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Gas chromatographic column for the storage of sample profiles

The concept of a sample retention column that preserves the true time profile of an analyte of interest is studied. This storage system allows for the detection to be done at convenient times, as opposed to the nearly continuous monitoring that is required by other systems to preserve a sample time profile. The sample storage column is essentially a gas chromatography column, although its use is not the separation of sample components. The functions of the storage column are the selective isolation of the component of interest from the rest of the components present in the sample and the storage of this component as a function of time. Using octane as a test substance, the sample storage system was optimized with respect to such parameters as storage and readout temperature, flow rate through the storage column, column efficiency and storage time. A 3-h sample profile was collected and stored at 30 degrees C for 20 h. The profile was then retrieved, essentially intact, in 5 min at 130 degrees C.

NASA Program Exobiology↗

Carbon isotope evidence for a magmatic origin for Archaean gold-quartz vein ore deposits

Sediments from three sites in the Santa Barbara Basin were examined with a 160X power light microscope and TEM equipment to characterize the magnetostatic bacteria (MB) in the samples. Both the free magnetite and the crystals in the MB in the samples had lengths from 40-60 nm in length and increased in size from one end to the next. An intact magnetosome was also observed. Scanning the sediments with saturation isothermal remanent magnetization (SIRM) and altering field demagnetization techniques using a SQUID magnetometer yielded coercivity spectra which showed that the primary remanence carrier in the sediments was single domain magnetite. Although it is expected that the predominance of the bacterial magnetite component will decrease with depth in the open ocean basin, single-domain bacteria as old as 50 Myr have been observed in oceanic sediments.

Burrows, D. R.↗

Gas release and ordering of carbon in the Allende meteorite

An attempt is made to ascertain whether the inert gas atoms leave their carrier phases by volume diffusion, with intact internal phase frameworks, or are instead expelled from the solids as a results of substantial rearrangement, during release from samples of the Allende carbonaceous meteorite. Gas release over the 300-1100 C range was followed by Raman spectroscopic studies in the 1360 and 1580/cm wavelength bands of carbon. The results obtained indicate that the gas release at high temperatures is causally related to the ordering of carbon.

Heymann, D.↗

Dividing the Concentrator Target From the Genesis Mission

The Genesis spacecraft, launched in 2001, traveled to a Lagrangian point between the Earth and Sun to collect particles from the solar wind and return them to Earth. However, during the return of the spacecraft in 2004, the parachute failed to open during descent, and the Genesis spacecraft crashed into the Utah desert. Many of the solar wind collectors were broken into smaller pieces, and the field team rapidly collected the capsule and collector pieces for later assessment. On each of the next few days, the team discovered that various collectors had survived intact, including three of four concentrator targets. Within a month, the team had imaged more than 10,000 fragments and packed them for transport to the Astromaterials Acquisition and Curation Office within the ARES Directorate at JSC. Currently, the Genesis samples are curated along with the other extraterrestrial sample collections within ARES. Although they were broken and dirty, the Genesis solar wind collectors still offered the science community the opportunity to better understand our Sun and the solar system as a whole. One of the more highly prized concentrator collectors survived the crash almost completely intact. The Genesis Concentrator was designed to concentrate the solar wind by a factor of at least 20 so that solar oxygen and nitrogen isotopes could be measured. One of these materials was the Diamond-on-Silicon (DoS) concentrator target. Unfortunately, the DoS concentrator broke on impact. Nevertheless, the scientific value of the DoS concentrator target was high. The Genesis Allocation Committee received a request for approximately 1 cm(sup 2) of the DoS specimen taken near the focal point of the concentrator for the analysis of solar wind nitrogen isotopes. The largest fragment, Genesis sample 60000, was designated for this allocation and needed to be precisely cut. The requirement was to subdivide the designated sample in a manner that prevented contamination of the sample and minimized the risk of losing or breaking the precious requested sample fragment. The Genesis curator determined that the use of laser scribing techniques to "cut" a precise line and subsequently cleave the sample (in a controlled break of the sample along that line) was the best method for accomplishing the sample subdivision. However, there were risks, including excess heating of the sample, that could cause some of the implanted solar wind to be lost via thermal diffusion. Accidentally breaking the sample during the handling and cleaving process was an additional risk. Early in fiscal year 2013, to address this delicate, complicated task, the ARES Directorate assembled its top scientists to develop a cutting plan that would ensure success when applied to the actual concentrator target wafer; i.e., to produce an approximately 1 cm(sup 2) piece from the requested area of the wafer. The team, subsequently referred to as the JSC Genesis Tiger Team, spent months researching and testing parameters and techniques related to scribing, cleaving, transporting, handling, and holding (i.e., mounting) the specimen. The investigation required considerable "thinking outside the box," and many, many trials using nonflight wafer analogs. After all preliminary testing, the following method was adopted as the final cutting plan. It was used in two final end-to-end practice runs before being used on the actual flight target wafer. The wafer was oriented on the laser cutting stage with the 100 and 010 directions of the wafer parallel to the corresponding X and Y directions of the cutting stage. The laser was programed to scribe 31 lines of the appropriate length along the Y stage direction. The programed scribe lines were separated by 5 micron in the X direction. The laser parameters were set as follows: (1) The laser power was 0.5 watts; (2) each line consisted of 50 passes, with the Z position being advanced 5 micron per pass; and (3) 30 s would elapse before the next line was scribed to allow for wafer cool down from any possible heating via the laser. The ablated material that "stuck" in the "scribe-cut" was removed from the "cut" using an ultrasonic micro-tool. After all the ablated silicon was removed from the wafer, the wafer was repositioned in exactly the same orientation on the laser stage. The laser was focused using the bottom of the wafer channel, and the 31-line scribing pattern described above was reprogrammed using the Z position of the groove bottom as the starting Z value instead of the top wafer surface, which was used previously. Upon completion of the second set of scribes, the ultrasonic micro-tool was again used to clean out the cut. The wafer was remounted on the stage in exactly the same orientation as before. The laser was again focused on the bottom of the groove. This time, however, the laser was.programed to scribe only one line down the exact center of the channel. The final scribe line consisted of 100 passes with a Z advance of 5 micron per pass and with the laser power set at 0.5 watts. As mentioned above, the final cutting plan was practiced in two end-to-end trials using non-flight, triangular-shaped silicon wafers similar in size and orientation to the actual DOS 60000 target sample. The actual scribing of the triangular-shaped wafers required scribing two lines and cleaving (i.e. scribe-cleave, then scribe-cleave) to obtain the piece requested for allocation. Early in December 2012, after many months of experiments and practicing and perfecting the techniques and procedures, the team successfully subdivided the Genesis DoS 60000 target sample, one of the most scientifically important samples from the Genesis mission (figure 2). On December 17, 2012, the allocated piece of concentrator target sample was delivered to the requesting principal investigator.The cutting plan developed for the subdivision of this sample will be used as the model for subdividing future requested Genesis flight wafers (appropriately modified for different wafer types).

Lauer, H. V., Jr.↗

NM-Scale Anatomy of an Entire Stardust Carrot Track

Comet Wild-2 samples collected by NASA s Stardust mission are extremely complex, heterogeneous, and have experienced wide ranges of alteration during the capture process. There are two major types of track morphologies: "carrot" and "bulbous," that reflect different structural/compositional properties of the impactors. Carrot type tracks are typically produced by compact or single mineral grains which survive essentially intact as a single large terminal particle. Bulbous tracks are likely produced by fine-grained or organic-rich impactors [1]. Owing to their challenging nature and especially high value of Stardust samples, we have invested considerable effort in developing both sample preparation and analytical techniques tailored for Stardust sample analyses. Our report focuses on our systematic disassembly and coordinated analysis of Stardust carrot track #112 from the mm to nm-scale.

Nakamura-Messenger, K.↗

Blood Collection

The method that is used for the collection, storage and real-time analysis of blood and other bodily fluids has been licensed to DBCD, Inc. by NASA. The result of this patent licensing agreement has been the development of a commercial product that can provide serum or plasma from whole blood volumes of 20 microliters to 4 milliliters. The device has a fibrous filter with a pore size of less than about 3 microns, and is coated with a mixture of mannitol and plasma fraction protein. The coating causes the cellular fraction to be trapped by the small pores, leaving the cellular fraction intact on the fibrous filter while the acellular fraction passes through the filter for collection in unaltered form from the serum sample collection chamber. The method used by this product is useful to NASA for blood analysis on manned space missions.

Source record↗

Laser Subdivision of the Genesis Concentrator Target Sample 60000

The Genesis Allocation Committee received a request for ~ 1 square centimeter of the diamond-like-carbon (DLC) concentrator target for the analysis of solar wind nitrogen isotopes. The target consists of a single crystal float zone (FZ) silicon substrate having a thickness on the order of 550 micrometers with a 1.5-3.0 micrometer-thick coating of DLC on the exposed surface. The solar wind is implanted shallowly in the front side DLC. The original target was a circular quadrant with a radius of 3.1 cm; however, the piece did not survive intact when the spacecraft suffered an anomalous landing upon returning to Earth on September 8, 2004. An estimated 75% of the DLC target was recovered in at least 18 fragments. The largest fragment, Genesis sample 60000, has been designated for this allocation and is the first sample to be subdivided using our laser scribing system Laser subdivision has associated risks including thermal diffusion of the implant if heating occurs and unintended breakage during cleavage. A careful detailed study and considerable subdividing practice using non-flight FZ diamond on silicon, DOS, wafers has considerably reduced the risk of unplanned breakage during the cleaving process. In addition, backside scribing reduces the risk of possible thermal excursions affecting the implanted solar wind, implanted shallowly in the front side DLC.

Lauer, Howard V., Jr.↗

Stardust Interstellar Preliminary Examination IV: Scanning Transmission X-Ray Microscopy Analyses of Impact Features in the Stardust Interstellar Dust Collector

We report the quantitative characterization by synchrotron soft X-ray spectroscopy of 31 potential impact features in the aerogel capture medium of the Stardust Interstellar Dust Collector. Samples were analyzed in aerogel by acquiring high spatial resolution maps and high energy-resolution spectra of major rock-forming elements Mg, Al, Si, Fe, and others. We developed diagnostic screening tests to reject spacecraft secondary ejecta and terrestrial contaminants from further consideration as interstellar dust candidates. The results support an extraterrestrial origin for three interstellar candidates: I1043,1,30 (Orion) is a 3 pg particle with Mg-spinel, forsterite, and an iron-bearing phase. I1047,1,34 (Hylabrook) is a 4 pg particle comprising an olivine core surrounded by low-density, amorphous Mg-silicate and amorphous Fe, Cr, and Mn phases. I1003,1,40 (Sorok) has the track morphology of a high-speed impact, but contains no detectable residue that is convincingly distinguishable from the background aerogel. Twenty-two samples with an anthropogenic origin were rejected, including four secondary ejecta from impacts on the Stardust spacecraft aft solar panels, nine ejecta from secondary impacts on the Stardust Sample Return Capsule, and nine contaminants lacking evidence of an impact. Other samples in the collection included I1029,1,6, which contained surviving solar system impactor material. Four samples remained ambiguous: I1006,2,18, I1044,2,32, and I1092,2,38 were too dense for analysis, and we did not detect an intact projectile in I1044,3,33. We detected no radiation effects from the synchrotron soft X-ray analyses; however, we recorded the effects of synchrotron hard X-ray radiation on I1043,1,30 and I1047,1,34.

Dust↗

Automated, Miniaturized Instrument for Measuring Gene Expression in Space

To facilitate astrobiological studies on the survival and adaptation of microorganisms and mixed microbial cultures to space environment, we have been developing a fully automated, miniaturized system for measuring their gene expression on small spacecraft. This low-cost, multi-purpose instrument represents a major scientific and technological advancement in our ability to study the impact of the space environment on biological systems by providing data on cellular metabolism and regulation orders of magnitude richer than what is currently available. The system supports growth of the organism, lyse it to release the expressed RNA, label the RNA, read the expression levels of a large number of genes by microarray analysis of labeled RNA and transmit the measurements to Earth. To measure gene expression we use microarray technology developed by CombiMatrix, which is based on electrochemical reactions on arrays of electrodes on a semiconductor substrate. Since the electrical integrity of the microarray remains intact after probe synthesis, the circuitry can be employed to sense nucleic acid binding at each electrode. CombiMatrix arrays can be sectored to allow multiple samples per chip. In addition, a single array can be used for several assays. The array has been integrated into an automated microfluidic cartridge that uses flexible reagent blisters and pinch pumping to move liquid reagents between chambers. The proposed instrument will help to understand adaptation of terrestrial life to conditions beyond the planet of origin, identify deleterious effects of the space environment, develop effective countermeasures against these effects, and test our ability to sustain and grow in space organisms that can be used for life support and in situ resource utilization during long-duration space exploration. The instrument is suitable for small satellite platforms, which provide frequent, low cost access to space. It can be also used on any other platform in space, including the ISS. It can be replicated and used with only small modifications in multiple biological experiments with a broad range of goals in mind.

Pohorille, A.↗

The NASA Orbital Debris Engineering Model 3.1: Development, Verification, and Validation

The NASA Orbital Debris Program Office has developed the Orbital Debris Engineering Model (ORDEM) primarily as a tool for spacecraft designers and other users to understand the long-term risk of collisions with orbital debris. The newest version, ORDEM 3.1, incorporates the latest and highest fidelity datasets available to build and validate representative orbital debris populations encompassing low Earth orbit (LEO) to geosynchronous orbit (GEO) altitudes for the years 2016-2050. ORDEM 3.1 models fluxes for object sizes > 10 μm within or transiting LEO and > 10 cm in GEO. The deterministic portion of the populations in ORDEM 3.1 is based on the U.S. Space Surveillance Network (SSN) catalog, which provides coverage down to approximately 10 cm in LEO and 1 m in GEO. Observational datasets from radar, in situ, and optical sources provide a foundation from which the model populations are statistically extrapolated to smaller sizes and orbit regions that are not well-covered by the SSN catalog, yet may pose the greatest threat to operational spacecraft. Objects in LEO ranging from approximately 5 mm to 10 cm are modeled using observational data from ground-based radar, namely the Haystack Ultrawideband Satellite Imaging Radar (HUSIR – formerly known as Haystack). The LEO population smaller than approximately 3 mm in size is characterized based on a reanalysis of in situ data from impacts to the windows and radiators of the U.S. Space Transportation System orbiter vehicle, i.e., the Space Shuttle. Data from impacts on the Hubble Space Telescope are also used to validate the sub-millimeter model populations in LEO. Debris in GEO with sizes ranging from 10 cm to 1 m is modeled using optical measurement data from the Michigan Orbital DEbris Survey Telescope (MODEST). Specific, major debris-producing events, including the Fengyun-1C, Iridium 33, and Cosmos 2251 debris clouds, and unique populations, such as sodium-potassium droplets, have been re-examined and are modeled and added to the ORDEM environment separately. The debris environment greater than 1 mm is forecast using NASA’s LEO-to- GEO ENvironment Debris model (LEGEND). Future explosions of intact objects and collisions involving objects greater than 10 cm are assessed statistically, and the NASA Standard Satellite Breakup Model is used to generate fragments from these events. Fragments smaller than 10 cm are further differentiated based on material density categories, i.e., high-, medium-, and low-density, to better characterize the potential debris risk posed to spacecraft. The future projection of the sub-millimeter environment is computed using a special small-particle degradation model where small particles are created from intact spacecraft and rocket bodies. This work discusses the development, features, and capabilities of the ORDEM 3.1 model; the ne new data analyses used to build the model populations; and sample verification and validation results.

Matney, M.↗

The LDCE Particle Impact Experiment as flown on STS-46

Many materials and techniques have been developed by the authors to sample the flux of particles in Low Earth Orbit (LEO). Though regular in-site sampling of the flux in LEO the materials and techniques have produced data which compliment the data now being amassed by the Long Duration Exposure Facility (LDEF) research activities. Orbital debris models have not been able to describe the flux of particles with d sub p less than or = 0.05 cm, because of the lack of data. Even though LDEF will provide a much needed baseline flux measurement, the continuous monitoring of micron and sub-micron size particles must be carried out. A flight experiment was conducted on the Space Shuttle as part of the LDCE payload to develop an understanding of the Spatial Density (concentration) as a function of size (mass) for particle sizes 1 x 10(exp 6) cm and larger. In addition to the enumeration of particle impacts, it is the intent of the experiment that hypervelocity particles be captured and returned intact. Measurements will be performed post flight to determine the flux density, diameters, and subsequent effects on various optical, thermal control and structural materials. In addition to these principal measurements, the Particle Impact Experiment (PIE) also provides a structure and sample holders for the exposure of passive material samples to the space environment, e.g., thermal cycling, and atomic oxygen, etc. The experiment will measure the optical property changes of mirrors and will provide the fluence of the ambient atomic oxygen environment to other payload experimenters. In order to augment the amount of material returned in a form which can be analyzed, the survivability of the experiment as well as the captured particles will be assessed. Using Sandia National Laboratory's hydrodynamic computer code CTH, hypervelocity impacts on the materials which comprise the experiments have been investigated and the progress of these studies are reported.

Maag, Carl R.↗

Stability Analysis of ISS Medications

It is known that medications degrade over time, and that extreme storage conditions will hasten their degradation. The temperature and humidity conditions of the ISS have been shown to be within the ideal ranges for medication storage, but the effects of other environmental factors, like elevated exposure to radiation, have not yet been evaluated. Current operational procedures ensure that ISS medications are re-stocked before expiration, but this may not be possible on long duration exploration missions. For this reason, medications that have experienced long duration storage on the ISS were returned to JSC for analysis to determine any unusual effects of aging in the low- Earth orbit environment. METHODS Medications were obtained by the JSC Pharmacy from commercial distributors and were re-packaged by JSC pharmacists to conserve up mass and volume. All medication doses were part of the ISS crew medical kit and were transported to the International Space Station (ISS) via NASA's Shuttle Transportation System (Space Shuttle). After 568 days of storage, the medications were removed from the supply chain and returned to Earth on a Dragon (SpaceX) capsule. Upon return to Earth, medications were transferred to temperature and humidity controlled environmental chambers until analysis. Nine medications were chosen on the basis of their availability for study. The medications included several of the most heavily used by US crewmembers: 2 sleep aids, 2 antihistamines/decongestants, 3 pain relievers, an antidiarrheal and an alertness medication. Each medication was available at a single time point; analysis of the same medication at multiple time points was not possible. Because the samples examined in this study were obtained opportunistically from medical supplies, there were no control samples available (i.e. samples aged for a similar period of time on the ground); a significant limitation of this study. Medications were analyzed using the HPLC/MS methods described in the United States Pharmacopeia (USP) to measure the amount of intact active ingredient, identify degradation products and measure their amounts. Some analyses were conducted by an independent analytical laboratory, but certain (Schedule) medications could not be shipped to their facility and were analyzed at JSC. RESULTS Nine medications were analyzed with respect to active pharmaceutical ingredient (API) and degradant amounts. Results were compared to the USP requirements for API and degradants/impurities content for every FDA-approved medication. One medication met USP requirements at 5 months after its expiration date. Four of the nine (44% of those tested) medications tested met USP requirements up to 8 months post-expiration. Another 3 medications (33% of those tested) met USP guidelines 2-3 months before expiration. One medication, a compound classed by the FDA as a dietary supplement and sometimes used as a sleep aid, failed to meet USP requirements at 11 months post-expiration. CONCLUSION Analysis of each medication at a single time point provides limited information on the stability of a medication stored in particular conditions; it is not possible to predict how long a medication may be safe and effective from these data. Notwithstanding, five of the nine medications tested (56%) met USP requirements for API and degradants/impurities at least 5 months past expiration dates. The single compound that failed to meet USP requirements is not regulated as strictly as prescription medications are during manufacture; it is unknown if this medication would have met the requirements prior to flight. Notably, it was the furthest beyond its expiration date. Only more comprehensive analysis of flight-aged samples compared to appropriate ground controls will permit determination of spaceflight effects on medication stability.

Wotring, V. E.↗

Vesta Evolution from Surface Mineralogy: Mafic and Ultramafic Mineral Distribution

Vesta is the only intact, differentiated, rocky protoplanet and it is the parent body of HED meterorites. Howardite, eucrite and diogenite (HED) meteorites represent regolith, basaltic-crust, lower-crust and possibly ultramafic-mantle samples of asteroid Vesta. Only a few of these meteorites, the orthopyroxene-rich diogenites, contain olivine, a mineral that is a major component of the mantles of differentiated bodies, including Vesta. The HED parent body experienced complex igneous processes that are not yet fully understood and olivine and diogenite distribution is a key measurement to understand Vesta evolution. Here we report on the distribution of olivine and its constraints on vestan evolution models.

DeSanctis, M. C.↗

Responses of Florida Scrub Vegetation to Water Additions from a Groundwater Treatment Project and to Hurricane Disturbance

Florida scrub is a fire-maintained shrub vegetation of well-drained, sandy soils; dominant species include several species of Quercus and Serenoa repens. In a remediation project, treated groundwater was distributed through an exfiltration gallery into intact scrub. We established eight permanent line-intercept transects (15 m length) in the site in April 2002, four close to the exfiltration gallery and four more distant from it. We sampled vegetation, < 0.5 m and ≥ 0.5 m, along each transect and measured vegetation height at four points (0, 5, 10, 15 m) annually through 2019. The initial phase of the project operated from October 2002 to early March 2004 (494 days) and distributed 1.74 x 10^8 L of water. The final phase of the project occurred from March 2005 through August 2008 (1251 days) and distributed 1.90 x 10^8 L of water. Pumping raised the water table near the exfiltration gallery. Vegetation height did not differ between the near and far transects initially. Vegetation height increased in the near transects by 2004 with the greatest percent change in 2003 and 2004 as did total cover ≥ 0.5 m. Total cover < 0.5 m and bare ground were similar initially in the near and far transects and declined in the near transects by 2004. Scrub species, particularly the dominant scrub oaks, increased height and cover in response to water additions with no loss of dominant scrub species and no establishment of mesophytes. Hurricane Frances (September 2004) reduced cover ≥ 0.5 m the following year. Hurricane Matthew (October 2016) and Hurricane Irma (September 2017) caused greater damage including breaking limbs as reflected in reduced height and total cover ≥ 0.5 m probably because the older, taller scrub was more vulnerable to wind damage.

Florida scrub↗

The Stuff of Other Worlds

Extraterrestrial material eternally rains down on Earth. Meteorites flare in the night sky. Cosmic rays plow into Earth's atmosphere, creating invisible bursts of secondary particles. These processes began when the Earth formed in the primordial solar system and have continued ever since, indifferent to the exceedingly recent presence of human intelligence. For us to seek out stuff of other worlds, in contrast, takes a great deal of determined ingenuity. First we have to send a spacecraft somewhere else in the solar system. Indigenous material has to be collected and then brought back to Earth without exposure to conditions that might significantly alter it. The material must undergo meaningful scientific analysis. Most important, part of the material is preserved intact for future investigations. Beginning with bringing back Moon rocks, and now moving onward in the form of new missions to capture the hot thin solar wind and cold thin atmosphere of comets, extraterrestrial sample return takes place on the cutting edge of scientific technology. Sample return is also the fulcrum of an energetic debate about how to do planetary science missions. Scientists and engineers are debating whether to rely on remote sensing and in situ analysis, or to plan missions to undertake sample return. The latter is definitely more expensive on a per mission basis, and is usually technologically more challenging. But for an initially high investment of money and technology, bringing the stuff of other worlds back to Earth yields an incomparable return in scientific results.

Stansbery, EIleen K.↗

Contaminated Solar Array Handrail Samples Retrieved From Mir Analyzed

In January 1998 during the shuttle STS 89 mission, an eight-section Russian solar array panel was retrieved after more than 10 years of exposure to the orbital space environment on Mir. The array was deployed June 16, 1987, and removed on November 3, 1997. It had been actively used as a source of electrical power for 8 years. This operational array had been located on the Mir core module, located directly above the Kvant-2 module. Its retrieval provided a unique opportunity to study the effects of the low-Earth-orbit environment on a functional solar array. The intact solar array underwent scientific inspections and preliminary tests by a joint team of U.S. and Russian investigators to evaluate the effects of long-term space exposure. Upon initial examination, significant contamination was observed over most components of the array. One panel, panel 8, was provided to the U.S. scientists for further evaluation. As part of the U.S. investigations, two solar array handrail samples from panel 8 were evaluated for contamination at the NASA Glenn Research Center at Lewis Field. One is a section of a rigid handrail, and the other is a section of woven fabric tape that was overwrapped around a flexible handhold. Both the flexible handhold woven fabric and the rigid handrail were significantly darkened after 10 years of space exposure. They were evaluated with optical microscopy, field emission scanning electron microscopy (FESEM), and energy-dispersive spectroscopy. Solar absorptance and room-temperature emittance values also were obtained. The returned contaminated solar array segment is very similar in design to the solar arrays being supplied by the Russians for the International Space Station. Therefore, it was desirable to determine what the contaminants on various surfaces are and what the sources of the contamination were.

deGroh, Kim K.↗

Characterization of Meteorites by Focused Ion Beam Sectioning: Recent Applications to CAIs and Primitive Meteorite Matrices

Focused ion beam (FIB) sectioning has revolutionized preparation of meteorite samples for characterization by analytical transmission electron microscopy (TEM) and other techniques. Although FIB is not "non-destructive" in the purest sense, each extracted section amounts to no more than nanograms (approximately 500 cubic microns) removed intact from locations precisely controlled by SEM imaging and analysis. Physical alteration of surrounding material by ion damage, fracture or sputter contamination effects is localized to within a few micrometers around the lift-out point. This leaves adjacent material intact for coordinate geochemical analysis by SIMS, microdrill extraction/TIMS and other techniques. After lift out, FIB sections can be quantitatively analyzed by electron microprobe prior to final thinning, synchrotron x-ray techniques, and by the full range of state-of-the-art analytical field-emission scanning transmission electron microscope (FE-STEM) techniques once thinning is complete. Multiple meteorite studies supported by FIB/FE-STEM are currently underway at NASA-JSC, including coordinated analysis of refractory phase assemblages in CAIs and fine-grained matrices in carbonaceous chondrites. FIB sectioning of CAIs has uncovered epitaxial and other overgrowth relations between corundum-hibonite-spinel consistent with hibonite preceding corundum and/or spinel in non-equilibrium condensation sequences at combinations of higher gas pressures, dust-gas enrichments or significant nebular transport. For all of these cases, the ability of FIB to allow for coordination with spatially-associated isotopic data by SIMS provides immense value for constraining the formation scenarios of the particular CAI assemblage. For carbonaceous chondrites matrix material, FIB has allowed us to obtain intact continuous sections of the immediate outer surface of Murchison (CM2) after it has been experimentally ion processed to simulate solar wind space weathering. The surface amorphization and loss of OH produced by the irradiation provides important clues regarding space weathering on primitive asteroids such as the OSIRIS-Rex target 101955 Bennu.

Christoffersen, Roy↗

The Non-Destructive Separation of Diverse Astrobiologically Relevant Organic Molecules By Customizable Capillary Zone Electrophoresis and Monolithic Capillary Electrochromatography

The in situ detection of organic molecules in space is key to understanding the variety and the distribution of the building blocks of life, and possibly the detection of extraterrestrial life itself. Gas chromatography mass spectrometry (GC-MS) has been the most sensitive analytical instrument for organic analyses in flight, and was used on missions from NASA’s Viking, Phoenix, Curiosity missions to ESA’s Rosetta space probe. While pyrolysis GC-MS revealed the first organics on Mars, this step alters or degrades certain fragile molecules that are excellent biosignatures including polypeptides, oligonucleotides and polysaccharides, rendering the intact precursors undetectable. We have identified a solution tailored to the detection of biopolymers and other biomarkers by the use of liquid-based capillary electrophoresis and electrochromatography. In this study, we show that a capillary electrochromatography (CEC) approach using monolithic stationary phases with tailor-made surface chemistry can separate and identify various polycyclic aromatic hydrocarbons (PAHs), nucleobases and aromatic acids that could be formed under astrophysically relevant conditions. In order to simulate flyby organic sample capture, we conducted hypervelocity impact experiments which consisted of accelerating peptide-soaked montmorillonite particles to a speed of 5.6 km/sec, and capturing them in an amorphous silica aerogel of 10 and 30 mg/cc bulk density. Bulk peptide extraction from aerogel followed by capillary zone electrophoresis led to the detection of only two stereoisomeric peptide peaks. The recovery rates of each step of the extraction procedure after the hypervelocity impact suggest that major peptide loss occurred during the impact. Our study provides initial exploration of feasibility of this approach for capturing intact peptides, and subsequently detecting candidate biomolecules during flight missions that would be missed by GC-MS alone. As the monolith-based electrochromatography technology could be customized to detect specific classes of compounds as well as miniaturized, these results demonstrate the potential of the instrumentation for future astrobiology-related spaceflight missions.

Flyby sample return↗