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NASA NTRS2003

STS-113/11A: Assessment of Air Quality in the International Space Station (ISS) and Space Shuttle Based on Samples Returned in December 2002 and in May 2003 aboard Soyuz 5

The toxicological assessments of grab sample canisters (GSCs) returned aboard STS-l13 and Soyuz 5 are reported. Analytical methods have not changed from earlier reports. Surrogate standard recoveries from the GSCs were 79-120% except as noted in the table. One sample was returned with the valve opened. 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 and formaldehyde contributions). Control of atmospheric alcohols is important to the water recovery system engineers, hence total alcohols (including acetone) are also shown for each sample. Octafluoropropane (OFP) has leaked from heat-exchange units in large quantities, so its concentration is tracked separately. Because formaldehyde is quantified from sorbent badges, its concentration is also listed separately. The table shows that the air quality in general was acceptable for crew respiration through the middle of December 2002. No conclusions can be made about the air quality after that date due to NASA's inability to return air samples from the ISS . Alcohols are not being controlled to the recently lowered guideline of 5 mg/m3, which was recommended to protect the water recovery systems. The airlock sample was taken during the regeneration of Met ox canisters in the adjacent Node. The trace pollutants were not increased above background; however, inspection of table 1 in the appendix shows a CO2 concentration of 17,000 mg/cu m, which is a relatively high concentration, but still below the 24-hour SMAC of23,000 mg/cu m. The control of OFP continues to be adequate at least through December 2002. Formaldehyde concentrations suggest that the high levels that were being found in the Lab atmosphere have subsided. This is probably attributable to the restoration of IMV in early February 2003 . Before the obstructing material was removed from ducts the Lab formaldehyde concentrations approached 0.06 mg/cu m, whereas after the repair the levels were near 0.04 mg/m3 . This does not mean that local sources in the Lab have been reduced, only that the excess of formaldehyde produced in the Lab is distributed into the whole volume of the ISS.

James, John T.↗
NASA NTRS2016

Microorganisms, Organic Carbon, and Their Relationship with Oxidant Activity in Hyper-Arid Mars-Like Soils: Implications for Soil Habitability

Soil samples from the hyper-arid region in the Atacama 23 Desert in Southern Peru (La Joya Desert) were analyzed for total and labile organic carbon (TOC & LOC), phospholipid fatty acids analysis (PLFA), quantitative real time polymerase chain reaction (qRT-PCR), 4',6- diamidino-2-phenylindole (DAPI)-fluorescent microscopy, culturable microorganisms, and oxidant activity, in order to understand the relationship between the presence of organic matter and microorganisms in these types of soils. TOC content levels were similar to the labile pool of carbon suggesting the absence of recalcitrant carbon in these soils. The range of LOC was from 2 to 60 micro-g/g of soil. PLFA analysis indicated a maximum of 2.3 x 10(exp 5) cell equivalents/g. Culturing of soil extracts yielded 1.1 x 10(exp 2)-3.7 x 10(exp 3) CFU/g. qRT-PCR showed between 1.0 x 10(exp 2) and 8 x 10(exp 3) cells/g; and DAPI fluorescent staining indicated bacteria counts up to 5 x 104 cells/g. Arid and semiarid samples (controls) showed values between 10(exp 7) and 10(exp 11) cells/g with all of the methods used. Importantly, the concentration of microorganisms in hyper-arid soils did not show any correlation with the organic carbon content; however, there was a significant dependence on the oxidant activity present in these soil samples evaluated as the capacity to decompose sodium formate in 10 hours. We suggest that the analysis of oxidant activity could be a useful indicator of the microbial habitability in hyper-arid soils, obviating the need to measure water activity over time. This approach could be useful in astrobiological studies on other worlds.

Mars-like soils↗
NASA NTRS1993

Galileo photometry of Apollo landing sites

As of December 1992, the Galileo spacecraft performed its second and final flyby (EM2), of the Earth-Moon system, during which it acquired Solid State Imaging (SSI) camera images of the lunar surface suitable for photometric analysis using Hapke's, photometric model. These images, together with those from the first flyby (EM1) in December 1989, provide observations of all of the Apollo landing sites over a wide range of photometric geometries and at eight broadband filter wavelengths ranging from 0.41 micron to 0.99 micron. We have completed a preliminary photometric analysis of Apollo landing sites visible in EM1 images and developed a new strategy for a more complete analysis of the combined EM1 and EM2 data sets in conjunction with telescopic observations and spectrogoniometric measurements of returned lunar samples. No existing single data set, whether from spacecraft flyby, telescopic observation, or laboratory analysis of returned samples, describes completely the light scattering behavior of a particular location on the Moon at all angles of incidence (i), emission (e), and phase angles (a). Earthbased telescopic observations of particular lunar sites provide good coverage of incidence nad phase angles, but their range in emission angle is limited to only a few degrees because of the Moon's synchronous rotation. Spacecraft flyby observations from Galileo are now available for specific lunar features at many photometric geometries unobtainable from Earth; however, this data set lacks coverage at very small phase angles (a less than 13 deg) important for distinguishing the well-known 'opposition effect'. Spectrogoniometric measurements from returned lunar samples can provide photometric coverage at almost any geometry; however, mechanical properties of prepared particulate laboratory samples, such as particle compaction and macroscopic roughness, likely differ from those on the lunar surface. In this study, we have developed methods for the simultaneous analysis of all three types of data: we combine Galileo and telescopic observations to obtain the most complete coverage with photometric geometry, and use spectrogoniometric observations of lunar soils to help distinguish the photometric effects of macroscopic roughness from those caused by particle phase function behavior (i.e., the directional scattering properties of regolith particles).

Helfenstein, P.↗
NASA NTRS1993

Synthesis of phthalocyanine doped sol-gel materials

The synthesis of sol-gel silica materials doped with three different types of metallophthalocyanines has been studied. Homogeneous materials of good optical quality were prepared and the first optical limiting measurements of dyes in sol-gel hosts were carried out. The properties of these solid state limiters are similar to limiters based on phthalocyanine (Pc) in solution. Sol-gel silica materials containing copper, tin and germanium phthalocyanines were investigated. The initial step in all cases was to prepare silica sols by the sonogel method using tetramethoxy silane (TMOS), HCl and distilled water. Thereafter, the synthesis depended upon the specific Pc and its solubility characteristics. Copper phthalocyanine tetrasulfonic acid tetra sodium salt (CuPc4S) is soluble in water and various doping levels (1 x 10 (exp -4) M to 1 x 10 (exp -5) M) were added to the sol. The group IV Pc's, SnPc(OSi(n-hexyl)3)2 and GePc(OSi(n-hexyl)3)2, are insoluble in water and the process was changed accordingly. In these cases, the compounds were dissolved in THF and then added to the sol. The Pc concentration in the sol was 2 x 10(exp -5)M. The samples were then aged and dried in the standard method of making xerogel monoliths. Comparative nanosecond optical limiting experiments were performed on silica xerogels that were doped with the different metallophthalocyanines. The ratio of the net excited state absorption cross section (sigma(sub e)) to the ground state cross section (sigma(sub g)) is an important figure of merit that is used to characterize these materials. By this standard the SnPc sample exhibits the best limiting for the Pc doped sol-gel materials. Its cross section ratio of 19 compares favorably with the value of 22 that was measured in toluene. The GePc materials appear to not be as useful as those containing SnPc. The GePc doped solids exhibit a higher onset energy (2.5 mj and lower cross section ratio, 7. The CuPc4S sol-gel material has a still lower cross section ratio, 4, however, the tetrasulfonate groups make the dye soluble in water which greatly facilitates its incorporation into the sol-gel matrix. The nonlinear transmission of CuPc4S in a pH 2 buffer solution and in a silica xerogel were compared. It is evident that the CuPc4S preserves its optical limiting behavior in the sol-gel matrix, indicating that the fundamental excited state absorption process is essentially the same for a molecule in solution or in the solid state. Although the spectroscopic details of energy level lifetimes are unknown, the significance is that passive optical limiting has been achieved in the solid state via incorporation of a dye into an inorganic host. The only compromise occurs at the extremely high energy regime where photobleaching is observed. This is a result of the limited mobility of the dye molecules in the solid silica host relative to a liquid host. The effects of photodegradation in the xerogel are additive, whereas the solution provides a supply of fresh molecules that are free to enter the active volume between pulses.

Dunn, Bruce↗
NASA NTRS2013

The Search for Nitrates on Mars by the Sample Analysis at Mars (SAM) Instrument

Planetary models suggest that nitrogen was abundant in the early Martian atmosphere as N2 but it was lost by sputtering and photochemical loss to space, impact erosion, and chemical oxidation to nitrates. A nitrogen cycle may exist on Mars where nitrates, produced early in Mars' history, may have been later decomposed back into N2 by the current impact flux. Nitrates are a fundamental source of nitrogen for terrestrial microorganisms, and they have evolved metabolic pathways to perform both oxidation and reduction to drive a complete biological nitrogen cycle. Therefore, the characterization of nitrogen in Martian soils is important to assess habitability of the Martian environment, particularly with respect to the presence of nitrates. The only previous mission that was designed to search for soil nitrates was the Phoenix mission but N-containing species were not detected by TEGA or the MECA WCL. Nitrates have been tentatively identified in Nakhla meteorites, and if nitrogen was oxidized on Mars, this has important implications for the habitability potential of Mars. Here we report the results from the Sample Analysis at Mars (SAM) instrument suite aboard the Curiosity rover during the first year of surface operations in Gale Crater. Samples from the Rocknest aeolian deposit and sedimentary rocks (John Klein) were heated to approx 835degC under helium flow and the evolved gases were analyzed by MS and GC-MS. Two and possibly three peaks may be associated with the release of m/z 30 at temperatures ranging from 180degC to 500degC. M/z 30 has been tentatively identified as NO; other plausible contributions include CH2O and an isotopologue of CO, 12C18O. NO, CH2O, and CO may be reaction products of reagents (MTBSTFA/DMF) carried from Earth for the wet chemical derivatization experiments with SAM and/or derived from indigenous soil nitrogenated organics. Laboratory analyses indicate that it is also possible that <550degC evolved NO is produced via reaction of HCl with nitrates arising from the decomposition of perchlorates. All sources of m/z 30 whether it be martian or terrestrial will be considered and their implications for Mars will be discussed.

Navarro-Gonzalez, Rafael↗
NASA NTRS1985

Scientific objectives for a 1996 Mars Sample Return Mission

The Mars Sample Return Mission, designed to return a variety of surface and subsurface samples as well as atmospheric samples, is described. Primary information about the planet is essential to understanding its place in the evolution of the solar system. The most accurate landing techniques will be used to place the lander near geologically interesting features. A capable rover will be an essential element of the sample collection strategy to maximize the diversity of the samples. The sample collection and return systems will keep the samples at Mars ambient conditions or colder to preserve the abundances and distribution of volatile components. Planetary quarantine is an important consideration for both the Mars lander and the earth return vehicle. Quarantine procedures must be consistent with the primary objectives of the mission and must not compromise the investigations of the returned samples.

Blanchard, D. P.↗
NASA NTRS1995

Basic principles and recent observations of rotationally sampled wind

The concept of rotationally sampled wind speed is described. The unusual wind characteristics that result from rotationally sampling the wind are shown first for early measurements made using an 8-point ring of anemometers on a vertical plane array of meteorological towers. Quantitative characterization of the rotationally sampled wind is made in terms of the power spectral density function of the wind speed. Verification of the importance of the new concept is demonstrated with spectral analyses of the response of the MOD-OA blade flapwise root bending moment and the corresponding rotational analysis of the wind measured immediately upwind of the MOD-OA using a 12-point ring of anemometers on a 7-tower vertical plane array. The Pacific Northwest Laboratory (PNL) theory of the rotationally sampled wind speed power spectral density function is tested successfully against the wind spectrum measured at the MOD-OA vertical plane array. A single-tower empirical model of the rotationally sampled wind speed is also successfully tested against the measurements from the full vertical plane array. Rotational measurements of the wind velocity with hotfilm anemometers attached to rotating blades are shown to be accurate and practical for research on winds at the blades of wind turbines. Some measurements at the rotor blade of a MOD-2 turbine using the hotfilm technique in a pilot research program are shown. They are compared and contrasted to the expectations based upon application of the PNL theory of rotationally sampled wind to the MOD-2 size and rotation rate but without teeter, blade bending, or rotor induction accounted for. Finally, the importance of temperature layering and of wind modifications due to flow over complex terrain is demonstrated by the use of hotfilm anemometer data, and meteorological tower and acoustic doppler sounder data from the MOD-2 site at Goodnoe Hills, Washington.

Connell, James R.↗
NASA NTRS1971

Preliminary description of Apollo 15 sample environments

Approximately 78 kg of lunar rock and soil samples were returned by Apollo 15. The rather complete documentation of the locations of nearly all of the samples allows for relating the samples to the specific and detailed geologic environments from which they were collected. This is especially important in an area as geologically complex as the Hadley-Apennine site. All of the material presented was derived from the pre-mission photogeologic maps, lunar surface television video tapes, air-to-ground transcript and crew debriefings, photographs taken on the lunar surface by the Apollo 15 crew, and information supplied by the Lunar Sample Preliminary Examination team from which the samples were categorized into groups consisting of, broadly, basalts and breccias. The breccias are considered loosely in terms of coherent breccias and soil breccias.

Swann, G. A.↗
NASA NTRS2004

Discrete X-Ray Source Populations and Star-Formation History in Nearby Galaxies

This program aims in understanding the connection between the discrete X-ray source populations observed in nearby galaxies and the history of star-formation in these galaxies. The ultimate goal is to use this knowledge in order to constrain X-ray binary evolution channels. For this reason although the program is primarily observational it has a significant modeling component. During the first year of this study we focused on the definition of a pilot sample of galaxies with well know star-formation histories. A small part of this sample has already been observed and we performed initial analysis of the data. However, the majority of the objects in our sample either have not been observed at all, or the detection limit of the existing observations is not low enough to probe the bulk of their young X-ray binary populations. For this reason we successfully proposed for additional Chandra observations of three targets in Cycle-5. These observations are currently being performed. The analysis of the (limited) archival data for this sample indicated that the X-ray luminosity functions (XLF) of the discrete sources in these galaxies may not have the same shape as is widely suggested. However, any solid conclusions are hampered by the small number of detected sources. For this reason during the second year of this study, we will try to extend the sample in order to include more objects in each evolutionary stage. In addition we are completing the analysis of the Chandra monitoring observations of the Antennae galaxies. The results from this work, apart from important clues on the nature of the most luminous sources (Ultra-luminous X-ray sources; ULXs) provide evidence that source spectral and/or temporal variability does not significantly affect the shape of their X-ray luminosity functions. This is particularly important for comparisons between the XLFs of different galaxies and comparisons with predictions from theoretical models. Results from this work have been presented in several conferences. Refereed journal papers presenting these conclusions are currently in preparation. An important part of this study is the Chandra survey of the Small Magellanic Cloud, our second nearest star- forming galaxy. So far we have been awarded 5 Chandra observations of the central youngest part of the galaxy. These observations will help to study the very faint end of the young X-ray binary populations which is not possible to probe in more distant objects. Results from this study have been presented in several conferences and two papers are in preparation. In addition during year-2 we are planning of undertaking the task of identifying optical counterparts to the X-ray sources, which will help us to isolate interlopers (sources not associated with the SMC) and classify the X-ray binaries which are found to be associated with the SMC. In the theoretical front, the Star-Track X-ray binary population synthesis code which will be used for the modeling of the X-ray binary populations (led by co-I V. Kalogera and C. Belczynski), is complete. A first test using the XLF of the star-forming galaxy NGC-1569 showed remarkable agreement between the observed and the modeled XLF. These results are presented in an ApJ. Letters paper (Belczynski et al, 2004, 601, 147). During year-2 of this study we are planning of performing a parameter study in order to investigate which parameters are most important for the shape of the XLF. In addition we will perform comparisons with observations of other galaxies from our sample as they become available.

Zezas, Andreas↗
NASA NTRS1994

Measuring track densities in lunar grains using image analysis

We have used digitized scanning electron micrographs and computer image analysis programs to measure track densities in lunar soil grains. Tracks were formed by highly ionizing solar energetic particles and cosmic rays. Back-scattered electron images produced suitable high contrast images for analysis. We used computer counting and measurement of area to obtain track densities. We found an excellent correlation with manual measurements for track densities below 1x10(exp 8) cm(exp -2). For track densities between 1x10(exp 8) to 1x10(exp 9) cm(exp -2) we found that a regression formula using the percentage area covered by tracks gave good agreement with manual measurements. Measurement of tract densities in lunar samples has been a very rewarding technique for measuring exposure ages and soil maturation processes. We have shown that we can reliably measure track densities in lunar grains using image analysis techniques. Automating track counting may allow application of this technique to important problems in regolith dynamics including the ratio of radiation exposure to reworking in various surface and core samples and in regolith breccias.

Blanford, G. E.↗
NASA NTRS1994

Opportunity to sample something different: The dark, unweathered, mafic sands of Cerberus and the Pathfinder 1997 Mars landing

A very important surface component, typically described as 'dark gray material', was not seen at the Viking lander sites, but is common to all low-albedo regions on Mars. Dark material probably includes unaltered mafic volcanic and/or crustal rock and soil not coated by dust, weathering rinds, or varnish. A Pathfinder landing in Cerberus (9 deg N - 16 deg N, 194 deg W - 215 deg W) will guarantee examination of materials that are distinctly different from the two Viking lander sites. In situ study of dark material will provide vital ground truth for orbiter-based observations like those anticipated from Mars '94/'96 and Mars Global Surveyor.

Edgett, Kenneth S.↗
NASA NTRS2007

Development of Natural Flaw Samples for Evaluating Nondestructive Testing Methods for Foam Thermal Protection Systems

Low density polyurethane foam has been an important insulation material for space launch vehicles for several decades. The potential for damage from foam breaking away from the NASA External Tank was not realized until the foam impacts on the Columbia Orbiter vehicle caused damage to its Leading Edge thermal protection systems (TPS). Development of improved inspection techniques on the foam TPS is necessary to prevent similar occurrences in the future. Foamed panels with drilled holes for volumetric flaws and Teflon inserts to simulate debonded conditions have been used to evaluate and calibrate nondestructive testing (NDT) methods. Unfortunately the symmetric edges and dissimilar materials used in the preparation of these simulated flaws provide an artificially large signal while very little signal is generated from the actual defects themselves. In other words, the same signal are not generated from the artificial defects in the foam test panels as produced when inspecting natural defect in the ET foam TPS. A project to create more realistic voids similar to what actually occurs during manufacturing operations was began in order to improve detection of critical voids during inspections. This presentation describes approaches taken to create more natural voids in foam TPS in order to provide a more realistic evaluation of what the NDT methods can detect. These flaw creation techniques were developed with both sprayed foam and poured foam used for insulation on the External Tank. Test panels with simulated defects have been used to evaluate NDT methods for the inspection of the External Tank. A comparison of images between natural flaws and machined flaws generated from backscatter x-ray radiography, x-ray laminography, terahertz imaging and millimeter wave imaging show significant differences in identifying defect regions.

Workman, Gary L.↗
NASA NTRS2007

Mini-Survey of SDSS OIII AGN with Swift

There is a common wisdom that every massive galaxy has a massive block hole. However, most of these objects either are not radiating or until recently have been very difficult to detect. The Sloan Digital Sky Survey (SDSS) data, based on the [OIII] line indicate that perhaps up to 20% of all galaxies may be classified as AGN a surprising result that must be checked with independent data. X-ray surveys have revealed that hard X-ray selected AGN show a strong luminosity dependent evolution and their luminosity function (LF) shows a dramatic break towards low Lx (at all z). This is seen for all types of AGN, but is stronger for the broad-line objects. In sharp contrast, the local LF of (optically-selected samples) shows no such break and no differences between narrow and broad-line objects. Assuming both hard X-ray and [OIII] emission are fair indicators of AGN activity, it is important to understand this discrepancy. We present here the results of a mini-survey done with Swift on a selected sample of SDSS selected AGN. The objects have been sampled at different L([OIII]) to check the relation with the Lx observed with Swift.

Angelina, Lorella↗
NASA NTRSDate not supplied

The Dominion Range (DOM) Lunar Regolith Breccia Pairing Group

With the Chang-E missions, ANGSA sample analysis, and Artemis mission progress as three examples of excitement about lunar science, we want to reaffirm and emphasize the importance of lunar meteorites to our understanding of the Moon. There are over 600 lunar meteorites documented with a total combined mass over 1000 kg, roughly 3x more mass than the Apollo samples. The 2018-19 season ANSMET team recovered lunar meteorites, reported in three different newsletters. Because these have been announced across three years, 2019-2022, we here provide an overview of their characteristics, reported findings, and comparison to other lunar meteorites. In particular, we emphasize their unique properties and how they may contribute to advancing lunar science. Eight pieces were recovered in the 2018-19 ANSMET season. All were found near the northern edge of the blue ice tongue or at the edge in the moraine. The largest mass is 45.87 g, ranging down to lowest mass of 5.46 g.

meteorite↗
NASA NTRS2001

Rheology of Diabase: Implications for Tectonics on Venus and Mars

Two important goals of our experimental investigation of the rheological behavior of diabase rocks were: (1) to determine flow laws describing their creep behavior over wide ranges of temperature, stress and strain rate and (2) to develop an understanding of the physical mechanisms by which these rocks flow under laboratory conditions. With this basis, a primary objective then was to construct constitutive equations that can be used to extrapolate from laboratory to planetary conditions. We specifically studied the rheological properties of both natural rock samples and synthetic aggregates. The former provided constraints for geologic systems, while the latter defined the relative contributions of the constituent mineral phases and avoided the influence of glass/melt found in natural samples. In addition, partially molten samples of crustal rock composition were deformed in shear to large strains (greater than 200%) important in crustal environments. The results of this research yielded essential rheological properties essential for models of crustal deformation on terrestrial planets, specifically Venus and Mars, as well as on the geodynamical evolution of these planets. Over the past three years, we also completed our investigation of the creep behavior of water ice with applications to the glaciers, ice sheets and icy satellites. Constitutive equations were determined that describe flow over a wide ranged of stress, strain rate, grain size and temperature. In the case of ice, three creep regimes were delineate. Extrapolation demonstrates that dislocation glide and grain boundary sliding processes dominate flow in ice I under planetary conditions and that diffusion creep is not an important deformation mechanism either in the laboratory or on icy satellites. These results have already been incorporated by other investigators into models describing, for example, the thickness and stability of the ice shell on Europa and to unravel long-standing discrepancies between field observations on glaciers and laboratory results.

Kohlstedt, David L.↗
NASA NTRS1987

Concepts for collection of aerosols in Titan's atmosphere

This paper considers design of instruments for collection of aerosols during entry in Titan's atmosphere. Major constraints on designs are small sample collection time, low aerosol column density, and the need to collect 1-10 micrograms of aerosol for gas chromatographic analysis. Thus, it is important to maximize aerosol collection through collector design, which includes consideration of various types of collectors, and maximizing the collection efficiency of a given type of collector. Sampling systems discussed include inertial impactors, filters, electrostatic devices, and multistage instruments. Aerosol sampling is reviewed in the context of high-altitude (200-70 km) and low-altitude (60-30 km) regions of Titan's atmosphere.

Oberbeck, Verne R.↗
NASA NTRS2012

Analysis of Direct Samples of Early Solar System Aqueous Fluids

Over the past three decades we have become increasingly aware of the fundamental importance of water, and aqueous alteration, on primitive solar-system bodies. Some carbonaceous and ordinary chondrites have been altered by interactions with liquid water within the first 10 million years after formation of their parent asteroids. Millimeter to centimeter-sized aggregates of purple halite containing aqueous fluid inclusions were found in the matrix of two freshly-fallen brecciated H chondrite falls, Monahans (1998, hereafter simply "Monahans") (H5) and Zag (H3-6) (Zolensky et al., 1999; Whitby et al., 2000; Bogard et al., 2001) In order to understand origin and evolution of the aqueous fluids inside these inclusions we much measure the actual fluid composition, and also learn the O and H isotopic composition of the water. It has taken a decade for laboratory analytical techniques to catch up to these particular nanomole-sized aqueous samples. We have recently been successful in (1) measuring the isotopic composition of H and O in the water in a few fluid inclusions from the Zag and Monahans halite, (2) mineralogical characterization of the solid mineral phases associated with the aqueous fluids within the halite, and (3) the first minor element analyses of the fluid itself. A Cameca ims-1270 equipped with a cryo-sample-stage of Hokkaido University was specially prepared for the O and H isotopic measurements. The cryo-sample-stage (Techno. I. S. Corp.) was cooled down to c.a. -190 C using liquid nitrogen at which the aqueous fluid in inclusions was frozen. We excavated the salt crystal surfaces to expose the frozen fluids using a 15 keV Cs+ beam and measured negative secondary ions. The secondary ions from deep craters of approximately 10 m in depth emitted stably but the intensities changed gradually during measurement cycles because of shifting states of charge compensation, resulting in rather poor reproducibility of multiple measurements of standard fluid inclusions of +/- 90 0/00(2 sigma) for delta D, and +/- 29 0/00 (2 sigma) for delta O-18. On the other hand, the reproducibility of Delta O-17 is plus or minus 8 /00 (2 sigma ) because the observed variations of isotope ratios follow a mass dependent fractionation law. Variations of delta D of the aqueous fluids range over sog,a 330(90; 2 sigma ) to +1200(90) 0/00 for Monahans and delta 300(96) 0/00 to +90(98)0/00 for Zag. Delta O-17 of aqueous fluids range over delta 16(22) 0/00 to +18(10) 0/00 for Monahans and +3(10) 0/00 to +27(11) 0/00 for Zag. These variations are larger than the reproducibility of standard analyses and suggest that isotope equilibria were under way in the fluids before trapping into halite. The mean values of delta D and Delta O-17 are +290 0/00 and +9 0/00, respectively. The mean values and the variations of these fluids are different from the representative values of ordinary chondrites, verifying our working hypothesis that the fluid inclusion-bearing halites were not indigenous to the H chondrite parent-asteroid but rather represent exogenous material delivered onto the asteroid from a separate cryovolcanically-active body. This initial isotopic work has demonstrated the feasibility of the measurements, but also revealed sample processing and analytical shortcomings that are now being addressed. Examination of solid mineral inclusions within Monahans and Zag halite grains by confocal Raman spectroscopy at the Carnegie Geophysical Laboratory has revealed them to be metal, magnetite, forsteritic olivine (Fo.98), macromolecular carbon (MMC), pyroxenes, feldspar with Raman spectral affinity to anorthoclase and, probably, fine-grained lepidocrocite (FeO(OH)). In addition, one inclusion features aliphatic material with Raman spectral features consistent with a mixture of short-chain aliphatic compounds. We have initiated analyses of the bulk composition of the fluids within the inclusions in Zag and Monahans halites at Virginia Tech by LA ICPMS using angilent 7500ce quadrupole ICPMS and a Lambda Physik GeoLas 193 nm excimer laser ablation system. Preliminary results reveal that the inclusion aqueous fluids contain highly charged cations of Ca, Mg and Fe. The minerals and compounds discovered thus far within Monahans/Zag halites are indicative of an originating body at least partly composed of unequilibrated anhydrous materials (high Fo olivine, pyroxenes, feldspars, possibly the metal) which were subjected to aqueous alteration (the halite parent brine) and containing a light organic component (the short-chain aliphatic compounds). This material was ejected from the originating body with little or no disruption, as evidenced with the presence of fluid inclusions. An actively geysering body similar to modern Enceladus (Postberg et al., 2011) may be a reasonable analogue in this respect. Also, the originating body should have been within close proximity to the H chondrite parent in order to generate the number of halite grains seen in Monahans and Zag. Other candidates for Monahans/Zag halite parent bodie(s) may include a young Ceres with its possible liquid ocean, or Main Belt comets.

Zolensky, Michael E.↗
NASA NTRS2002

Maximizing Macromolecule Crystal Size for Neutron Diffraction Experiments

A challenge in neutron diffraction experiments is growing large (greater than 1 cu mm) macromolecule crystals. In taking up this challenge we have used statistical experiment design techniques to quickly identify crystallization conditions under which the largest crystals grow. These techniques provide the maximum information for minimal experimental effort, allowing optimal screening of crystallization variables in a simple experimental matrix, using the minimum amount of sample. Analysis of the results quickly tells the investigator what conditions are the most important for the crystallization. These can then be used to maximize the crystallization results in terms of reducing crystal numbers and providing large crystals of suitable habit. We have used these techniques to grow large crystals of Glucose isomerase. Glucose isomerase is an industrial enzyme used extensively in the food industry for the conversion of glucose to fructose. The aim of this study is the elucidation of the enzymatic mechanism at the molecular level. The accurate determination of hydrogen positions, which is critical for this, is a requirement that neutron diffraction is uniquely suited for. Preliminary neutron diffraction experiments with these crystals conducted at the Institute Laue-Langevin (Grenoble, France) reveal diffraction to beyond 2.5 angstrom. Macromolecular crystal growth is a process involving many parameters, and statistical experimental design is naturally suited to this field. These techniques are sample independent and provide an experimental strategy to maximize crystal volume and habit for neutron diffraction studies.

Judge, R. A.↗