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NASA NTRS2004

Preliminary Sample Analysis Plan for the Cometary and Interstellar Samples Being Returned by the Stardust Spacecraft

The NASA Stardust comet sample return mission is proceeding very well, and the science team breathed a collective sigh of relief following the successful comet sample collection phase which occurred during a 6.1 km/s, 340km-close flyby of comet Wild-2 on Jan 2 of this year. Multiple images of the comet nucleus were obtained and a variety of onboard instruments returned in situ data on the spatial distribution, particle size frequency and composition of the dust in the comet s coma. These data are currently being processed and analyzed. It is expected that 500-1000 comet particles >15 m were collected by impact into low density silica aerogel, as well as many more smaller grains. Previous tests with hypervelocity guns firing small particles into aerogel indicate that material should have successfully been collected by the Stardust aerogel [1&2]. In addition, many (~100) grains of interstellar material newly entering the Solar System should have been collected by the spacecraft during its cruise phase to the comet.

Zolensky, M.↗
NASA NTRS2008

Transmission Electron Microscopy of Cometary Residues from Micron-Sized Craters in the Stardust Al-Foils

We report Transmission Electron Microscopy (TEM) investigations of micro-craters that originated from hypervelocity impacts of comet 81P/Wild 2 dust particles on the aluminium foil of the Stardust collector. The craters were selected by Scanning Electron Microscopy (SEM) and then prepared by Focused Ion Beam (FIB) milling techniques in order to provide electron transparent cross-sections for TEM studies. The crater residues contain both amorphous and crystalline materials in varying proportions and compositions. The amorphous component is interpreted as resulting from shock melting during the impact and the crystalline phases as relict minerals. The latter show evidence for shock metamorphism. Based on the residue morphology and the compositional variation, the impacting particles are inferred to have been dominated by mixtures of submicron olivine, pyroxene and Fe-sulfide grains, in agreement with prior results of relatively coarse-grained mineral assemblages in the aerogel collector.

Leroux, Hugues↗
NASA NTRS2009

Detection of Cometary Amines in Samples Returned by the Stardust Spacecraft

The delivery of amino acids to the early Earth by comets and their fragments could have been a significant source of the early Earth's prebiotic organic inventory that led to the emergence of life (Chyba and Sagan, 1992). Over 20 organic molecules including methane, ethane, ammonia, cyanic acid, formaldehyde, formamide, acetaldehyde, acetonitrile, and methanol have been identified by radio spectroscopic observations of the comae of comets Hale-Bopp and Hyakutake (Crovisier et al. 2004). These simple molecules could have provided the organic reservoir to allow the formation of more complex prebiotic organic compounds such as amino acids. After a 7-year mission, the Stardust spacecraft returned to Earth samples from comet Wild 2 on January 15, 2006 providing the opportunity to analyze the organic composition and isotopic distribution of cometary material with state-of-the-art laboratory instrumentation. The Preliminary Examination Team analyses of organics in samples returned by Stardust were largely focused on particles that impacted the collector aerogel and aluminum foil (Sandford et al. 2006). However, it is also possible that Stardust returned a "diffuse" sample of gas-phase organic molecules that struck the aerogel directly or diffused away from the grains after impact. To test this possibility, samples of Stardust flight aerogel and foil were carried through a hot water extraction and acid hydrolysis procedure to see if primary amine compounds were present in excess of those seen in controls. Here we report highly sensitive liquid chromatography time-of-flight mass spectrometry measurements of amino acids and amines in samples returned from a comet (Glavin et al. 2008). A suite of amino acids and amines including glycine, L-alanine, methylamine (MA), and ethylamine (EA) were identified in the Stardust bulk aerogel. With the exception of MA and EA, all other primary amines detected in comet-exposed aerogels were also present in the aerogel witness tile that was not exposed to Wild 2, suggesting that most amines are terrestrial in origin. However, the enhanced abundances of MA, EA, and possibly glycine in comet-exposed aerogel compared to controls, coupled with MA to EA ratios (1 to 2) that are distinct from preflight aerogels (7 to 10), suggest that these amines were captured from Wild 2. It is possible that MA and EA were formed on energetically processed icy grains containing methane, ethane, and ammonia. The presence of cometary amines in Stardust material supports the hypothesis that comets were an important source of prebiotic organics on the early Earth. To better understand their origin, a systematic compound specific carbon isotopic analysis (C-CSIA) via gas chromatography quadrupole mass spectrometry in with parallel with combustion isotope ratio mass spectrometry (GCQMS/ IRMS) is being conducted. We will discuss our latest C-CSIA measurements and what they indicate about the origin of amino acids extracted from Stardust samples.

Glavin, Daniel P.↗
NASA NTRS2010

Detection of Cometary Amines in Samples Returned by the Stardust Spacecraft

The delivery of amino acids to the early Earth by comets and their fragments could have been a significant source of the early Earth's prebiotic organic inventory that led to the emergence of life (Chyba and Sagan, 1992). Over 20 organic molecules including methane, ethane, ammonia, cyanic acid, formaldehyde, formamide, acetaldehyde, acetonitrile, and methanol have been identified by radio spectroscopic observations of the comae of comets Hale-Bopp and Hyakutake (Crovisier et al. 2004). These simple molecules could have provided the organic reservoir to allow the forn1ation of more complex prebiotic organic compounds such as amino acids. After a 7 -year mission, the Stardust spacecraft returned to Earth samples from comet Wild 2 on January 15, 2006 providing the opportunity to analyze the organic composition and isotopic distribution of cometary material with state-of-the-art laboratory instrun1entation. The Preliminary Examination Team analyses of organics in samples returned by Stardust were largely focused on particles that impacted the collector aerogel and aluminum foil (Sandford et al. 2006). However, it is also possible that Stardust returned a "diffuse" sample of gas-phase organic molecules that struck the aerogel directly or diffused away from the grains after impact. To test this possibility, samples of Stardust flight aerogel and foil were carried through a hot water extraction and acid hydrolysis procedure to see if primary amine compounds were present in excess of those seen in controls. Here we report highly sensitive liquid chromatography time-of-flight mass spectron1etry measurements of amino acids and amines in samples returned from a comet (Glavin et al. 2008). A suite of amino acids and amines including glycine, L-alanine, methylamine (MA), and ethylamine (EA) were identified in the Stardust bulk aerogel. With the exception of MA and EA, all other primary amines detected in comet-exposed aerogels were also present in the aerogel witness tile that was not exposed to Wild 2, suggesting that most amines are terrestrial in origin. However, the enhanced abundances of MA, EA, and possibly glycine in comet-exposed aerogel compared to controls, coupled with MA to EA ratios (1 to 2) that are distinct from preflight aerogels (7 to 10), suggest that these amines were captured from Wild 2. It is possible that MA and EA were formed on energetically processed icy grains containing methane, ethane, and ammonia. The presence of cometary amines in Stardust material supports the hypothesis that comets were an important source of pre biotic organics on the early Earth. To better understand their origin, a systematic compound specific carbon isotopic analysis (C-CSIA) via gas chromatography quadrupole mass spectrometry in with parallel with combustion isotope ratio mass spectrometry (GC-QMS/IRMS) is being conducted. We will discuss our latest C-CSIA measurements and what they indicate about the origin of amino acids extracted from Stardust samples.

Glavin, Daniel P.↗
NASA NTRS1996

Interplanetary and Interstellar Dust Particles: Reentry Heating and Capture in Aerogel

Studies of interplanetary and interstellar dust can provide significant information on the evolution of the solar system or stars, respectively. However, for reliable analysis it is crucial to know how the particles have been modified during reentry (in the case of interplanetary dust particles, or [DP's) and impact into the capture medium. In the case of stratospheric capture, particles will be heated by atmospheric drag. Subsequent capture of the particles will result in heating, ablation, accretion of the capture medium and possible fragmentation. Modeling of these processes is a useful way of assessing their effects on the interpretation of the compositional data for these particles. Previous work on reentry heating has shown that heat diffusion alone cannot adequately account for temperature gradients observed in IDP's. In fact, for any reasonable thermal parameters, calculations show the particles to be nearly isothermal. Here we extend those studies to include phase transitions. These preliminary results are promising and show a significant temperature gradient for a 100 micron (diameter) particle. The actual capture of the particles in silica aerogel is being modeled using a comprehensive shock hydrodynamic code (called CTH). Various options of this code were investigated to attempt to make the most appropriate choice of methods of impact, equations of state, and processes of energy transfer from capture material to particle. The initial calculations with the code used only 'reasonable' estimates for the physical parameters of silica aerogel. Through the literature searches and personal contacts with the knowledgeable scientists, the best possible mechanical and thermal data have been made available for these computations.

Szydlik, Paul P.↗
NASA NTRS1993

Intact capture of hypervelocity particles on Shuttle

The capability for capturing micrometeoroid analogs intact through laboratory simulations in passive underdense media offers a valuable tool for cosmic dust research. However, no amount of laboratory simulations can replace actual space experiments due to the technical inability to launch high fidelity analogs of micrometeoroids in ground laboratories and then reliably simulating high hypervelocities (greater than 7 km/s). Fluffy composite micrometeoroid analogs tend to break up and have not survived laboratory launches at beyond 4 km/s, however, a new technique of launching cluster analogs was developed for the two-stage light-gas gun at NASA Ames Vertical Gun Range. Plasma drag or electrostatic accelerators may be able to achieve higher speeds than two-stage light-gas guns but only with very limited projectile compositions and may result in severe projectile deformation. Consequently, a space demonstration of intact capture was sought since 1983. Initial results from our STS-47 flight, which carried the first Shuttle Sample Return Experiment (SRE) with silica aerogel capture media, are reported.

Tsou, P.↗
NASA NTRS2014

Stardust Interstellar Preliminary Examination VII: Synchrotron X-Ray Fluorescence Analysis of Six Stardust Interstellar Candidates Measured with the Advanced Photon Source 2-ID-D Microprobe

The NASA Stardust spacecraft exposed an aerogel collector to the interstellar dust passing through the solar system. We performed X-ray fluorescence element mapping and abundance measurements, for elements 19 < or = Z < or = 30, on six "interstellar candidates," potential interstellar impacts identified by Stardust@Home and extracted for analyses in picokeystones. One, I1044,3,33, showed no element hot-spots within the designated search area. However, we identified a nearby surface feature, consistent with the impact of a weak, high-speed particle having an approximately chondritic (CI) element abundance pattern, except for factor-of-ten enrichments in K and Zn and an S depletion. This hot-spot, containing approximately 10 fg of Fe, corresponds to an approximately 350 nm chondritic particle, small enough to be missed by Stardust@Home, indicating that other techniques may be necessary to identify all interstellar candidates. Only one interstellar candidate, I1004,1,2, showed a track. The terminal particle has large enrichments in S, Ti, Cr, Mn, Ni, Cu, and Zn relative to Fe-normalized CI values. It has high Al/Fe, but does not match the Ni/Fe range measured for samples of Al-deck material from the Stardust sample return capsule, which was within the field-of-view of the interstellar collector. A third interstellar candidate, I1075,1,25, showed an Al-rich surface feature that has a composition generally consistent with the Al-deck material, suggesting that it is a secondary particle. The other three interstellar candidates, I1001,1,16, I1001,2,17, and I1044,2,32, showed no impact features or tracks, but allowed assessment of submicron contamination in this aerogel, including Fe hot-spots having CI-like Ni/Fe ratios, complicating the search for CI-like interstellar/interplanetary dust.

Stardust↗
NASA NTRS1991

Are some chondrule rims formed by impact processes? - Observations and experiments

The ability of high-speed impacts into a parent body regolith to account for the textures and compositions observed for rims on some chondrules is presently supported by both observational and experimental data. Experimental results obtained with a light-gas gun encompass recovered-grain characteristics ranging from fragmented projectile grains mixed with melted aerogel, demonstrating that rim-like thermal and mechanical alterations of projectiles may be due to a high-velocity encounter with a low density target. Irrespective of conclusions for other types of rims, granular and opaque rim characteristics seem inconsistent with nebular condensation.

Bunch, T. E.↗
NASA NTRS2006

Review of Current State of the Art and Key Design Issues With Potential Solutions for Liquid Hydrogen Cryogenic Storage Tank Structures for Aircraft Applications

Due to its high specific energy content, liquid hydrogen (LH2) is emerging as an alternative fuel for future aircraft. As a result, there is a need for hydrogen tank storage systems, for these aircraft applications, that are expected to provide sufficient capacity for flight durations ranging from a few minutes to several days. It is understood that the development of a large, lightweight, reusable cryogenic liquid storage tank is crucial to meet the goals of and supply power to hydrogen-fueled aircraft, especially for long flight durations. This report provides an annotated review (including the results of an extensive literature review) of the current state of the art of cryogenic tank materials, structural designs, and insulation systems along with the identification of key challenges with the intent of developing a lightweight and long-term storage system for LH2. The broad classes of insulation systems reviewed include foams (including advanced aerogels) and multilayer insulation (MLI) systems with vacuum. The MLI systems show promise for long-term applications. Structural configurations evaluated include single- and double-wall constructions, including sandwich construction. Potential wall material candidates are monolithic metals as well as polymer matrix composites and discontinuously reinforced metal matrix composites. For short-duration flight applications, simple tank designs may suffice. Alternatively, for longer duration flight applications, a double-wall construction with a vacuum-based insulation system appears to be the most optimum design. The current trends in liner material development are reviewed in the case that a liner is required to minimize or eliminate the loss of hydrogen fuel through permeation.

Mital, Subodh K.↗
NASA NTRS2014

Stardust Interstellar Preliminary Examination IX: High-Speed Interstellar Dust Analog Capture in Stardust Flight-Spare Aerogel

The NASA Stardust mission used silica aerogel slabs to slowly decelerate and capture impinging cosmic dust particles for return to Earth. During this process, impact tracks are generated along the trajectory of the particle into the aerogel. It is believed that the morphology and dimensions of these tracks, together with the state of captured grains at track termini, may be linked to the size, velocity, and density of the impacting cosmic dust grain. Here, we present the results of laboratory hypervelocity impact experiments, during which cosmic dust analog particles (diameters of between 0.2 and 0.4 lm), composed of olivine, orthopyroxene, or an organic polymer, were accelerated onto Stardust flight spare low-density (approximately 0.01 g/cu cm) silica aerogel. The impact velocities (3-21 km/s) were chosen to simulate the range of velocities expected during Stardust's interstellar dust (ISD) collection phases. Track lengths and widths, together with the success of particle capture, are analyzed as functions of impact velocity and particle composition, density, and size. Captured terminal particles from low-density organic projectiles become undetectable at lower velocities than those from similarly sized, denser mineral particles, which are still detectable (although substantially altered by the impact process) at 15 km/s. The survival of these terminal particles, together with the track dimensions obtained during low impact speed capture of small grains in the laboratory, indicates that two of the three best Stardust candidate extraterrestrial grains were actually captured at speeds much lower than predicted. Track length and diameters are, in general, more sensitive to impact velocities than previously expected, which makes tracks of particles with diameters of 0.4 lm and below hard to identify at low capture speeds (<10 km/s). Therefore, although captured intact, the majority of the interstellar dust grains returned to Earth by Stardust remain to be found.

Stardust↗
NASA NTRS1996

Sol-gel Technology and Advanced Electrochemical Energy Storage Materials

Advanced materials play an important role in the development of electrochemical energy devices such as batteries, fuel cells, and electrochemical capacitors. The sol-gel process is a versatile solution for use in the fabrication of ceramic materials with tailored stoichiometry, microstructure, and properties. This processing technique is particularly useful in producing porous materials with high surface area and low density, two of the most desirable characteristics for electrode materials. In addition,the porous surface of gels can be modified chemically to create tailored surface properties, and inorganic/organic micro-composites can be prepared for improved material performance device fabrication. Applications of several sol-gel derived electrode materials in different energy storage devices are illustrated in this paper. V2O5 gels are shown to be a promising cathode material for solid state lithium batteries. Carbon aerogels, amorphous RuO2 gels and sol-gel derived hafnium compounds have been studied as electrode materials for high energy density and high power density electrochemical capacitors.

Chung-tse Chu↗
NASA NTRS2007

STARDUST Curation and Science at JSC

Dust particles released from comet 81P/Wild-2 were captured in silica aerogel on-board the STARDUST spacecraft and returned to Earth on January 15, 2006. STARDUST recovered thousands of particles ranging in size from 1 to 100 micrometers. During the six month Preliminary Examination period an international consortium of 180 scientists investigated their mineralogy/petrology, organic/inorganic chemistry, optical properties and isotopic compositions. Stardust samples are now available for research by the entire research community.

Nakamura-Messenger, K.↗
NASA NTRS1998

Noble Metal Immersion Spectroscopy of Silica Alcogels and Aerogels

We have fabricated aerogels containing gold and silver nanoparticles for gas catalysis applications. By applying the concept of an average or effective dielectric constant to the heterogeneous interlayer surrounding each particle, we extend the technique of immersion spectroscopy to porous or heterogeneous media. Specifically, we apply the predominant effective medium theories for the determination of the average fractional composition of each component in this inhomogeneous layer. Hence, the surface area of metal available for catalytic gas reaction is determined. The technique is satisfactory for statistically random metal particle distributions but needs further modification for aggregated or surfactant modified systems. Additionally, the kinetics suggest that collective particle interactions in coagulated clusters are perturbed during silica gelation resulting in a change in the aggregate geometry.

Smith, David D.↗
NASA NTRS2004

The Stardust: A Successful Encounter with the Remarkable Comet Wild 2

On January 2, 2004 the Stardust spacecraft completed a close flyby of comet Wild2 (P81). Flying at a relative speed of 6.1 km/s within 237km of the 5 km nucleus, the spacecraft took 72 close-in images, measured the flux of impacting particles and did in-situ compositional analysis of freshly released dust with a time-of-flight mass spectrometer. The primary goal of the mission is to collect >500 particles >15 m diameter and return them to Earth on January 15, 2006. The cometary particles ranging in size from a micron to approx.100 microns were collected in low density silica aerogel. After returning over a hundred 2x4x3 cm aerogel collection cells will be processed at the curatorial facility at the NASA Johnson Space Center and 5 to 100 micron size extracted cometary particles will be distributed to analysts by a system that will be based on the allocation procedures for cosmic dust, Antarctic meteorites and lunar samples.

Brownlee, D. E.↗
NASA NTRS1997

Surface Plasmon Resonance Evaluation of Colloidal Metal Aerogel Filters

We have fabricated aerogels containing gold, silver, and platinum nanoparticles for gas catalysis applications. By applying the concept of an average or effective dielectric constant to the heterogeneous interlayer surrounding each particle, we extend the technique of immersion spectroscopy to porous or heterogeneous media. Specifically, we apply the predominant effective medium theories for the determination of the average fractional composition of each component in this inhomogeneous layer. Hence, the surface area of metal available for catalytic gas reaction is determined. The technique is satisfactory for statistically random metal particle distributions but needs further modification for aggregated or surfactant modified systems. Additionally, the kinetics suggest that collective particle interactions in coagulated clusters are perturbed during silica gelation resulting in a change in the aggregate geometry.

Smith, David D.↗
NASA NTRS2005

Electron Beam Analysis of Micrometeoroids Captured in Aerogel as Stardust Analogues

In January 2004, NASA s Stardust spacecraft passed through the tail of Comet 81P/Wild-2. The on-board dust flux monitor instrument indicated that numerous micro- and nano-meter sized cometary dust particles were captured by the dedicated silica aerogel capture cell. The collected cometary particles will be returned to Earth in January 2006. Current Stardust analogues are: (i) Light-gas-gun accelerated individual mineral grains and carbonaceous meteoritic material in aerogels at the Stardust encounter velocity ca.approximately 6 kilometers per second. (ii) Aerogels exposed in low-Earth orbit (LEO) containing preserved cosmic dust grains. Studies of these impacts offer insight into the potential state of the captured cometary dust by Stardust and the suitability of various analytical techniques. A number of papers have discussed the application of sophisticated synchrotron analytical techniques to analyze Stardust particles. Yet much of the understanding gained on the composition and mineralogy of interplanetary dust particles (IDPs) has come from electron microscopy studies. Here we discuss the application of scanning electron microscopy (SEM) for Stardust during the preliminary phase of post-return investigations.

Graham, G. A.↗
NASA NTRS2014

Coordinated Mineralogical and Isotopic Analysis of a Cosmic Symplectite Identified in a Stardust Terminal Particle

Comet Wild-2 samples returned by the Stardust spacecraft contain a chemically diverse mixture of material, underscoring the complex nature of comets. Studies of entire Stardust aerogel tracks afford the opportunity to examine the fine-grained particle fragments distributed along the length of the track as well as the terminal particles. Previous TEM characterization of a terminal particle (TP) in track #147 revealed a symplectically intergrown iron sulfide and oxide assemblage. Mineralogically similar assemblages, known as cosmic symplectites (COS, formerly termed "new-PCP"), have only been identified in the primitive carbonaceous chondrite Acfer 094. Meteoritic COS have isotopically heavy O compositions (delta (sup 17), O-18 = 180per mille) that point to interactions with early solar system primordial water. In this study we report mineralogical and O isotopic measurements of the Wild-2 COS assemblage. Experimental: Track #147 is a "bulbous"-type track (4600 microns long) containing 7 terminal particles. The TPs were removed from the track, embedded in epoxy, and ultramicrotomed. A JEOL 2500SE 200 keV field-emission scanning-transmission electron microscope was used to obtain quantitative elemental maps and detailed mineralogical characterization. Following TEM analysis, two thin sections of TP4 (12 microns) were analyzed for O isotopes by raster ion imaging with the JSC NanoSIMS 50L. All three O isotopes were measured simultaneously using electron multipliers. San Carlos olivine grains were used as isotopic standards. Results and Discussion: The COS in the Wild-2 track #147 TP4 sample consists of symplectically intergrown pentlandite and nanocrystalline maghemite which coexists with high-Ca pyroxene with Na and Cr (kosmochlor component). This kosmochlor component could have a nebular origin and be precursors to type II chondrules in ordinary chondrites. Yet pentlandite is not a stable phase in the nebula. The COS in Acfer 094 also consists of pentlandite, but contains magnetite [4] rather than the more oxidized maghemite observed in the Wild-2 COS. The Acfer 094 COS display heavy O isotopic compositions that are the result of sulfidization and oxidation of Fe, Ni-metal grains and sulfides by O-17- and O-18-rich water in the solar nebula or possibly on the parent body. The O isotopic composition of the Wild-2 COS, however, is indistinguishable from terrestrial, indicating it was not altered by the same primordial aqueous reservoir as the Acfer 094 COS. The alteration could have occurred on the parent body by isotopically equilibrated ice. The mineralogy and petrography of Wild-2 samples suggests an incomplete or nascent hydration process. In future work we will analyze S isotopes in the track #147 TP4 COS and search for additional COS in Stardust samples.

Nguyen, A. N.↗
NASA NTRS2004

Measurement of the Abundance of Radioactive Be-10 and Other Light Isotopes in Cosmic Radiation Up to 2 GeV /Nucleon with the Balloon-Borne Instrument Isomax

The Isotope Magnet Experiment (ISOMAX), a balloon-borne superconducting magnet spectrometer, was designed to measure the isotopic composition of the light isotopes (3 les than or = Z less than or = 8) of cosmic radiation up to 4 GeV/nucleon with a mass resolution of better than 0.25 amu by using the velocity versus rigidity technique. To achieve this stringent mass resolution, ISOMAX was composed of three major detector systems: a magnetic rigidity spectrometer with a precision drift chamber tracker in conjunction with a three-layer time-of-flight system, and two silica-aerogel Cerenkov counters for velocity determination. A special emphasis of the ISOMAX program was the accurate measurement of radioactive Be-10 with respect to its stable neighbor isotope Be-9, which provides important constraints on the age of cosmic rays in the Galaxy. ISOMAX had its first balloon flight on 1998 August 4-5 from Lynn Lake, Manitoba, Canada. Thirteen hours of data were recorded during this flight at a residual atmosphere of less than 5 g/sq cm. The isotopic ratio at the top of the atmosphere for Be-10/Be-9 was measured to be 0.195 +/- 0.036 (statistical) +/- 0.039 (systematic) between 0.26 and 1.03 GeV/nucleon and 0.317 +/- 0.109(statistical) +/- 0.042(systematic) between 1.13 and 2.03 GeV/nucleon. This is the first measurement of its kind above l GeV/nucleon. ISOMAX results tend to be higher than predictions from current propagation models. In addition to the beryllium results, we report the isotopic ratios of neighboring lithium and boron in the energy range of the time-of-flight system (up to approx. 1 GeV/nucleon). The lithium and boron ratios agree well with existing data and model predictions at similar energies.

Hams, T.↗