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NASA NTRS2006

Optical Spectroscopy of Stardust Samples

The Stardust spacecraft collected dust samples of the Kuiper belt comet 81P Wild-2 in aerogel and returned them to Earth January 15, 2006. Preliminary examination (PE) of the collected dust includes teams focused on mineralogy, chemical composition, isotopic measurements, organic analysis, cratering and spectroscopic properties. The main PE science goals are to provide an initial characterization of the returned samples with an emphasis on the capture process and its effects on the samples, a comparison of Stardust samples to other meteoritic materials, and the abundance of presolar materials in the Stardust samples. The science objectives of the Spectroscopy team are to obtain spectroscopic data on Stardust particles through infrared (IR), UV/Vis and Raman measurements of particles in aerogel, extracted particles, keystones, and microtome thin sections. These data will be used to answer fundamental science questions about the nature of the samples, but will also serve as preliminary mineralogical data to guide follow-on measurements that will be performed in the other preliminary examination teams. The IR characteristics of Stardust particles are measured to determine: 1) the nature of the indigenous 3.4 micron organic feature, is it detected and can it be differentiated/deconvolved from the contaminated aerogel? How does it compare to features observed in interplanetary dust particles (IDPs) and to astronomical measurements of comets and interstellar dust? 2) the shape and fine structure within the 10 micron silicate feature. Overlap with the strong Si-O stretching vibration from the aerogel complicates this analysis, but we hope to determine if the feature is dominated by amorphous silicates such as those observed in IDPs and comets and whether or not crystalline silicates (e.g. olivine, pyroxene, clays) are present, 3) the presence of secondary (alteration) phases. Deep Impact results suggest that IR observations of Stardust particles should be evaluated for the presence of hydrated materials (water bands at 3 and 6 microns) and carbonates (6.8 microns and other resonances) and 4) the detection of crystalline features in the far-IR (20-100 microns) region where crystalline silicates and other minerals have strong bands that can be used both for phase analysis and phase chemistry. It has been demonstrated that these far-IR measurements can be obtained in situ on particles in aerogel keystones.

Keller, Lindsay P.↗
NASA NTRS2006

Stardust Sample: Investigator's Guidebook

In January 2006, the Stardust spacecraft returned the first in situ collection of samples from a comet, and the first samples of contemporary interstellar dust. Stardust is the first US sample return mission from a planetary body since Apollo, and the first ever from beyond the moon. This handbook is a basic reference source for allocation procedures and policies for Stardust samples. These samples consist of particles and particle residues in aerogel collectors, in aluminum foil, and in spacecraft components. Contamination control samples and unflown collection media are also available for allocation.

Allen, Carl↗
NASA NTRS2007

Sample Curation at a Lunar Outpost

The six Apollo surface missions returned 2,196 individual rock and soil samples, with a total mass of 381.6 kg. Samples were collected based on visual examination by the astronauts and consultation with geologists in the science back room in Houston. The samples were photographed during collection, packaged in uniquely-identified containers, and transported to the Lunar Module. All samples collected on the Moon were returned to Earth. NASA's upcoming return to the Moon will be different. Astronauts will have extended stays at an out-post and will collect more samples than they will return. They will need curation and analysis facilities on the Moon in order to carefully select samples for return to Earth.

Allen, Carlton C.↗
NASA NTRS2007

Overview of the Results of the Organics PET Study of the Cometary Samples from Comet Wild 2 by the Stardust Mission

STARDUST is the first mission designed to bring samples back to Earth from a known comet. The captured samples were successfully returned to Earth on 15 Jan 2006, after which they were subjected to a preliminary examination by a number of teams of scientists from around the world. This abstract describes the efforts of the Organics Preliminary Examination Team (PET). More detailed discussions of specific analyses of the samples can be found in other papers presented at this meeting by individual members of the Organics PET (see the author list above for team members). The studied Wild 2 gas and dust samples were collected by impact onto aerogel tiles and Al foils when the spacecraft flew through the coma of 81P/Wild 2 on 2 Jan 2004 at a relative velocity of approx.6.1 kilometers per second. After recovery of the Sample Return Capsule (SRC) on 15 Jan 2006, the aerogel collector trays were removed in a clean room at JSC. After documentation of the collection, selected aerogel tiles and aluminum foils were removed and aerogel and cometary samples extracted for study.

Sandford, S. A.↗
NASA NTRS2007

Genesis Contingency Planning and Mishap Recovery: The Sample Curation View

Planning for sample preservation and curation was part of mission design from the beginning. One of the scientific objectives for Genesis included collecting samples of three regimes of the solar wind in addition to collecting bulk solar wind during the mission. Collectors were fabricated in different thicknesses for each regime of the solar wind and attached to separate frames exposed to the solar wind during specific periods of solar activity associated with each regime. The original plan to determine the solar regime sampled for specific collectors was to identify to which frame the collector was attached. However, the collectors were dislodged during the hard landing making identification by frame attachment impossible. Because regimes were also identified by thickness of the collector, the regime sampled is identified by measuring fragment thickness. A variety of collector materials and thin films applied to substrates were selected and qualified for flight. This diversity provided elemental measurement in more than one material, mitigating effects of diffusion rates and/or radiation damage. It also mitigated against different material and substrate strengths resulting in differing effects of the hard landing. For example, silicon crystal substrates broke into smaller fragments than sapphire-based substrates and diamond surfaces were more resilient to flying debris damage than gold. The primary responsibility of the curation team for recovery was process documentation. Contingency planning for the recovery phase expanded this responsibility to include not only equipment to document, but also gather, contain and identify samples from the landing area and the recovered spacecraft. The team developed contingency plans for various scenarios as part of mission planning that included topographic maps to aid in site recovery and identification of different modes of transport and purge capability depending on damage. A clean tent, set-up at Utah Test & Training Range to control the environment for processing the sample return capsule and cleanly installing a nitrogen purge to the canister, was used to control the environment for extracting collector fragments from the damaged canister and to document and package over 10,000 collector fragments.

Stansbery, E. K.↗
NASA NTRS2008

Astrobiology Sample Analysis Program (ASAP) for Advanced Life Detection Instrumentation Development and Calibration

Scientific ground-truth measurements for near-term Mars missions, such as the 2009 Mars Science Laboratory (MSL) mission, are essential for validating current in situ flight instrumentation and for the development of advanced instrumentation technologies for life-detection missions over the next decade. The NASA Astrobiology Institute (NAI) has recently funded a consortium of researchers called the Astrobiology Sample Analysis Program (ASAP) to analyze an identical set of homogenized martian analog materials in a "round-robin" style using both state-of-the-art laboratory techniques as well as in-situ flight instrumentation including the SAM gas chromatograph mass spectrometer and CHEMIN X-ray diffraction/fluorescence instruments on MSL and the Urey and MOMA organic analyzer instruments under development for the 2013 ExoMars missions. The analog samples studied included an Atacama Desert soil from Chile, the Murchison meteorite, a gypsum sample from the 2007 AMASE Mars analog site, jarosite from Panoche Valley, CA, a hydrothermal sample from Rio Tinto, Spain, and a "blind" sample collected during the 2007 MSL slow-motion field test in New Mexico. Each sample was distributed to the team for analysis to: (1) determine the nature and inventory of organic compounds, (2) measure the bulk carbon and nitrogen isotopic composition, (3) investigate elemental abundances, mineralogy and matrix, and (4) search for biological activity. The experimental results obtained from the ASAP Mars analog research consortium will be used to build a framework for understanding the biogeochemistry of martian analogs, help calibrate current spaceflight instrumentation, and enhance the scientific return from upcoming missions.

Glavin, Daniel↗
NASA NTRS2008

Approximation of Failure Probability Using Conditional Sampling

In analyzing systems which depend on uncertain parameters, one technique is to partition the uncertain parameter domain into a failure set and its complement, and judge the quality of the system by estimating the probability of failure. If this is done by a sampling technique such as Monte Carlo and the probability of failure is small, accurate approximation can require so many sample points that the computational expense is prohibitive. Previous work of the authors has shown how to bound the failure event by sets of such simple geometry that their probabilities can be calculated analytically. In this paper, it is shown how to make use of these failure bounding sets and conditional sampling within them to substantially reduce the computational burden of approximating failure probability. It is also shown how the use of these sampling techniques improves the confidence intervals for the failure probability estimate for a given number of sample points and how they reduce the number of sample point analyses needed to achieve a given level of confidence.

Giesy. Daniel P.↗
NASA NTRS2009

Carbon XANES Data from Six Aerogel Picokeystones Cut from the Top and Bottom Sides of the Stardust Comet Sample Tray

Great care and a large effort was made to minimize the amount of organic matter contained within the flight aerogel used to collect Comet 81P/Wild 2 samples. Even so, by the very nature of the production process and silica aerogel s affinity for volatile organics keeping silica aerogel free from organics is a monumental task. Silica aerogel from three production batches was flown on the Stardust sample return mission. All 3 types had layered densities varying from 5mg/ml to 50 mg/ml where the densest aerogel was farthest away from the collection area. A 2 step gelation process was used to make the flight aerogel and organics used in this process were tetraethylorthosilicate, ethanol and acetonitrile. Both ammonium hydroxide and nitric acid were also used in the aerogel production process. The flight aerogel was baked at JPL at 300 C for 72 hours, most of the baking was done at atmosphere but twice a day the oven was pumped to 10 torr for hour [1]. After the aerogel was baked it was stored in a nitrogen purged cabinet until flight time. One aerogel cell was located in the SRC away from any sample collection area as a witness to possible contamination from out gassing of the space craft, re-entry gases and any other organic encounter. This aerogel was aerogel used in the interstellar collection sample tray and is the least dense of the 3 batches of aerogel flown. Organics found in the witness tile include organics containing Si-CH3 bonds, amines and PAHS. Besides organic contamination, hot spots of calcium were reported in the flight aerogel. Carbonates have been detected in comet 81P/Wild2 samples . During preflight analyses, no technique was used to analyze for carbonates in aerogel. To determine if the carbonates found in 81P/Wild2 samples were from the comet, it is necessary to analyze the flight aerogel for carbonate as well as for organics.

Wirick, S.↗
NASA NTRS2009

Rotary Percussive Auto-Gopher for Deep Drilling and Sampling

The term "rotary percussive auto-gopher" denotes a proposed addition to a family of apparatuses, based on ultrasonic/ sonic drill corers (USDCs), that have been described in numerous previous NASA Tech Briefs articles. These apparatuses have been designed, variously, for boring into, and/or acquiring samples of, rock or other hard, brittle materials of geological interest. In the case of the rotary percussive autogopher, the emphasis would be on developing an apparatus capable of penetrating to, and acquiring samples at, depths that could otherwise be reached only by use of much longer, heavier, conventional drilling-and-sampling apparatuses. To recapitulate from the prior articles about USDCs: A USDC can be characterized as a lightweight, low-power jackhammer in which a piezoelectrically driven actuator generates ultrasonic vibrations and is coupled to a tool bit through a free mass. The bouncing of the free mass between the actuator horn and the drill bit converts the actuator ultrasonic vibrations into sonic hammering of the drill bit. The combination of ultrasonic and sonic vibrations gives rise to a hammering action (and a resulting chiseling action at the tip of the tool bit) that is more effective for drilling than is the microhammering action of ultrasonic vibrations alone. The hammering and chiseling actions are so effective that the size of the axial force needed to make the tool bit advance into soil, rock, or another material of interest is much smaller than in ordinary rotary drilling, ordinary hammering, or ordinary steady pushing. The predecessor of the rotary percussive auto-gopher is an apparatus, now denoted an ultrasonic/sonic gopher and previously denoted an ultrasonic gopher, described in "Ultrasonic/ Sonic Mechanism for Drilling and Coring" (NPO-30291), NASA Tech Briefs Vol. 27, No. 9 (September 2003), page 65. The ultrasonic/sonic gopher is intended for use mainly in acquiring cores. The name of the apparatus reflects the fact that, like a gopher, it periodically stops advancing at the end of the hole to bring excavated material (in this case, a core sample) to the surface, then re-enters the hole to resume the advance of the end of the hole. By use of a cable suspended from a reel on the surface, the gopher is lifted from the hole to remove a core sample, then lowered into the hole to resume the advance and acquire the next core sample.

Bar-Cohen, Yoseph↗
NASA NTRS2009

Two-Stage Variable Sample-Rate Conversion System

A two-stage variable sample-rate conversion (SRC) system has been pro posed as part of a digital signal-processing system in a digital com munication radio receiver that utilizes a variety of data rates. The proposed system would be used as an interface between (1) an analog- todigital converter used in the front end of the receiver to sample an intermediatefrequency signal at a fixed input rate and (2) digita lly implemented tracking loops in subsequent stages that operate at v arious sample rates that are generally lower than the input sample r ate. This Two-Stage System would be capable of converting from an input sample rate to a desired lower output sample rate that could be var iable and not necessarily a rational fraction of the input rate.

Tkacenko, Andre↗
NASA NTRS2009

Apparatus Measures Thermal Conductance Through a Thin Sample from Cryogenic to Room Temperature

An apparatus allows the measurement of the thermal conductance across a thin sample clamped between metal plates, including thermal boundary resistances. It allows in-situ variation of the clamping force from zero to 30 lb (133.4 N), and variation of the sample temperature between 40 and 300 K. It has a special design feature that minimizes the effect of thermal radiation on this measurement. The apparatus includes a heater plate sandwiched between two identical thin samples. On the side of each sample opposite the heater plate is a cold plate. In order to take data, the heater plate is controlled at a slightly higher temperature than the two cold plates, which are controlled at a single lower temperature. The steady-state controlling power supplied to the hot plate, the area and thickness of samples, and the temperature drop across the samples are then used in a simple calculation of the thermal conductance. The conductance measurements can be taken at arbitrary temperatures down to about 40 K, as the entire setup is cooled by a mechanical cryocooler. The specific geometry combined with the pneumatic clamping force control system and the steady-state temperature control approach make this a unique apparatus.

Tuttle, James G.↗
NASA NTRS2009

Pre-Flight Characterization of Samples for the MISSE-7 Spacesuit Fabric Exposure Experiment

A series of six sample spacesuit pressure garment assembly (PGA) fabric samples were prepared for the Materials International Space Station Experiment 7 (MISSE-7) flight experiment to test the effects of damage by lunar dust on the susceptibility of the fabrics to radiation damage. These included pristine Apollo-era fluorinated ethylene-propylene (FEP) fabric, Apollo-era FEP fabric that had been abraded with JSC-1A lunar simulant, and a piece of Alan Bean s Apollo 12 PGA sectioned from near the left knee. Also included was a sample of pristine orthofabric, and orthofabric that had been abraded to two different levels with JSC-1A. The samples were characterized using optical microscopy, field emission scanning electron microscopy, and atomic force microscopy. Two sets of six samples were then loaded in space environment exposure hardware, one of which was stored as control samples. The other set was affixed to the MISSE-7 experiment package, and will be mounted on the International Space Station, and exposed to the wake-side low Earth orbit environment. It will be retrieved after an exposure of approximately 12 months, and returned for post flight analysis.

Gaier, James R.↗
NASA NTRS2010

Environmental Stress Testing of the Single Sample Cylinder: A Proven Consensus Standard for Internal Gas Analysis (IGA) or Residual Gas Analysis (RGA)

In August 2008, Schuessler Consulting was contracted by NASA GSFC in support of the NASA Electronic Parts and Packaging (NEPP) program to perform two separate studies on moisture laden air in a stainless steel cylinder that had been designed to become a consensus standard for Test Method 1018. This Test Method was originally released for hybrids under Mil. Std. 883 but was quickly utilized on other microelectronic devices under the auspice of Mil. Std. 750. The cylinder had subsequently been fabricated for the 750 community. It was back-filled with moist air and subsequently analyzed over a period of time under a previous NASA contract. It had been shown that moisture in the 4000 - 5000 ppm range could be analyzed rather precisely with a mass spectrometer, commonly referred to as a Residual Gas Analyzer (RGA). The scope of this study was to ascertain if the composition and precision varied as a function of thermal shock at sub-zero temperatures and whether there was consensus when the standard was submitted to other RGA units. It was demonstrated and published that the consensus standard would yield precise RGA data for moisture within +/- 1% when optimized for a given RGA unit. It has been subsequently shown in this study at Oneida Research Services, that sub-zero storage did not affect that precision when a well-defined protocol for the analysis was followed. The consensus standard was taken to a second facility for analysis where it was found that moisture adsorption on the transfer lines caused precision to drop to +/- 12%. The Single Sample Cylinder (SSC) is a one liter stainless steel cylinder with associated sampling valves and has considerable weight and volume. But this considerable size allows for approximately 300 gas samples of the same composition to be delivered to any RGA unit. Lastly, a smaller cylinder, approximately 75 cc, of a second consensus standard was fabricated and tested with a different mix of fixed gases where moisture was kept in the 100 ppm range. This second standard has the potential of providing 30 gaseous samples and can be readily shipped to any analytical facility that desires to generate comparison RGA data. A series of comparison residual gas analyses was performed at the Honeywell Federal Manufacturing & Technologies facility in the National Nuclear Facility Administration s plant in Kansas City to complete this project. It was shown that improvements in the precision of a given RGA unit can be done by controlling the cycle time for each analysis and increasing analysis temperatures to minimize moisture adsorption. It was also found that a "one time event" in the subzero storage of the large SSC did not effect the units ability to continuously supply precise samples of the same chemistry, however the "event" caused a permanent +8% shift in the reported value of the moisture content. Lastly, a set of SSC RGA results was plotted on a common graph with DSCC "correlation study" RGA data. The result demonstrates the ability of the SSC to remove many of the individual variances that single, individual samples introduce. The consensus standards are now in storage at Oneida Research Services, one of the DSCC certified houses that does RGA to Military Standards, where they await future studies. The analytical data and the operational parameters of the instruments used are provided in the following discussion. Limitations and suggested means for improvement of both precision and accuracy are provided.

Schuessler, Philipp WH↗
NASA NTRS2011

Apollo Lunar Sample Integration into Google Moon: A New Approach to Digitization

The Google Moon Apollo Lunar Sample Data Integration project is part of a larger, LASER-funded 4-year lunar rock photo restoration project by NASA s Acquisition and Curation Office [1]. The objective of this project is to enhance the Apollo mission data already available on Google Moon with information about the lunar samples collected during the Apollo missions. To this end, we have combined rock sample data from various sources, including Curation databases, mission documentation and lunar sample catalogs, with newly available digital photography of rock samples to create a user-friendly, interactive tool for learning about the Apollo Moon samples

Dawson, Melissa D.↗
NASA NTRS2011

Restoration and PDS Archive of Apollo Lunar Rock Sample Data

In 2008, scientists at the Johnson Space Center (JSC) Lunar Sample Laboratory and Image Science & Analysis Laboratory (under the auspices of the Astromaterials Research and Exploration Science Directorate or ARES) began work on a 4-year project to digitize the original film negatives of Apollo Lunar Rock Sample photographs. These rock samples together with lunar regolith and core samples were collected as part of the lander missions for Apollos 11, 12, 14, 15, 16 and 17. The original film negatives are stored at JSC under cryogenic conditions. This effort is data restoration in the truest sense. The images represent the only record available to scientists which allows them to view the rock samples when making a sample request. As the negatives are being scanned, they are also being formatted and documented for permanent archive in the NASA Planetary Data System (PDS) archive. The ARES group is working collaboratively with the Imaging Node of the PDS on the archiving.

Garcia, P. A.↗
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 NTRS2011

Almahata Sitta and Brecciated Ureilites: Insights into the Heterogeneity of Asteroids and Implications for Sample Return

Analysis of samples returned to terrestrial laboratories enables more precise measurements and a wider range of techniques to be utilized than can be achieved with either remote sensing or rover instruments. Furthermore, returning samples to Earth allows them to be stored and re-examined with future technology. Following the success of the Hayabusa mission, returning samples from asteroids should be a high priority for understanding of early solar system evolution, planetary formation and differentiation. Meteorite falls provide us with materials and insight into asteroidal compositions. Almahata Sitta (AS) was the first meteorite fall from a tracked asteroid (2008 TC3) [1] providing a rare opportunity to compare direct geochemical observations with remote sensing data. Although AS is predominantly ureilitic, multiple chondritic fragments have been associated with this fall [2,3]. This is not unique, with chondritic fragments being found in many howardite samples (as described in a companion abstract [4]) and in brecciated ureilites, some of which are known to represent ureilitic regolith [5-7]. The heterogeneity of ureilite samples, which are thought to all originate from a single asteroidal ureilite parent body (UPB) [5], gives us information about both internal and external asteroidal variations. This has implications both for the planning of potential sample return missions and the interpretation of material returned to Earth. This abstract focuses on multiple fragments of two meteorites: Almahata Sitta (AS); and Dar al Gani (DaG) 1047 (a highly brecciated ureilite, likely representative of ureilite asteroidal regolith).

Ross, A. J.↗
NASA NTRS2001

Assessment of Air Quality in the Shuttle and International Space Station (ISS) Based on Samples Returned by STS-102 at the Conclusion of 5A.1

The toxicological assessment of air samples returned at the end of the STS-102 (5A.1) flight to the ISS is reported. ISS air samples were taken in late February 2001 from the Service Module, FGB, and U.S. Laboratory using grab sample canisters (GSCs) and/or formaldehyde badges . A "first-entry" sample of the multipurpose logistics module (MPLM) atmosphere was taken with a GSC, and preflight and end-of-mission samples were obtained from Discovery using GSCs. Analytical methods have not changed from earlier reports, and all quality control measures were met for the data presented herein. The two general criteria used to assess air quality are the total-non-methane-volatile organic hydrocarbons (NMVOCs) and the total T-value (minus the CO2 contribution). Control of atmospheric alcohols is important to the water recovery system engineers, hence total alcohols were also assessed in each sample. Formaldehyde is quantified separately.

James, John T.↗