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At least 451 records · Page 25

Microfocus/Polycapillary-Optic Crystallographic X-Ray System

A system that generates an intense, nearly collimated, nearly monochromatic, small-diameter x-ray beam has been developed for use in macromolecular crystallography. A conventional x-ray system for macromolecular crystallography includes a rotating-anode x-ray source, which is massive (.500 kg), large (approximately 2 by 2 by 1 m), and power-hungry (between 2 and 18 kW). In contrast, the present system generates a beam of the required brightness from a microfocus source, which is small and light enough to be mounted on a laboratory bench, and operates at a power level of only tens of watts. The figure schematically depicts the system as configured for observing x-ray diffraction from a macromolecular crystal. In addition to the microfocus x-ray source, the system includes a polycapillary optic . a monolithic block (typically a bundle of fused glass tubes) that contains thousands of straight or gently curved capillary channels, along which x-rays propagate with multiple reflections. This particular polycapillary optic is configured to act as a collimator; the x-ray beam that emerges from its output face consists of quasi-parallel subbeams with a small angular divergence and a diameter comparable to the size of a crystal to be studied. The gap between the microfocus x-ray source and the input face of the polycapillary optic is chosen consistently with the focal length of the polycapillary optic and the need to maximize the solid angle subtended by the optic in order to maximize the collimated x-ray flux. The spectrum from the source contains a significant component of Cu K (photon energy is 8.08 keV) radiation. The beam is monochromatized (for Cu K ) by a nickel filter 10 m thick. In a test, this system was operated at a power of 40 W (current of 897 A at an accelerating potential of 45 kV), with an anode x-ray spot size of 41+/-2 microns. Also tested, in order to provide a standard for comparison, was a commercial rotating-anode x-ray crystallographic system with a pyrolytic graphite monochromator and a 250-micron pinhole collimator, operating at a power of 3.15 kW (current of 70 mA at an accelerating potential of 45 kV). The flux of collimated Cu K radiation in this system was found to be approximately 16 times that in the rotatinganode system. Data on x-ray diffraction from crystals of tetragonal form of lysozyme (protein) in this system were found to be of high quality and to be reducible by use of standard crystallographic software.

Joy, Marshall↗

Ultra-Thin Coatings Beautify Art

The craftsmen in the Roman Empire who constructed the Lycurgus Cup 17 centuries ago probably didn't think their artifact would survive for nearly 2,000 years as a prized possession. And they certainly couldn't have known that the technology they used to make it would eventually become an important part of space exploration. Carved from one solid mass, the cup is one of the few complete glass objects from that period, and the only one made from dichroic glass. Meaning "two-colored" in Greek, dichroic glass was originally created by adding trace amounts of gold and silver to a large volume of glass melt. The resulting medium partially reflects the light passing through it, causing an observer to see different colors depending on the direction of the light source. The Lycurgus Cup, for example, is famous for appearing green in daylight and red when lit at night, symbolic of the ripening grapes used to fill it with wine. NASA revitalized the production of dichroic glass in the 1950s and 1960s as a means of protecting its astronauts. Ordinary clear substances cannot protect human vision from the harsh rays of unfiltered sunlight, and everything from the human body to spacecraft sensors and computers are at risk if left unprotected from the radiation that permeates space. The microscopic amounts of metal present in dichroic glass make it an effective barrier against such harmful radiation. While the ancient manufacturing technique called for adding metals to glass melt, NASA developed a process in which metals are vaporized by electron beams in a vacuum chamber and then applied directly to surfaces in an ultra-thin film. The vapor condenses in the form of crystal structures, and the process is repeated for up to several dozen coatings. The resulting material, still only about 30 millionths of an inch thick, is sufficient to reflect radiation even while the glass, or polycarbonate, as in the case of space suit helmets, remains transparent to the human eye.

Source record↗

Controlling Vapor Pressure In Hanging-Drop Crystallization

Rate of evaporation adjusted to produce larger crystals. Device helps to control vapor pressure of water and other solvents in vicinity of hanging drop of solution containing dissolved enzyme protein. Well of porous frit (sintered glass) holds solution in proximity to drop of solution containing protein or enzyme. Vapor from solution in frit controls evaporation of solvent from drop to control precipitation of protein or enzyme. With device, rate of nucleation limited to decrease number and increase size (and perhaps quality) of crystals - large crystals of higher quality needed for x-ray diffraction studies of macromolecules.

Carter, Daniel C.↗

Determining the Oxygen Fugacity of Lunar Pyroclastic Glasses Using Vanadium Valence - An Update

We have been developing an oxygen barometer based on the valence state of V (V(2+), V(3+), V(4+), and V(5+)) in solar system basaltic glasses. The V valence is determined by synchrotron micro x-ray absorption near edge structure (XANES), which uses x-ray absorption associated with core-electronic transitions (absorption edges) to reveal a pre-edge peak whose intensity is directly proportional to the valence state of an element. XANES has advantages over other techniques that determine elemental valence because measurements can be made non-destructively in air and in situ on conventional thin sections at a micrometer spatial resolution with elemental sensitivities of approx. 100 ppm. Recent results show that fO2 values derived from the V valence technique are consistent with fO2 estimates determined by other techniques for materials that crystallized above the IW buffer. The fO2's determined by V valence (IW-3.8 to IW-2) for the lunar pyroclastic glasses, however, are on the order of 1 to 2.8 log units below previous estimates. Furthermore, the calculated fO2's decrease with increasing TiO2 contents from the A17 VLT to the A17 Orange glasses. In order to investigate these results further, we have synthesized lunar green and orange glasses and examined them by XANES.

Karner, J. M.↗

Acoustic field positioning for containerless processing

The non-contact positioning of materials in a space processing chamber is accomplished using a new type of acoustic levitator. Liquid and solid materials are positioned using a single source of sound. Fine control of position may be obtained by motion of an acoustical reflector. Electrical power required is usually less than 100 watts. The system operates satisfactorily at high and low temperatures and is adaptable as an add-on feature to existing space experiments. Containerless melting and solidification can be performed and a freely suspended liquid can be shaped to the contour of the sound field. Experiments are described in which aluminum, glass and plastic materials are melted and solidified in the containerless state. The system has applications to containerless crystal growth, melting and related processes.

Whymark, R. R.↗

Acoustic field positioning for containerless processing

The noncontact positioning of materials in a space processing chamber is accomplished using a new type of acoustic levitator. Liquid and solid materials are positioned using a single source of sound. Fine control of position may be obtained by motion of an acoustical reflector. The electrical power required is usually less than 100 watts. The system operates satisfactorily at high and low temperatures and is adaptable as an 'add-on' feature to existing space experiments. Containerless melting and solidification can be performed and a freely suspended liquid can be shaped to the contour of the sound field. Experiments are described in which aluminum, glass and plastic materials are melted and solidified in the containerless state. The system has applications to containerless crystal growth, melting and related processes.

Whymark, R. R.↗

Very low-Ti mare basalts

Bulk compositions, petrology, and mineralogy of lithic fragments discovered in polished sections of Apollo 17 drill core samples 70007, 70008, and 70009 and Luna 24 soil 24077, 43 are described. The fragments have unambiguous affinities to mare basalts, but are exceptionally low in TiO2 (less than 1.0 wt.% TiO2). Apollo 17 rake sample 78526 is a green glassy rock of similar composition. Together the samples represent a distinct variety of mare basalts. Bulk compositional relationships suggest that they are related to Apollo 15 green glass, but the data do not permit one to discern the precise nature of the relationship. Both fractional crystallization and partial melting models can explain the observed compositional trends.

Taylor, G. J.↗

Apollo Sample 64455: Petrologic and Geochemical Characterization of a Glass-Coated Impact Melt Rock

Introduction and Background: Impact melts are a key product of the impact cratering process. Impact melts can turbulently entrain pre-existing rock fragments, and melt part of those entrained materials until thermal equilibrium is achieved [1–3]. Lunar impact melt rocks are valuable for determining the precise ages of basin-forming and cratering events, which anchor the cratering chronology and dynamics of the entire solar system [4, and references therein]. Additionally, entrained clasts can inform on the petrology and age of crustal materials that predate the melt-forming impact. In lithologies where no pristine samples are available, entrained materials may hold the record of endogenous lunar volatiles, provided we can untangle their impact histories as high temperature impact melt can heat the clasts and may alter their native volatiles or isotopic signatures [5–6]. Here, we characterize an Apollo 16 sample, 64455,70B, in an effort to understand the physical, microstructural, and geochemical consequences of impact melt contact metamorphism. We acquired optical light and x-ray maps of the sample, as well as quantitative analyses via electron probe microanalysis (EPMA). These tasks allow us to better understand the interaction between impact melts and entrained clasts, ultimately closing knowledge gaps in high-temperature impact processing on planetary surfaces. Sample Description: Sample 64455 is an oblong crystalline rock encased in glass to form an egg-like shape [7–8]. The impact melt coating has altered the outer (1 to 2 mm) rind of the crystalline rock and has preserved schlieren. The interior crystalline rock is likely a crystalline impact melt rock based on its bulk Ir content of 2.25 parts per billion [9]. The composition of the impact melt glass rind cannot be solely derived from the crystalline interior, the glassy rind is more aluminous and less magnesian [10]. Neither the crystalline interior nor the glassy rind were radiometrically age dated, although several studies investigated its cosmogenic isotopes and exposure ages, which reveal the sample was exposed on the lunar surface for ~1–2 Ma [11–13]. Preliminary Results: The interior crystalline rock consists primarily of plagioclase with interstitial pyroxene and olivine. Plagioclase grains are zoned and compositions range from An97–89, while pyroxene compositions generally range from En68Fs19Wo13 to En82Fs15Wo3 and olivine are Fo77 to Fo85. Minor phases include Fe-Ni metal, Ca-phosphates, a K- and Si-rich phase, sulfides, and Fe-phosphides. The glass rind contains approximately 44 wt.% SiO2, 25 wt.% Al2O3, 6 wt.% FeO, 8 wt.% MgO, and 14 wt.% CaO, with other oxides at <1 wt.% each, although the composition of the glass becomes more variable closest to the crystalline rock. The rind consists of rounded plagioclase, pyroxene, and olivine crystals with interstitial melt. In some locations, the rounded crystals are surrounded by closely-packed, blade-like crystals, <5 µm in width. These results indicate that the crystalline interior has partially melted where in contact with the high-temperature impact melt and while further investigation is needed, pyroxene may have preferentially melted relative to olivine and plagioclase. Future Work: We plan to conduct electron backscatter diffraction (EBSD) mapping in order to determine crystallinity and crystal orientation. Next using transmission electron microscopy (TEM) data in conjunction with EBSD and EPMA information, we will model the diffusion of moderately volatile elements between the melt and remnant crystals.

A C Stadermann↗

Electrostatic Stabilization Of Growing Protein Crystals

Proposed technique produces large crystals in compact, economical apparatus. Report presents concept for supporting protein crystals during growth in microgravity. Yields crystals larger and more-nearly perfect than those grown on Earth. Combines best features of sandwich-drop and electrostatic-levitation methods of support. Drop of protein solution inserted between pair of glass or plastic plates, as in sandwich-drop-support method. Electrostatically charged ring confines drop laterally and shapes it, as in electrostatic technique. Apparatus also made to accommodate several drops simultaneously between same pair of supporting plates. Drops can be inserted and crystals removed through ducts in plates.

Shlichta, Paul J.↗

Experimental petrology and origin of Fra Mauro rocks and soil.

Results of melting experiments over the pressure range from 0 to 20 kb on Apollo 14 igneous rocks 14310 and 14072, and on comprehensive fines 14259. It is found that low-pressure crystallization of rocks 14310 and 14072 proceeds as predicted from the textural relationships displayed by thin sections of these rocks. The mineralogy and textures of these rocks are the result of near-surface crystallization. The chemical compositions of these lunar samples all show special relationships to multiply saturated liquids in the system anorthite-forsterite-fayalite-silica at low pressure. Partial melting of a lunar crust consisting largely of plagioclase, low-calcium pyroxene, and olivine, followed by crystal fractionation at the lunar surface, is a satisfactory mechanism for the production of the igneous rocks and soil glasses sampled by Apollo 14. The KREEP component of other lunar soils, may have a similar origin.

Walker, D.↗

New works in space

Goods and services that may be furnished by the Space Shuttle are described. A single multibeam antenna array capable of supplying satellite communication for 256 U.S. cities, a disaster warning network, and a TV link to remote areas is discussed. Attention is also given to such materials processing programs as crystal growth (for example, production of mercuric iodide crystals for gamma-ray detectors), eutectic growth of solid-solution crystals such as mercury-cadmium-telluride, manufacture of uniform latex spheres for medical applications, and development of small glass spheres for fusion power applications. In addition to the Space Telescope, a meter-class telescope on the Shuttle and a wide-field survey instrument are under study.

Kingsbury, J. E.↗

Spectra of Fe-Ti silicate glasses - Implications to remote-sensing of planetary surfaces

Optical spectra of synthetic Fe-Ti silicate glasses and the temperature variations of the spectral features were investigated. The spectra are assigned to absorptions due to crystal field (CF) transitions in Ti(3+), Fe(2+) in octahedral coordination, and Fe(2+) in tetrahedral coordination, and to metal-metal and oxygen-metal charge transfer (CT) transitions which contribute to the near ultraviolet absorption edge. Temperature variations of the optical bands have been studied to explore implications for remote sensing. Caution is urged in the use of the absorption edge as a measure of TiO2 concentrations on planetary surfaces and in regolith samples.

Nolet, D. A.↗

Processing Glass Fiber from Moon/Mars Resources

Processing of Lunar/Mars raw materials into usable structural and thermal components for use on a Lunar/Mars base will be essential for human habitation. One such component will be glass fiber which can be used in a number of applications. Glass fiber has been produced from two lunar soil simulants. These two materials simulate lunar mare and lunar highlands soil compositions. Short fibers containing recrystallized areas were produced from the as-received simulants. Doping the highland simulant with 8 weight percent boria yielded a material which could be spun continuously. The effects of lunar gravity on glass fiber formation were studied utilizing NASA's KC 135 aircraft. Gravity was found to play a role in crystallization and final fiber diameter.

Tucker, Dennis S.↗

Samples for estimating primary volatiles in Martian magmas and ancient atmospheric pressures on Mars

Inclusions of glass are likely to be present in phenocrysts in volcanic rocks from Mars, because these occur in volcanic rocks from both Earth and Moon. The usefulness of the inclusions depends upon their size and composition. The compositions of tiny inclusions may be modified by diffusion during growth of the enclosing crystal, the modifications increasing with melt viscosity (silica). Slow cooling results in crystallization and possible redistribution of volatiles, the effects increasing with decreasing silica. Primary volatile concentrations are best sought in inclusions larger than about 50 micrometer diameter in olivine or chromite crystals from quickly cooled basaltic scoria. Such crystals may be present in sands, but it would be preferable to extract them from individual rocks which could be dated and compositionally characterized. This would allow eventual understanding of the role of time and place in outgassing and volcanism on Mars. Analyses of volatiles in inclusions of more siliceous glass in non-basaltic rocks will reveal whether deep outgassing occurs and whether surface volatiles are recycled. Most volcanic crystals contain inclusions, but large inclusions can be uncommon. In the case of terrestrial basalts sample masses of several hundred grams are generally sufficient.

Anderson, A. T., Jr.↗

Crystal Stratigraphy of Two Basalts from Apollo 16: Unique Crystallization of Picritic Basalt 606063,10-16 and Very-Low-Titanium Basalt 65703,9-13

A geochemical survey of Apollo 16 regolith fragments found five basaltic samples from among hundreds of 2-4 mm regolith fragments of the Apollo 16 site. These included a high-Ti vitrophyric basalt (60603,10-16) and one very-low-titanium (VLT) crystalline basalt (65703,9-13). Apollo 16 was the only highlands sample return mission distant from the maria (approx. 200 km). Identification of basaltic samples at the site not from the ancient regolith breccia indicates input of material via lateral transport by post-basin impacts. The presence of basaltic rocklets and glass at the site is not unprecedented and is required to satisfy mass-balance constraints of regolith compositions. However, preliminary characterization of olivine and plagioclase crystal size distributions indicated the sample textures were distinct from other known mare basalts, and instead had affinities to impact melt textures. Impact melt textures can appear qualitatively similar to pristine basalts, and quantitative analysis is required to distinguish between the two in thin section. The crystal stratigraphy method is a powerful tool in studying of igneous systems, utilizing geochemical analyses across minerals and textural analyses of phases. In particular, trace element signatures can aid in determining the ultimate origin of these samples and variations document subtle changes occurring during their petrogenesis.

Donohue, P. H.↗

Photophysical behavior of doubly bridged d7-d7 metal-metal bonded compounds - The crystal structure and the excited- and ground-state electronic spectra of Re2(CO)6(dmpm)2 (dmpm = bis/dimethylphosphino/ methane)

Re2(CO)6(dmpm)2 shows photophysical behavior in a rigid medium that differs dramatically from that observed in fluid solution. In a hydrocarbon glass at 77 K, metal-metal bond homolysis is suppressed and an intense phosphorescence is observed. The transient absorption spectrum, which shows only weak transitions to the red of the ground state 1(sigma-sigma asterisk) transition, permits assignment of the emitting state to a 3(sigma-sigma asterisk) transition. The crystal structure of Re2(CO)6(dmpm)2 is also reported. The ground-state electronic structure is discussed relative to the structural data.

Milder, Steven J.↗

Experimental petrology and origin of Fra Mauro rocks and soil

Melting experiments over the pressure range 0 to 20 kilobars were conducted on Apollo 14 igneous rocks 14310 and 14072 and on comprehensive fines 14259. The mineralogy and textures of rocks 14310 and 14072 are presumed to be the result of near-surface crystallization. The chemical compositions of the samples show special relationships to multiply-saturated liquids in the system: anorthite-forsterite-fayalite-silica at low pressure. Partial melting of a lunar crust consisting largely of plagioclase, low calcium pyroxene, and olivine, followed by crystal fractionation at the lunar surface is proposed as a mechanism for the production of the igneous rocks and soil glasses sampled by Apollo 14.

Walker, D.↗

Sol-Gel Glasses

Multicomponent homogeneous, ultrapure noncrystalline gels/gel derived glasses are promising batch materials for the containerless glass melting experiments in microgravity. Hence, ultrapure, homogeneous gel precursors could be used to: (1) investigate the effect of the container induced nucleation on the glass forming ability of marginally glass forming compositions; and (2) investigate the influence of gravity on the phase separation and coarsening behavior of gel derived glasses in the liquid-liquid immiscibility zone of the nonsilicate systems having a high density phase. The structure and crystallization behavior of gels in the SiO2-GeO2 as a function of gel chemistry and thermal treatment were investigated. As are the chemical principles involved in the distribution of a second network former in silica gel matrix being investigated. The procedures for synthesizing noncrystalline gels/gel-monoliths in the SiO2-GeO2, GeO2-PbO systems were developed. Preliminary investigations on the levitation and thermal treatment of germania silicate gel-monoliths in the Pressure Facility Acoustic Levitator were done.

Mukherjee, S. P.↗