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NASA NTRS2017

Volatiles in High-K Lunar Basalts

Chlorine is an unusual isotopic system, being essentially unfractionated ((delta)Cl-37 approximately 0 per mille ) between bulk terrestrial samples and chondritic meteorites and yet showing large variations in lunar (approximately -4 to +81 per mille), martian, and vestan (HED) samples. Among lunar samples, the volatile-bearing mineral apatite (Ca5(PO4)3[F,Cl,OH]) has been studied for volatiles in K-, REE-, and P (KREEP), very high potassium (VHK), low-Ti and high-Ti basalts, as well as samples from the lunar highlands. These studies revealed a positive correlation between in-situ (delta)Cl-37 measurements and bulk incompatible trace elements (ITEs) and ratios. Such trends were interpreted to originate from Cl isotopic fractionation during the degassing of metal chlorides during or shortly after the differentiation of the Moon via a magma ocean. In this study, we investigate the volatile inventories of a group of samples for which new-era volatile data have yet to be reported - the high-K (greater than 2000 ppm bulk K2O), high-Ti, trace element-rich mare basalts. We used isotope imaging on the Cameca NanoSIMS 50L at JSC to obtain the Cl isotopic composition [((Cl-37/(35)Clsample/C-37l/(35)Clstandard)-1)×1000, to get a value in per thousand (per mille)] which ranges from approximately -2.7 +/- 2 per mille to +16.1 +/- 2 per mille (2sigma), as well as volatile abundances (F & Cl) of apatite in samples 10017, 10024 & 10049. Simply following prior models, as lunar rocks with high bulk-rock abundances of ITEs we might expect the high-K, high-Ti basalts to contain apatite characterized by heavily fractionated (delta)Cl-37 values, i.e., Cl obtained from mixing between unfractionated mantle Cl (approximately 0 per mille) and the urKREEP reservoir (possibly fractionated to greater than +25 per mille.). However, the data obtained for the studied samples do not conform to either the early degassing or mixing models. Existing petrogentic models for the origin of the high-K, high-Ti basalts do not include urKREEP assimilation into their LMO cumulate sources. Therefore, Cl in these basalts either originated from source region heterogeneity or through assimilation or metasomatism by volatile and incompatible trace element rich materials. The new data presented here could provide evidence for the existence of region(s) in the lunar interior that are ITE-enriched and contain Cl that does not share isotopic affinities with lunar urKREEP, possibly representing the composition of the purported 'neuKREEP'.

Barnes, Jessica J.↗
NASA NTRS2017

Multiple Nebular Gas Reservoirs Recorded by Oxygen Isotope Variation in a Spinel-rich CAI in CO3 MIL 090019

We conducted NanoSIMS O-isotopic imaging of a primitive spinel-rich CAI spherule (27-2) from the MIL 090019 CO3 chondrite. Inclusions such as 27-2 are proposed to record inner nebula processes during an epoch of rapid solar nebula evolution. Mineralogical and textural analyses suggest that this CAI formed by high temperature reactions, partial melting, and condensation. This CAI exhibits radial O-isotopic heterogeneity among multiple occurrences of the same mineral, reflecting interactions with distinct nebular O-isotopic reservoirs.

Simon, J. I.↗
NASA NTRS2017

Microstructural Study of an 18-O-Poor Presolar Silicate Grain from The Meteorite Hills 00426 Cr2 Chondrite

The majority of presolar silicate and oxide grains derive from low-mass red giant and asymptotic giant branch (AGB) stars of approximately solar metallicity (Z). A small subclass of presolar O-rich grains (less than 7%) is thought to originate from stars having lower-than-solar Z. These "Group 3" [1] grains have depletions in 18O and 17O that typically fall along or above the Galactic chemical evolution (GCE) line. Other Group 3 grains show greater 17O than 18O depletions and most likely have supernova (SN) origins. Owing to their rarity, only two Group 3 silicates have been mineralogically examined in detail [2, 3]. Here we present a mineralogical study of a Group 3 presolar silicate to explore its formation conditions and interstellar history.

Nguyen, A. N.↗
NASA NTRS2017

PHYS: Division of Physical Chemistry 258 - Properties and Origins of Cometary and Asteroidal Organic Matter Delivered to the Early Earth

Comets and asteroids may have contributed much of the Earth's water and organic matter. The Earth accretes approximately 4x10(exp 7) Kg of dust and meteorites from these sources every year. The least altered meteorites contain complex assemblages of organic compounds and abundant hydrated minerals. These carbonaceous chondrite meteorites probably derive from asteroids that underwent hydrothermal processing within the first few million years after their accretion. Meteorite organics show isotopic and chemical signatures of low-T ion-molecule and grain-surface chemistry and photolysis of icy grains that occurred in cold molecular clouds and the outer protoplanetary disk. These signatures have been overprinted by aqueously mediated chemistry in asteroid parent bodies, forming amino acids and other prebiotic molecules. Comets are much richer in organic matter but it is less well characterized. Comet dust collected in the stratosphere shows larger H and N isotopic anomalies than most meteorites, suggesting better preservation of primordial organics. Rosetta studies of comet 67P coma dust find complex organic matter that may be related to the macromolecular material that dominates the organic inventory of primitive meteorites. The exogenous organic material accreting on Earth throughout its history is made up of thousands of molecular species formed in diverse processes ranging from circumstellar outflows to chemistry at near absolute zero in dark cloud cores and the formative environment within minor planets. NASA and JAXA are currently flying sample return missions to primitive, potentially organic-rich asteroids. The OSIRIS-REx and Hayabusa2 missions will map their target asteroids, Bennu and Ryugu, in detail and return regolith samples to Earth. Laboratory analyses of these pristine asteroid samples will provide unprecedented views of asteroidal organic matter relatively free of terrestrial contamination within well determined geological context. Studies of extraterrestrial materials and returned samples are essential to understand the origins of Solar System organic material and the roles of comets and asteroids to providing the starting materials for the emergence of life.

Messenger, Scott↗
NASA NTRS2017

OSIRIS-REx Asterod Sample Return Mission

OSIRIS-REx is NASA's third New Frontiers Program mission, following New Horizons that completed a flyby of Pluto in 2015 and the Juno mission to Jupiter that has just begun science operations. The OSIRIS-REx mission's primary objective is to collect pristine surface samples of a carbonaceous asteroid and return to Earth for analysis. Carbonaceous asteroids and comets are 'primitive' bodies that preserved remnants of the Solar System starting materials and through their study scientists can learn about the origin and the earliest evolution of the Solar System. The OSIRIS-REx spacecraft was successfully launched on September 8, 2016, beginning its seven year journey to asteroid 101955 Bennu. The robotic arm will collect 60-2000 grams of material from the surface of Bennu and will return to Earth in 2023 for worldwide distribution by the Astromaterials Curation Facility at NASA Johnson Space Center. The name OSIRIS-REx embodies the mission objectives (1) Origins: Return and analyze a sample of a carbonaceous asteroid, (2) Spectral Interpretation: Provide ground-truth for remote observation of asteroids, (3) Resource Identification: Determine the mineral and chemical makeup of a near-Earth asteroid (4) Security: Measure the non-gravitational that changes asteroidal orbits and (5) Regolith Explorer: Determine the properties of the material covering an asteroid surface. Asteroid Bennu may preserve remnants of stardust, interstellar materials and the first solids to form in the Solar System and the molecular precursors to the origin of life and the Earth's oceans. Bennu is a potentially hazardous asteroid, with an approximately 1 in 2700 chance of impacting the Earth late in the 22nd century. OSIRIS-REx collects from Bennu will help formulate the types of operations and identify mission activities that astronauts will perform during their expeditions. Such information is crucial in preparing for humanity's next steps beyond low Earthy orbit and on to deep space destinations.

Nakamura-Messinger, Keiki↗
NASA NTRS2017

Osiris-REx Spacecraft Current Status and Forward Plans

The NASA New Frontiers OSIRIS-REx spacecraft executed a flawless launch on September 8, 2016 to begin its 23-month journey to near-Earth asteroid (101955). The primary objective of the OSIRIS-REx mission is to collect and return to Earth a pristine sample of regolith from the asteroid surface. The sampling event will occur after a two-year period of remote sensing that will ensure a high probability of successful sampling of a region on the asteroid surface having high science value and within well-defined geological context. The OSIRIS-REx instrument payload includes three high-resolution cameras (OCAMS), a visible and near-infrared spectrometer (OVIRS), a thermal imaging spectrometer (OTES), an X-ray imaging spectrometer (REXIS), and a laser altimeter (OLA). As the spacecraft follows its nominal outbound-cruise trajectory, the propulsion, power, communications, and science instruments have undergone basic functional tests, with no major issues. Outbound cruise science investigations include a search for Earth Trojan asteroids as the spacecraft approaches the Sun-Earth L4 Lagrangian point in February 2017. Additional instrument checkouts and calibrations will be carried out during the Earth gravity assist maneuver in September 2017. During the Earth-moon flyby, visual and spectral images will be acquired to validate instrument command sequences planned for Bennu remote sensing. The asteroid Bennu remote sensing campaign will yield high resolution maps of the temperature and thermal inertia, distributions of major minerals and concentrations of organic matter across the asteroid surface. A high resolution 3d shape model including local surface slopes and a high-resolution gravity field will also be determined. Together, these data will be used to generate four separate maps that will be used to select the sampling site(s). The Safety map will identify hazardous and safe operational regions on the asteroid surface. The Deliverability map will quantify the accuracy with which the navigation team can deliver the spacecraft to and from specific sites on the asteroid surface. The Sampleability map quantifies the regolith properties, providing an estimation of how much material would be sampled at different points on the surface. The final Science Value map synthesizes the chemical, mineralogical, and geological, observations to identify the areas of the asteroid surface with the highest science value. Here, priority is given to organic, water-rich regions that have been minimally altered by surface processes. Asteroid surface samples will be acquired with a touch-and-go sample acquisition system (TAGSAM) that uses high purity pressurized N2 gas to mobilize regolith into a stainless steel canister. Although the mission requirement is to collect at least 60 g of material, tests of the TAGSAM routinely exceeded 300 g of simulant in micro-gravity tests. After acquiring the sample, the spacecraft will depart Bennu in 2021 to begin its return journey, with the sample return capsule landing at the Utah Test and Training Range on September 23, 2023. The OSIRIS-REx science team will carry out a series of detailed chemical, mineralogical, isotopic, and spectral studies that will be used to determine the origin and history of Bennu and to relate high spatial resolution sample studies to the global geological context from remote sensing. The outline of the sample analysis plan is described in a companion abstract.

Messenger, Scott↗
NASA NTRS2017

NASA Curation Preparation for Ryugu Sample Returned by JAXA's Hayabusa2 Mission

The NASA OSIRIS-REx and JAXA Hayabusa2 missions to near-Earth asteroids Bennu and Ryugu share similar mission goals of understanding the origins of primitive, organic-rich asteroids. Under an agreement between JAXA and NASA, there is an on-going and productive collaboration between science teams of Hayabusa2 and OSIRIS-REx missions. Under this agreement, a portion of each of the returned sample masses will be exchanged between the agencies and the scientific results of their study will be shared. NASA’s portion of the returned Hayabusa2 sample, consisting of 10% of the returned mass, will be jointly separated by NASA and JAXA. The sample will be legally and physically transferred to NASA’s dedicated Hayabusa2 curation facility at Johnson Space Center (JSC) no later than one year after the return of the Hayabusa2 sample to Earth (December 2020). The JSC Hayabusa2 curation cleanroom facility design has now been completed. In the same manner, JAXA will receive 0.5% of the total returned OSIRIS-REx sample (minimum required sample to return 60 g, maximum sample return capacity of 2 kg) from the rest of the specimen. No later than one year after the return of the OSIRIS-REx sample to Earth (September 2023), legal, physical, and permanent custody of this sample subset will be transferred to JAXA, and the sample subset will be brought to JAXA’s Extraterrestrial Sample Curation Center (ESCuC) at Institute of Space and Astronautical Science, Sagamihara City Japan.

Nakamura-Messenger, Keiko↗
NASA NTRS2017

Sample Curation in Support of the OSIRIS-REx Asteroid Sample Return Mission

The OSIRIS-REx asteroid sample return mission launched to asteroid Bennu Sept. 8, 2016. The spacecraft will arrive at Bennu in late 2019, orbit and map the asteroid, and perform a touch and go (TAG) sampling maneuver in July 2020. After sample is stowed and confirmed the spacecraft will return to Earth, and the sample return capsule (SRC) will land in Utah in September 2023. Samples will be recovered from Utah [2] and then transported and stored in a new sample cleanroom at NASA Johnson Space Center in Houston [3]. The materials curated for the mission are described here. a) Materials Archive and Witness Plate Collection: The SRC and TAGSAM were built between March 2014 and Summer of 2015, and instruments (OTES,OVIRS, OLA, OCAMS, REXIS) were integrated from Summer 2015 until May 2016. A total of 395 items were received for the materials archive at NASA-JSC, with archiving finishing ~30 days after launch (with the final archived items being related to launch operations)[4]. The materials fall into several general categories including metals (stainless steel, aluminum, titanium alloys, brass and BeCu alloy), epoxies, paints, polymers, lubricants, non-volatile-residue samples (NVR), sapphire, and various miscellaneous materials. All through the ATLO process (from March 2015 until late August 2016) contamination knowledge witness plates (Si wafer and Al foil) were deployed in the various cleanrooms in Denver and KSC to provide an additional record of particle counts and volatiles that is archived for current and future scientific studies. These plates were deployed in roughly monthly increments with each unit containing 4 Si wafers and 4 Al foils. We archived 128 individual witness plates (64 Si wafers and 64 Al foils); one of each witness plate (Si and Al) was analyzed immediately by the science team after archiving, while the remaining 3 of each are archived indefinitely. Information about each material archived is stored in an extensive database at NASA-JSC, and key summary information for each will be presented in an online catalog. b) Bulk Asteroid sample: The Touch and Go Sampling Mechanism (TAGSAM) head will contain up to 1.5 kg of asteroid material. Upon return to Earth, the TAGSAM head with the sample canister will be subjected to a nitrogen purge and then opened in a nitrogen cabinet in Houston. Once the TAGSAM head is removed from the canister, it will be dis-assembled slowly and carefully under nitrogen until the sample can be removed for processing in a dedicated nitrogen glovebox. Bennu surface samples are expected to be sub-cm sized, based on thermal infrared and radar polarization ratio measurements [1]. The upper limit on material collected by the TAGSAM head is ~2 cm. Therefore, we will be prepared to handle, subdivide, and characterize materials of a wide grain size (from ~10 m to 2 cm), and for both organic (UV fluorescence) and inorganic (SEM, FTIR, optical) properties. Representative portions of the bulk sample will be prepared for JAXA (0.5 %; see also [5]) and Canadian Space Agency (4%), with the remaining divided between the science team (<25%) and archived for future studies (NASA) (>75%). c) Contact Pad samples: The base of the TAGSAM head contains 24 contact pads that are designed to trap the upper surface layer of material and thus offer an opportunity to study asteroid samples that have resided at the very top surface of the regolith. Asteroid material is trapped on the pads in spring steel Velcro hooks, and material will have to be removed from these pads by curation specialists in the lab. d) Hardware: Some canister and SRC hardware items will contain information that will be important to understanding the collected samples, including the canister gas filter, temperature strips, flight witness plates, and the TAGSAM and canister parts that might have adhering dust grains. Some challenges remaining for both bulk sample and contact pad samples include: i) working with intermediate size range (200 to 500 micron) samples - a size range NASA has not previously worked in such detail; ii) techniques for removal of contact pad material from the spring steel hooks, iii) static electrical effects of dust sized particles during sample handling and curation is likely to be significant, and iv) the TAGSAM head and associated canister hardware will undoubtedly be coated with fine adhering dust grains from Bennu. In the case of collection of a large bulk sample mass, the adhering dust grains may be of lower priority. If a small sample mass is returned, the adhering dust may attain a higher priority, so recovery of adhering dust grains is an additional challenge to consider. In the year leading up to sample return we plan a variety of sample handling rehearsals that will enables the curation team to be prepared for many new aspects posed by this sample suite.

Righter, Kevin↗
NASA NTRS2018

Osiris-Rex and Hayabusa2 Sample Cleanroom Design and Construction Planning at NASA-JSC

Final Paper and not the abstract is attached. The OSIRIS-REx asteroid sample return mission launched to asteroid Bennu September 8, 2016. The spacecraft will arrive at Bennu in late 2019, orbit and map the asteroid, and perform a touch and go (TAG) sampling maneuver in July 2020. After confirma-tion of successful sample stowage, the spacecraft will return to Earth, and the sample return capsule (SRC) will land in Utah in September 2023. Samples will be recovered from Utah and then transported and stored in a new sample cleanroom at NASA Johnson Space Center in Houston. All curation-specific ex-amination and documentation activities related to Ben-nu samples will be conducted in the dedicated OSIRIS-REx sample cleanroom to be built at NASA-JSC.

Righter, Kevin↗
NASA NTRS2018

Advances in Small Particle Handling of Astromaterials in Preparation for OSIRIS-REx and Hayabusa2: Initial Developments

The Astromaterials Acquisition and Curation office at NASA Johnson Space Center has established an Advanced Curation program that is tasked with developing procedures, technologies, and data sets necessary for the curation of future astromaterials collections as envisioned by NASA exploration goals. One particular objective of the Advanced Curation program is the development of new methods for the collection, storage, handling and characterization of small (less than 100 micrometer) particles. Astromaterials Curation currently maintains four small particle collections: Cosmic Dust that has been collected in Earth's stratosphere by ER2 and WB-57 aircraft, Comet 81P/Wild 2 dust returned by NASA's Stardust spacecraft, interstellar dust that was returned by Stardust, and asteroid Itokawa particles that were returned by the JAXA's Hayabusa spacecraft. NASA Curation is currently preparing for the anticipated return of two new astromaterials collections - asteroid Ryugu regolith to be collected by Hayabusa2 spacecraft in 2021 (samples will be provided by JAXA as part of an international agreement), and asteroid Bennu regolith to be collected by the OSIRIS-REx spacecraft and returned in 2023. A substantial portion of these returned samples are expected to consist of small particle components, and mission requirements necessitate the development of new processing tools and methods in order to maximize the scientific yield from these valuable acquisitions. Here we describe initial progress towards the development of applicable sample handling methods for the successful curation of future small particle collections.

Snead, C. J.↗
NASA NTRS2018

The CAESAR New Frontiers Comet Sample Return Mission

The Comet Astrobiology Exploration Sample Return (CAESAR) mission is one of two finalists selected by NASA for Phase A study in the New Frontiers program. CAESAR will acquire a minimum of 80 grams of material from the surface of comet 67P/Churuyumov-Gerasimenko and return it to Earth for laboratory analysis. CAESAR preserves much of the science of a cryogenic sample return by retaining volatiles in a dedicated reservoir securely separated from the solid sample. Comet 67P was selected based on its favorable orbital geometry and the risk reduction and scientific context provided by the ESA (European Space Agency)'s Rosetta mission. CAESAR's objectives are to understand the origins of the Solar System starting materials and how these components came together to form planets and give rise to life. We also seek to resolve the conflicting views of comet origins arising from the Stardust and Rosetta missions. While the greater than 1 micron solids returned by Stardust originated in the hot, inner solar nebula, measurements by Rosetta suggest 67P volatiles formed at cryogenic temperatures and remained unchanged for billions of years. This dichotomy provides the rationale for returning both solid and gaseous samples.

CAESAR New Frontiers↗
NASA NTRS2018

Precious Dust Two Mission Converge on Asteroid Sample Returns

Far-flung spacecraft deliver incredible views of distant worlds. But there's nothing like bringing samples back to Earth. Instruments carried by spacecraft have limitations-of power, complexity, size, and number. Their investigations leave many fundamental questions unanswered, questions that we might be able to answer if only we had samples. This summer marks the beginning of an exciting new era in sample-return missions: NASA's OSIRIS-REx spacecraft arrives at asteroid Bennu, and the Japanese Hayabusa2 spacecraft arrives at asteroid Ryugu. Both are primitive asteroids-dark remnants of Solar System formation that carry carbon and water-a type of asteroid that's never been visited before. After thoroughly mapping their respective asteroids for geology and mineralogy, each probe will collect surface samples and return them to Earth. I can't wait to study them in my laboratory. Cosmic-dust pioneer Kazu Tomeoka introduced me to the dream of sample-return missions 20 years ago. In those days, the only returned extraterrestrial samples were from the Moon. He said to his students, "In the near future, we will be able to collect samples from asteroids and comets. There will be no need to wait for meteorites or cosmic dust to come and fall from the sky. And some of you might be the first to look at those samples." This inspired my life's work: laboratory analysis of returned astromaterials.

Nakamura-Messenger, Keiko↗
NASA NTRS2018

Coordinated Microanalysis of Phosphates in High-Titanium Lunar Basalts

Laboratory studies of lunar apatite [Ca5(PO4)3(F,Cl,OH)] have been important for determining the volatile inventory of the interior and the roles volatiles played during the magmatic evolution of the Moon. It has been suggested that high-Ti mare basalts sample volatiles from a distinct reservoir in the lunar mantle. However, there is still debate surrounding the crystallization and post-crystallization history of apatite in those basalts. This information is required before we can use apatite to characterize the abundance or isotopic composition of volatiles in melts or magmatic source regions. Our goal is to investigate the mineral chemistry, crystal structure, and volatile inventory of phosphates in high-Ti basalts from Apollo 11, which will allow us to determine the crystallization history of apatite in these rocks and identify any potential secondary processes that have changed the volatile composition that apatite acquired from the melt.

Barnes, J. J.↗
NASA NTRS2018

Coordinated Analysis of Organic Matter in Primitive Meteorites

Carbonaceous chondrites (CC) preserve a diverse range of organic matter formed within cold interstellar environments, the solar nebula, and during subsequent parent body asteroidal processing. This organic matter maintains a unique geochemical and istopic record of organic evolution [1-4]. Bulk studies of organics within CC have revealed a complex array of organic species. However, bulk studies invariably involve solvent extraction, resulting in a loss of spatial context of the host mineral matrix [3, 5]. Correlated in situ chemical and isotopic studies suggest preservation of interstellar organics in the form of spherical, often hollow, micrometer sized organic nano-globules. Nanoglobules often exhibit significant delta 15N and delta D enrichments that imply formation through fractionation of ion-molecule reactions within cold molecular clouds and/or the outer protoplanetary disk [5]. In situ studies such as 6-8 are necessary to understand the organic evolutionary stages of nanoglobules and other components in the nebula and parent body [7]. We carried out coordinated in situ micrometer-scale chemical, mineralogical and isotopic studies of the Murchison (CM2), QUE 99177 (CR3), and Tagish Lake (C2 Ung) CC. These studies were performed using fluorescent microscopy, two-step laser mass spectrometry (microL2MS), NanoSIMS, and Scanning Electron Microscopy (SEM) with Energy Dispersive X-Ray Spectroscopy (EDX). Comparative analysis of three different meteorites will help reveal the effects of parent body processes on the chemistry and isotopic composition of organic matter.

meteorites↗
NASA NTRS2019

In Situ Coordinated Analysis of Carbonaceous Chondrite Organic Matter

Microanalytical studies of carbonaceous chondrites (CC’s) have identified a vast array of isotopically, chemically and texturally distinct organic components. These components were synthesized and processed within a range of physical and chemical environments, including the interstellar medium, the solar nebula and within asteroids. The nature and abundance of these molecules can be used to unravel the geochemical and isotopic record of their origins as well as their subsequent evolutionary journey.

Nevill, N. D.↗
NASA NTRS2018

Novel Applications of Focused Ion Beam Technique for Planetary Sample Analyses

We are using innovative FIB techniques to prepare samples of planetary materials for different types of coordinated analyses using ion microprobes, synchrotron beamlines, and specialized transmission electron microscopy (TEM) techniques. In these cases, the FIB sample preparation is the critical step in enabling these specialized analyses. We discuss several examples below utilizing the FEI Quanta3D instrument at the NASA Johnson Space Center. Trace element analyses utilizing synchrotron x-ray fluorescence. The trace element content of mineral grains in comet dust provides important clues on their formation and processing in the early solar system. We preformed coordinated analyses of a comet dust particle that had been prepared using ultramicrotomy for TEM analysis. Following the TEM analyses, we extracted a 70 nm thick section from a region of the carbon (C) film of the TEM grid, for additional analyses. A carbon ring ~2-3 μm thick was deposited on top of the C film using the FIB. The C film on the outer rim of the ring was milled away using various patterns to uniformly release the stresses on the film, preventing rupture and collapse, and was attached to the micromanipulator needle. We then isolated the ring completely and transferred the section to a silicon sample holder for analysis using the HXN (hard X-ray nanoprobe) beamline at NSLSII at Brookhaven National Lab. Coordinated Analyses of Presolar Grains. Rare sub-m presolar grains that originate in evolved stars and supernovae, occur in primitive astromaterials and are identified by their exotic isotopic compositions. Coordinated analyses of these grains using NanoSIMS, TEM, and other techniques on the same grain is enabled by innovative FIB sample preparation. In order to obtain subsequent isotopic analyses of Mg and Fe, contributions from surrounding grains were minimized. We precisely deposited a protective cap of Pt on top of the grain to preserve the grain of interest and then milled away about 5 μm diameter of the surrounding material. Following the isotopic analyses, the spindle was extracted and thinned to electron transparency for TEM microstructural analyses. In situ heating TEM experiments on lunar samples. We extracted a FIB thin section from Apollo 17 lunar rock 76015. To avoid ion-beam damage, e-beam deposition was used to deposit the first 500 nm of the C strap, followed by ion beam-assisted deposition of ~3 μm carbon. We performed an ex situ lift-out of the section and placed the section on one of the elements of a microelectromechanical systems (MEMS) - specialized heating substrate and attached the section to the substrate by depositing small C straps with the FIB. The heating chips utilize silicon nitride windows to support the samples and provide uniform heating while enabling TEM imaging. The heating chip was loaded into a Hitachi “Blaze” heating holder and analyzed using a Hitachi HF5000 at the University of Arizona.

Rahman, Z.↗
NASA NTRS2018

Water-Rock Interactions in Outer Solar System Bodies: Evidence from the Coordinated Analysis of Interplanetary Dust

NASA has an ongoing program of collecting interplanetary dust particles (IDPs) in the stratosphere using high altitude research aircraft. The collected IDPs are derived from asteroids and comets and here we report studies of a subset of hydrated IDPs rich in carbonaceous matter that are proposed to have a cometary origin. Our studies are aimed at understanding the evolution of oxygen reservoirs in the Solar System and their interaction with cometary minerals and organic matter. The small size (<20 μm) and fragility of these IDPs present a number of analytical challenges. We have pioneered techniques for performing chemical, mineralogical, isotopic, and spectroscopic measurements on the same sample in a carefully coordinated sequence. Coordinated analyses of nanogram-size samples is made possible by several delicate sample preparation techniques. To avoid organic contamination, we embed IDPs in elemental sulfur and use ultramicrotomy to partly section the particles (the first few micrometers). Multiple thin sections (50-70 nm thick) are placed on different substrates depending on the analysis technique. We use a JEOL 2500SE scanning, transmission electron microscope (STEM) to determine the mineralogy, microstructure, and elemental compositions of constituent minerals in the thin sections through a combination of high resolution imaging, electron diffraction, quantitative energy-dispersive x-ray mapping, and electron energy-loss spectroscopy. Following the STEM analyses, we use a NanoSIMS 50L for high spatial resolution isotopic measurements of H, C, N, and O to search for presolar grains and to understand the origin of the indigenous organic matter. The isotopic analyses are performed on the same sections analyzed in the STEM in order to correlate isotopic properties with the elemental and mineralogical data. We reserve other thin sections for non-destructive analyses utilizing synchrotron-based techniques including Fourier-transform infrared (FTIR) micro-spectroscopy and X-ray absorption near-edge structure (XANES) analyses, especially for functional group analysis of organic matter in the particles. The remainder of the IDP is extracted from the sulfur bead that was used for microtomy and is pressed into Au foil for quantitative analysis (including light elements) using a JEOL 8530F field emission electron probe microanalyzer (EPMA). After the EPMA measurements, high precision oxygen isotopic analyses are obtained using Cameca IMS1270/1290 instruments at UCLA. The hydrated IDPs in this study are dominated by saponitic clays, with minor magnetite, carbonate and abundant organic matter. The remarkable oxygen isotopic compositions, high carbon contents, and the abundance of isotopically anomalous organic matter, together suggest that the high carbon, hydrated IDPs are derived from primitive sources not yet represented in meteorite collections such as outer main belt P- and D-type asteroids or comets.

Keller, Lindsay P.↗