC micro-XRF instrument. Multiple scans were made at 40 kV accelerating voltage, 800 mA beam current, 30 m beam diameter, and a beam spacing of 30-120 micrometer. The micro-CT scan of 14305,483 (Figure 2) was able to identify several large lithic clasts (approx. 1 cm) within the interior of the slab. These clasts will be exposed by band-sawing or chipping of the slab, and their composition more fully characterized by subsequent micro-XRF analysis. In addition to lithic clasts, the micro-CT scans identified numerous mineral clasts, including many FeNi metal grains, as well as the prominent fractures within the slab. The micro-XRF analyses (Figure 1b,c) of the slab surfaces revealed the bulk chemical compositions (qualitative) of the different clast types observed. In particular, by looking at the ratios of major elements (e.g. Ca:Mg:Fe), differences among the many observed clast types are readily observed. Moreover, several clasts not apparent to the naked eye were revealed in the K:Al:Si ratio map. The scans are also able to identify small grains of Zr- and P-rich minerals (not shown), which could in turn yield important age dates for the samples

Applying Modern Analytical Techniques to the Apollo Samples: A Potential Model for Future Sample Return Missions

From 1969-1972 the Apollo missions collected 382 kg of lunar samples from six distinct locations on the Moon. Studies of the Apollo sample suite have shaped our understanding of the formation and early evolution of the Earth-Moon system, and have had important implications for studies of the other terrestrial planets (e.g., through the calibration of the crater counting record). Despite nearly 50 years of research on Apollo samples, scientists are still developing new theories about the origin and evolution of the Moon. In order to resolve these questions, scientists need access to new lunar samples, particularly new plutonic samples. Although no new large plutonic samples (i.e., hand-samples) remain to be discovered in the Apollo sample collection, there are many large polymict breccias in the Apollo collection containing relatively large (1 cm or larger) previously identified plutonic clasts, as well as a large number of unclassified lithic clasts. In addition, new, previously unidentified plutonic clasts are potentially discoverable within these breccias. The question becomes how to non-destructively locate and identify new lithic clasts of interest while minimizing the contamination and physical degradation of the samples