Skylab experiments. Volume 3: Materials science. [Skylab experiments on metallurgy, crystal growth, semiconductors, and combustion physics in weightless environment for high school level education

NASA Technical Reports Server (NTRS)

1973-01-01

The materials science and technology investigation conducted on the Skylab vehicle are discussed. The thirteen experiments that support these investigations have been planned to evaluate the effect of a weightless environment on melting and resolidification of a variety of metals and semiconductor crystals, and on combustion of solid flammable materials. A glossary of terms which define the space activities and a bibliography of related data are presented.

SABRE: Dark matter annual modulation detection in the northern and southern hemispheres

NASA Astrophysics Data System (ADS)

Tomei, C.

2017-02-01

SABRE (Sodium-iodide with Active Background REjection) is a new NaI(Tl) experiment designed to search for galactic Dark Matter through the annual modulation signature. SABRE will consist of highly pure NaI(Tl) crystals operated in an active liquid scintillator veto. The SABRE experiment will follow a two-phase approach. In the first phase, one high-purity NaI(Tl) crystal will be operated at LNGS in an active liquid scintillator veto with the goal of demonstrating backgrounds low enough for a sensitive test of the DAMA/LIBRA result. An unprecedented radio-purity for both the NaI powder and the crystal growth will be needed to achieve this goal. The second phase will consist in building two high-purity NaI(Tl) detector arrays, with a total mass of about 50 kg each, located at LNGS and in the Stawell Gold Mine in Australia. The operation of twin full-scale experiments in both the northern and the southern hemispheres will strengthen the reliability of the result against any possible seasonal systematic effect.

Waveguiding and bending modes in a plasma photonic crystal bandgap device

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wang, B., E-mail: bwang17@stanford.edu; Cappelli, M. A.

2016-06-15

Waveguiding and bending modes are investigated in a fully tunable plasma photonic crystal. The plasma device actively controls the propagation of free space electromagnetic waves in the S to X band of the microwave spectrum. An array of discharge plasma tubes form a square crystal lattice exhibiting a well-defined bandgap, with individual active switching of the plasma elements to allow for waveguiding and bending modes to be generated dynamically. We show, through simulations and experiments, the existence of transverse electric (TE) mode waveguiding and bending modes.

Ultrastructural studies of synthetic apatite crystals.

PubMed

Arends, J; Jongebloed, W L

1979-03-01

In this paper a survey is given of some ultrastructural properties of synthetic hydroxyapatite. The preparation method by which single crystals with a length in the range of 0.1-3.0mm and a defined purity and stoïchiometry can be produced is given. Two groups of materials are considered in detail: carbonate-rich (greater than 0.1% CO3) and low-carbonate hydroxyapatites. The experiments on carbonate-rich material, being the most interesting from a biological point of view, show that acids attack at an active site in the hexagonal basal-plane of the crystals. Later on the crystals dissolve in the center of the crystal parallel to the c-axis forming tube-like structures. The active site can be protected from dissolution if the crystals are pretreated by EHDP or MFP. A comparison with lattice defect theory shows that most likely dislocations of the "hollow-core" type are responsible for the preferential dissolution.

Perspectives in active liquid crystals

PubMed Central

Majumdar, Apala; Cristina, Marchetti M.; Virga, Epifanio G.

2014-01-01

Active soft matter is a young, growing field, with potential applications to a wide variety of systems. This Theme Issue explores this emerging new field by highlighting active liquid crystals. The collected contributions bridge theory to experiment, mathematical theories of passive and active nematics, spontaneous flows to defect dynamics, microscopic to continuum levels of description, spontaneous activity to biological activation. While the perspectives offered here only span a small part of this rapidly evolving field, we trust that they might provide the interested reader with a taste for this new class of non-equilibrium systems and their rich behaviour. PMID:25332386

Modeling of PCG fluid dynamics: Salient results

NASA Technical Reports Server (NTRS)

Ramachandran, N.

1993-01-01

Materials processing in space-based laboratories has already yielded higher quality crystals during previous space flights, and opportunities for several fluids experiments are anticipated during the extended duration missions planned for the future. Crystal growth in space benefits not only from its reduced gravity environment but also from the absence of the hydrostatic pressure which assists certain crystal growth and refinement methods. Gravity-driven phenomena are thus reduced in strength, and a purely diffusive fluid's behavior can be attained. In addition, past materials science experiments have shown that microgravity can also help produce larger crystals. While gravity-related effects are definitely curtailed in space, they are nevertheless present to some degree due to the acceleration environment onboard the spacecraft. This residual acceleration level is comprised of quasi-steady, oscillatory, and transient components, and is caused by a variety of mechanisms. For example, gravity gradient forces produce low frequency disturbances, and the operation of machinery, control thrusters, solar panels, human activity, etc. contribute to higher frequency accelerations. These disturbances are collectively referred to as g-jitter, and they can be deleterious to certain experiments where the minimization of the acceleration level is important. Advanced vibration isolation techniques can be utilized to actively filter out some of the detrimental frequencies and help in obtaining optimum results. However, the successful application of this technology requires the detailed analysis of candidate fluids experiments to gauge their response to g-jitter and to determine their acceleration sensitivities. Several crystal growth experiments in the Protein Crystal Growth (PCG) area, besides others, are expected to be carried out on future shuttle flights and on Space Station Freedom. The need for vibration isolation systems or components for microgravity science experiments can be expected to grow as experiments and available hardware becomes more complex. This technology will also find increased application as the science community develops an awareness of their specific needs relative to the environment available in manned space missions. Vibration isolation research strives to develop a microgravity environment requirement that defines tolerance limits on the allowable g-level, and provides the required technology to achieve it. This effort will assist in establishing the tolerable acceleration levels for specific fluids experiments. The primary effort is directed towards modeling PCG and the approach undertaken for this investigation is outlined. The objectives of this research are: (1) to computationally determine vibration sensitivity of protein crystal growth experiments; (2) determine if these experiments can benefit from vibration isolation techniques; and (3) provide realistic requirements for vibration isolation technology.

Visualizing Molecular Chirality in the Organic Chemistry Laboratory Using Cholesteric Liquid Crystals

ERIC Educational Resources Information Center

Popova, Maia; Bretz, Stacey Lowery; Hartley, C. Scott

2016-01-01

Although stereochemistry is an important topic in second-year undergraduate organic chemistry, there are limited options for laboratory activities that allow direct visualization of macroscopic chiral phenomena. A novel, guided-inquiry experiment was developed that allows students to explore chirality in the context of cholesteric liquid crystals.…

Flow Velocity Profiles in Actively-Driven 2D Nozzle Experiments using Freely-Suspended Smectic Liquid Crystal Films

NASA Astrophysics Data System (ADS)

Dutch, Evan; Briggs, Corrina; Ferguson, Kyle; Green, Adam; Park, Cheol; Glaser, Matt; Maclennan, Joe; Clark, Noel

Freely-suspended smectic A liquid crystal films have been used to explore a large range of interesting flow phenomena. Passive microrheology experiments have confirmed previously that such films are ideal systems with which to investigate two-dimensional (2D) hydrodynamics. Here we describe an experiment that uses smectic films to study actively-driven 2D flows. Flow excited by blowing air over a film of smectic liquid crystal material containing small inclusions is captured using digital video microscopy. The flow fields are extracted using particle imaging velocimetry. We have measured the velocity field generated by flow through a thin nozzle into a large rectangular reservoir and compared this to a theoretical model based on 2D complex potential flows. The observations confirm that there is parabolic flow in straight channels, and that the theory accurately models the film velocity flow field in the reservoir. This work was supported by NASA Grant No. NNX-13AQ81G, and NSF MRSEC Grants No. DMR-0820579 and DMR-1420736.

Experimental Deformation of Enstatite Single Crystals at Mantle Pressure and Temperature

NASA Astrophysics Data System (ADS)

Raterron, P. C.; Holyoke, C. W.; Girard, J.

2012-12-01

Orthopyroxenes (OPx) is the second most abundant constituent of the upper mantle, thus may significantly influence mantle plasticity. However, little is known on OPx rheology at high pressure; this is because apparatuses allowing controlled deformation experiments at asthenospheric pressures (P > 3 GPa) are available since only a decade (see Raterron and Merkel, 2009, J. Synch. Rad., 16, 748-756). Mackwell (1991, GRL, 18, 2027-2030) reports a preliminary study of the high-temperature rheology of enstatite single crystals, but these experiments were carried out at room pressure, i.e. in the protoenstatite stability field, and the results cannot directly apply to mantle phases. In order to quantify the effect of pressure on OPx rheology, deformation experiments were carried out in compression on natural enstatite (En90) single crystals in the Deformation-DIA apparatus (D-DIA), at P > 5 GPa and high temperature (T > 1200°C) within the orthoenstatite stability field. The applied stress and specimen strain rates were measured in situ using X-ray diffraction and imaging techniques at the X17B2 beamline of the National Synchrotron Light Source (NSLS, NY, USA). The cylindrical specimens were oriented with their axis - the compression direction - along [101]c crystallographic direction which forms a 45° angle with both [100] and [001] directions. This geometry imposes during compression a maximum shear stress in (001) plane along [001] direction, which results in the activation of [001](001) dislocation slip system known as the weakest slip in OPx. Specimens were deformed together with other crystals or aggregates - two by two, one atop the other in the compression column - in order to compare [101]c crystal plasticity with that of either [011]c enstatite crystals - within which [001](010) slip system is activated - or enstatite aggregates, or again orientated San Carlos olivine crystals of known rheology. Run products microstructures were investigated by electron microscopy. We will present these results which bring new light on the activity of orthoenstatite dislocation slips at mantle P and T conditions.

Final science results: Spacelab J

NASA Technical Reports Server (NTRS)

Leslie, Fred (Editor)

1995-01-01

This report contains a brief summary of the mission science conducted aboard Spacelab J (SL-J), a joint venture between the National Aeronautics and Space Administration (NASA) and the National Space Development Agency (NASDA) of Japan. The scientific objectives of the mission were to conduct a variety of material and life science experiments utilizing the weightlessness and radiation environment of an orbiting Spacelab. All 43 experiments were activated; 24 in microgravity sciences (material processing, crystal growth, fluid physics, and acceleration measurement) and 19 in life sciences (physiology, developmental biology, radiation effects, separation processes, and enzyme crystal growth). In addition, more than a dozen experiments benefited from the extra day through either additional experiment runs or extended growth time.

Crystal-contact engineering to obtain a crystal form of the Kelch domain of human Keap1 suitable for ligand-soaking experiments.

PubMed

Hörer, Stefan; Reinert, Dirk; Ostmann, Katja; Hoevels, Yvette; Nar, Herbert

2013-06-01

Keap1 is a substrate adaptor protein for a Cul3-dependent ubiquitin ligase complex and plays an important role in the cellular response to oxidative stress. It binds Nrf2 with its Kelch domain and thus triggers the ubiquitinylation and degradation of Nrf2. Oxidative stress prevents the degradation of Nrf2 and leads to the activation of cytoprotective genes. Therefore, Keap1 is an attractive drug target in inflammatory diseases. The support of a medicinal chemistry effort by structural research requires a robust crystallization system in which the crystals are preferably suited for performing soaking experiments. This facilitates the generation of protein-ligand complexes in a routine and high-throughput manner. The structure of human Keap1 has been described previously. In this crystal form, however, the binding site for Nrf2 was blocked by a crystal contact. This interaction was analysed and mutations were introduced to disrupt this crystal contact. One double mutation (E540A/E542A) crystallized in a new crystal form in which the binding site for Nrf2 was not blocked and was accessible to small-molecule ligands. The crystal structures of the apo form of the mutated Keap1 Kelch domain (1.98 Å resolution) and of the complex with an Nrf2-derived peptide obtained by soaking (2.20 Å resolution) are reported.

Metal Catalyzed Fusion: Nuclear Active Environment vs. Process

NASA Astrophysics Data System (ADS)

Chubb, Talbot

2009-03-01

To achieve radiationless dd fusion and/or other LENR reactions via chemistry: some focus on environment of interior or altered near-surface volume of bulk metal; some on environment inside metal nanocrystals or on their surface; some on the interface between nanometal crystals and ionic crystals; some on a momentum shock-stimulation reaction process. Experiment says there is also a spontaneous reaction process.

Structures of human thymidylate synthase R163K with dUMP, FdUMP and glutathione show asymmetric ligand binding

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gibson, Lydia M.; Celeste, Lesa R.; Lovelace, Leslie L.

Thymidylate synthase (TS) is a well validated target in cancer chemotherapy. Here, a new crystal form of the R163K variant of human TS (hTS) with five subunits per asymmetric part of the unit cell, all with loop 181-197 in the active conformation, is reported. This form allows binding studies by soaking crystals in artificial mother liquors containing ligands that bind in the active site. Using this approach, crystal structures of hTS complexes with FdUMP and dUMP were obtained, indicating that this form should facilitate high-throughput analysis of hTS complexes with drug candidates. Crystal soaking experiments using oxidized glutathione revealed thatmore » hTS binds this ligand. Interestingly, the two types of binding observed are both asymmetric. In one subunit of the physiological dimer covalent modification of the catalytic nucleophile Cys195 takes place, while in another dimer a noncovalent adduct with reduced glutathione is formed in one of the active sites.« less

Anatase TiO2 single crystals with dominant {0 0 1} facets: Synthesis, shape-control mechanism and photocatalytic activity

NASA Astrophysics Data System (ADS)

Tong, Huifen; Zhou, Yingying; Chang, Gang; Li, Pai; Zhu, Ruizhi; He, Yunbin

2018-06-01

Anatase TiO2 micro-crystals with 51% surface exposing highly active {0 0 1} facets are prepared by hydrothermal synthesis using TiF4 as Ti resource and HF as morphology control agent. In addition, anatase TiO2 single crystals exposing large {0 0 1} crystal facets are facilely synthesized with "green" NaF plus HCl replacing HF for the morphology control. A series of comparative experiments are carried out for separately studying the effects of F- and H+ concentrations on the growth of TiO2 crystals, which have not been understood very much in depth so far. The results indicate that both F- and H+ synergistically affect the synthesis of truncated anatase octahedrons, where F- is preferentially adsorbed on the {0 0 1} facets resulting in lateral growth of these facets and H+ adjusts the growth rate of anatase TiO2 along different orientations by tuning the hydrolysis rate. Based on this information, anatase TiO2 single crystals with small size (1.3 μm) and large exposure of {0 0 1} facets (45%) are successfully prepared under optimal conditions ([H+]/[F-] = 20:1). Photocatalytic activities of the as-prepared products toward methylene blue photo-degradation are further tested. It is revealed that both crystal size and percentage of {0 0 1} facets are decisive for the photocatalytic performance, and the crystals with a small size (1.3 μm) and large exposure of {0 0 1} facets (45%) are catalytically most active. This work has clarified the main factors that control the growth process and morphology of anatase TiO2 single crystals for achieving superior photocatalytic properties.

A Microfluidic, High Throughput Protein Crystal Growth Method for Microgravity

PubMed Central

Carruthers Jr, Carl W.; Gerdts, Cory; Johnson, Michael D.; Webb, Paul

2013-01-01

The attenuation of sedimentation and convection in microgravity can sometimes decrease irregularities formed during macromolecular crystal growth. Current terrestrial protein crystal growth (PCG) capabilities are very different than those used during the Shuttle era and that are currently on the International Space Station (ISS). The focus of this experiment was to demonstrate the use of a commercial off-the-shelf, high throughput, PCG method in microgravity. Using Protein BioSolutions’ microfluidic Plug Maker™/CrystalCard™ system, we tested the ability to grow crystals of the regulator of glucose metabolism and adipogenesis: peroxisome proliferator-activated receptor gamma (apo-hPPAR-γ LBD), as well as several PCG standards. Overall, we sent 25 CrystalCards™ to the ISS, containing ~10,000 individual microgravity PCG experiments in a 3U NanoRacks NanoLab (1U = 103 cm.). After 70 days on the ISS, our samples were returned with 16 of 25 (64%) microgravity cards having crystals, compared to 12 of 25 (48%) of the ground controls. Encouragingly, there were more apo-hPPAR-γ LBD crystals in the microgravity PCG cards than the 1g controls. These positive results hope to introduce the use of the PCG standard of low sample volume and large experimental density to the microgravity environment and provide new opportunities for macromolecular samples that may crystallize poorly in standard laboratories. PMID:24278480

Modifying Cookbook Labs.

ERIC Educational Resources Information Center

Clark, Robert, L.; Clough, Michael P.; Berg, Craig A.

2000-01-01

Modifies an extended lab activity from a cookbook approach for determining the percent mass of water in copper sulfate pentahydrate crystals to one which incorporates students' prior knowledge, engenders active mental struggling with prior knowledge and new experiences, and encourages metacognition. (Contains 12 references.) (ASK)

Hydrolytic weakening in olivine single crystals

NASA Astrophysics Data System (ADS)

Tielke, Jacob A.; Zimmerman, Mark E.; Kohlstedt, David L.

2017-05-01

Deformation experiments on single crystals of San Carlos olivine under hydrous conditions were performed to investigate the microphysical processes responsible for hydrolytic weakening during dislocation creep. Hydrogen was supplied to the crystals using either talc or brucite sealed in nickel capsules with the crystal. Deformation experiments were carried out using a gas medium apparatus at temperatures of 1050° to 1250°C, a confining pressure of 300 MPa, differential stresses of 45 to 294 MPa, and resultant strain rates of 1.5 × 10-6 to 4.4 × 10-4 s-1. For talc-buffered (i.e., water and orthopyroxene-buffered) samples at high temperatures, the dependence of strain rate on stress follows a power law relationship with a stress exponent (n) of ˜2.5 and an activation energy of ˜490 kJ/mol. Brucite-buffered samples deformed faster than talc-buffered samples but contained similar hydrogen concentrations, demonstrating that strain rate is influenced by orthopyroxene activity under hydrous conditions. The values of n and dependence of strain rate on orthopyroxene activity are consistent with hydrolytic weakening occurring in the climb-controlled dislocation creep regime that is associated with deformation controlled by lattice diffusion under hydrous conditions and by pipe diffusion under anhydrous conditions. Analyses of postdeformation electron-backscatter diffraction data demonstrate that dislocations with [100] Burgers vectors are dominant in the climb-controlled regime and dislocations with [001] are dominant in the glide-controlled regime. Comparison of the experimentally determined constitutive equations demonstrates that under hydrous conditions crystals deform 1 to 2 orders of magnitude faster than under anhydrous conditions.

The deformation mechanisms and size effects of single-crystal magnesium

NASA Astrophysics Data System (ADS)

Byer, Cynthia M.

In this work, we seek to understand the deformation mechanisms and size effects of single-crystal magnesium at the micrometer scale through both microcompression experiments and finite element simulations. Microcompression experiments are conducted to investigate the impact of initial dislocation density and orientation on size effects. Micropillars are fabricated using a focused ion beam and tested in a Nanoindenter using a diamond fiat tip as a compression platen. Two different initial dislocation densities are examined for [0001] oriented micropillars. Our results demonstrate that decreasing the initial dislocation density results in an increased size effect in terms of increased strength and stochasticity. Microcompression along the [23¯14] axis results in much lower strengths than for [0001] oriented samples. Post-mortem analysis reveals basal slip in both [0001] and [23¯14] micropillars. The application of a stochastic probability model shows good agreement between theoretical predictions and experimental results for size effects with our values of initial dislocation density and micropillar dimensions. Size effects are then incorporated into a single-crystal plasticity model (modified from Zhang and Joshi [1]) implemented in ABAQUS/STANDARD as a user-material subroutine. The model successfully captures the phenomena typically associated with size effects of increasing stochasticity and strength with decreasing specimen size and also accounts for the changing trends resulting from variations in initial dislocation density that we observe in the experiments. Finally, finite element simulations are performed with the original (traditional, without size effects) crystal plasticity model [1] to investigate the relative activities of the deformation modes of single-crystal magnesium for varying degrees of misalignment in microcompression. The simulations reveal basal activity in all micropillars, even for perfectly aligned compression along the [0001] axis. Pyramidal < c + a > activity dominates until the misalignment increases to 2°, when basal slip takes over as the dominant mode. The stress-strain curves for the case of 0° misalignment agrees well with experimental curves, indicating that good alignment was achieved during the experiments. Through this investigation, we gain a better understanding of how to control the size effects, as well as the deformation mechanisms operating at the small scale in magnesium.

Recent results and new hardware developments for protein crystal growth in microactivity

NASA Technical Reports Server (NTRS)

Delucas, L. J.; Long, M. M.; Moore, K. M.; Smith, C.; Carson, M.; Narayana, S. V. L.; Carter, D.; Clark, A. D., Jr.; Nanni, R. G.; Ding, J.

1993-01-01

Protein crystal growth experiments have been performed on 16 space shuttle missions since April, 1985. The initial experiments utilized vapor diffusion crystallization techniques similar to those used in laboratories for earth-based experiments. More recent experiments have utilized temperature induced crystallization as an alternative method for growing high quality protein crystals in microgravity. Results from both vapor diffusion and temperature induced crystallization experiments indicate that proteins grown in microgravity may be larger, display more uniform morphologies, and yield diffraction data to significantly higher resolutions than the best crystals of these proteins grown on earth.

Hydrodynamic interactions in active colloidal crystal microrheology.

PubMed

Weeber, R; Harting, J

2012-11-01

In dense colloids it is commonly assumed that hydrodynamic interactions do not play a role. However, a found theoretical quantification is often missing. We present computer simulations that are motivated by experiments where a large colloidal particle is dragged through a colloidal crystal. To qualify the influence of long-ranged hydrodynamics, we model the setup by conventional Langevin dynamics simulations and by an improved scheme with limited hydrodynamic interactions. This scheme significantly improves our results and allows to show that hydrodynamics strongly impacts the development of defects, the crystal regeneration, as well as the jamming behavior.

Inverse Slip Accompanying Twinning and Detwinning during Cyclic Loading of Magnesium Single Crystal

DOE PAGES

Yu, Qin; Wang, Jian; Jiang, Yanyao

2013-01-01

In situ , observation of twinning and detwinning in magnesium single crystals during tension-compression cyclic loading was made using optical microscopy. A quantitative analysis of plastic strain indicates that twinning and detwinning experience two stages, low and high work hardening de-twinning, and pure re-twinning and fresh twinning combined with retwinning. Slip is always activated. For the first time, inverse slip accompanying with pure retwinning and high work hardening detwinning was experimentally identified, which provides insights in better understanding of the activity of twining, detwinning, and slips.

What’s in a drop? Correlating observations and outcomes to guide macromolecular crystallization experiments

PubMed Central

Luft, Joseph R.; Wolfley, Jennifer R.; Snell, Edward H.

2011-01-01

Observations of crystallization experiments are classified as specific outcomes and integrated through a phase diagram to visualize solubility and thereby direct subsequent experiments. Specific examples are taken from our high-throughput crystallization laboratory which provided a broad scope of data from 20 million crystallization experiments on 12,500 different biological macromolecules. The methods and rationale are broadly and generally applicable in any crystallization laboratory. Through a combination of incomplete factorial sampling of crystallization cocktails, standard outcome classifications, visualization of outcomes as they relate chemically and application of a simple phase diagram approach we demonstrate how to logically design subsequent crystallization experiments. PMID:21643490

Crystal growth of device quality GaAs in space

NASA Technical Reports Server (NTRS)

Gatos, Harry C.; Lagowski, Jacek

1989-01-01

The program on Crystal Growth of Device Quality GaAs in Space was initiated in 1977. The initial stage covering 1977 to 1984 was devoted strictly to ground-based research. By 1985 the program had evolved into its next logical stage aimed at space growth experiments; however, since the Challenger disaster, the program has been maintained as a ground-based program awaiting activation of experimentation in space. The overall prgram has produced some 80 original scientific publications on GaAs crystal growth, crystal characterization, and new approaches to space processing. Publication completed in the last three years are listed. Their key results are outlined and discussed in the twelve publications included as part of the report.

Density functional theory determination of structural and electronic properties of struvite.

PubMed

Romanowski, Zbigniew; Kempisty, Paweł; Prywer, Jolanta; Krukowski, Stanisław; Torzewska, Agnieszka

2010-07-29

Crystallographic structure, total energy, electronic structure, and the most important elastic properties of struvite, NH(4)MgPO(4).6H(2)O, the main component of infectious urinary stones, are presented. The calculations were performed using ab initio full-electron calculations within the density functional theory-generalized gradient approximation (DFT-GGA) framework. The obtained crystallographic symmetry and the calculated lattice parameters and also the elastic constants are in good agreement with the experimental data. The elastic properties are essential for establishing an optimal response of urinary stones during shock-wave lithotripsy. The calculated electronic charge distribution confirms the layered structure of the struvite crystals. The polar character of the crystal, well-known from crystal growth experiments, was also confirmed by the magnitude of spontaneous polarization which was obtained from direct determination of the electrical dipole density. The calculated value of spontaneous polarization is equal to -8.8 microC cm(-2). This feature may play a key role in struvite crystallization, electrically binding the charged active impurities and other active species, and consequently determining urinary stone formation. We also present the results of our own experiment of the mineralization of struvite induced to growth by Proteus bacteria which are mainly isolated from infectious urinary stones.

Unsteady-state transfer of impurities during crystal growth of sucrose in sugarcane solutions

NASA Astrophysics Data System (ADS)

Martins, P. M.; Ferreira, A.; Polanco, S.; Rocha, F.; Damas, A. M.; Rein, P.

2009-07-01

In this work, we present growth rate data of sucrose crystals in the presence of impurities that can be used by both sugar technologists and crystal growth scientists. Growth rate curves measured in a pilot-scale evaporative crystallizer suggest a period of slow growth that follows the seeding of crystals into supersaturated technical solutions. The observed trend was enhanced by adding typical sugarcane impurities such as starch, fructose or dextran to the industrial syrups. Maximum growth rates of sucrose resulted at intermediate rather than high supersaturation levels in the presence of the additives. The effects of the additives on the sucrose solubility and sucrose mass transfer in solution were taken into account to explain the observed crystal growth kinetics. A novel mechanism was identified of unsteady-state adsorption of impurities at the crystal surface and their gradual replacement by the crystallizing solute towards the equilibrium occupation of the active sites for growth. Specifically designed crystallization experiments at controlled supersaturation confirmed this mechanism by showing increasing crystal growth rates with time until reaching a steady-state value for a given supersaturation level and impurity content.

Thermal, mechanical, optical and conductivity studies of a novel NLO active L-phenylalanine L-phenylalaninium dihydrogenphosphate single crystal

NASA Astrophysics Data System (ADS)

Sujatha, T.; Cyrac Peter, A.; Vimalan, M.; Merline Shyla, J.; Madhavan, J.

2010-08-01

An efficient, novel, semi-organic, nonlinear optical (NLO) material L-phenylalanine L-phenylalaninium dihydrogenphosphate (LPADHP), single crystal of dimension 11×5×2 mm 3, has been grown by the slow evaporation solution growth technique. Single crystal X-ray diffraction studies confirm that the grown crystal belongs to monoclinic system with the space group P2 1. The functional groups present in the crystal were confirmed by the Fourier transform infrared technique. Optical absorption spectrum shows that the material possesses very low absorption in the entire visible region. Thermal analysis confirmed that the crystal is thermally stable up to 161 °C. The frequency dependent dielectric properties of the grown crystal were studied for various temperatures. The second harmonic generation (SHG) efficiency of the grown crystal is 1.2 times greater than that of the potassium dihydrogenphosphate (KDP) single crystal. The laser induced surface damage threshold for the grown crystal was found to be 6.3 GW cm -2 with Nd:YAG laser assembly AC and DC conductivity and photoconductivity experiments are also carried out and the results are discussed.

Enriched TeO 2 bolometers with active particle discrimination: Towards the CUPID experiment

DOE PAGES

Artusa, D. R.; Avignone, F. T.; Beeman, J. W.; ...

2017-04-01

We present the performances of two 92% enriched 130TeO2 crystals operated as thermal bolometers in view of a next generation experiment to search for neutrinoless double beta decay of 130Te. The crystals, 435 g each, show an energy resolution, evaluated at the 2615 keV γ-line of 208Tl, of 6.5 and 4.3 keV FWHM. The only observable internal radioactive contamination arises from 238U (15 and 8 μBq/kg, respectively). The internal activity of the most problematic nuclei for neutrinoless double beta decay, 226Ra and 228Th, are both evaluated as <3.1 μBq/kg for one crystal and <2.3 μBq/kg for the second. Thanks tomore » the readout of the weak Cherenkov light emitted by β/γ particles by means of Neganov–Luke bolometric light detectors we were able to perform an event-by-event identification of β/γ events with a 95% acceptance level, while establishing a rejection factor of 98.21% and 99.99% for α particles.« less

Enriched TeO 2 bolometers with active particle discrimination: Towards the CUPID experiment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Artusa, D. R.; Avignone, F. T.; Beeman, J. W.

We present the performances of two 92% enriched 130TeO2 crystals operated as thermal bolometers in view of a next generation experiment to search for neutrinoless double beta decay of 130Te. The crystals, 435 g each, show an energy resolution, evaluated at the 2615 keV γ-line of 208Tl, of 6.5 and 4.3 keV FWHM. The only observable internal radioactive contamination arises from 238U (15 and 8 μBq/kg, respectively). The internal activity of the most problematic nuclei for neutrinoless double beta decay, 226Ra and 228Th, are both evaluated as <3.1 μBq/kg for one crystal and <2.3 μBq/kg for the second. Thanks tomore » the readout of the weak Cherenkov light emitted by β/γ particles by means of Neganov–Luke bolometric light detectors we were able to perform an event-by-event identification of β/γ events with a 95% acceptance level, while establishing a rejection factor of 98.21% and 99.99% for α particles.« less

Studying the Impact of Modified Saccharides on the Molecular Dynamics and Crystallization Tendencies of Model API Nifedipine.

PubMed

Kaminska, E; Tarnacka, M; Wlodarczyk, P; Jurkiewicz, K; Kolodziejczyk, K; Dulski, M; Haznar-Garbacz, D; Hawelek, L; Kaminski, K; Wlodarczyk, A; Paluch, M

2015-08-03

Molecular dynamics of pure nifedipine and its solid dispersions with modified carbohydrates as well as the crystallization kinetics of active pharmaceutical ingredient (API) above and below the glass transition temperature were studied in detail by means of broadband dielectric spectroscopy (BDS), differential scanning calorimetry (DSC), and X-ray diffraction method. It was found that the activation barrier of crystallization increases in molecular dispersions composed of acetylated disaccharides, whereas it slightly decreases in those consisting of modified monocarbohydrates for the experiments carried out above the glass transition temperature. As shown by molecular dynamics simulations it can be related to the strength, character, and structure of intermolecular interactions between API and saccharides, which vary dependently on the excipient. Long-term physical stability studies showed that, in solid dispersions consisting of acetylated maltose and acetylated sucrose, the crystallization of nifedipine is dramatically slowed down, although it is still observable for a low concentration of excipients. With increasing content of modified carbohydrates, the crystallization of API becomes completely suppressed. This is most likely due to additional barriers relating to the intermolecular interactions and diffusion of nifedipine that must be overcome to trigger the crystallization process.

Science Notes.

ERIC Educational Resources Information Center

School Science Review, 1985

1985-01-01

Presents 23 experiments, activities, field projects and computer programs in the biological and physical sciences. Instructional procedures, experimental designs, materials, and background information are suggested. Topics include fluid mechanics, electricity, crystals, arthropods, limpets, acid neutralization, and software evaluation. (ML)

Chemistry Notes.

ERIC Educational Resources Information Center

School Science Review, 1981

1981-01-01

Describes 13 activities, experiments and demonstrations, including the preparation of iron (III) chloride, simple alpha-helix model, investigating camping gas, redox reactions of some organic compounds, a liquid crystal thermometer, and the oxidation number concept in organic chemistry. (JN)

Dispersed-nanoparticle loading synthesis for monodisperse Au-titania composite particles and their crystallization for highly active UV and visible photocatalysts.

PubMed

Sakamoto, Takeshi; Nagao, Daisuke; Noba, Masahiro; Ishii, Haruyuki; Konno, Mikio

2014-06-24

Submicrometer-sized amorphous titania spheres incorporating Au nanoparticles (NPs) were prepared in a one-pot synthesis consisting of a sol-gel reaction of titanium(IV) isopropoxide in the presence of chloroauric acid and a successive reduction with sodium borohydride in a mixed solvent of ethanol/acetonitrile. The synthesis was allowed to prepare monodisperse titania spheres that homogeneously incorporated Au NPs with sizes of ca. 7 nm. The Au NP-loaded titania spheres underwent different crystallization processes, including 500 °C calcination in air, high-temperature hydrothermal treatment (HHT), and/or low-temperature hydrothermal treatment (LHT). Photocatalytic experiments were conducted with the Au NP-loaded crystalline titania spheres under irradiation of UV and visible light. A combined process of LHT at 80 °C followed by calcination at 500 °C could effectively crystallize titania spheres maintaining the dispersion state of Au NPs, which led to photocatalytic activity higher than that of commercial P25 under UV irradiation. Under visible light irradiation, the Au NP-titania spheres prepared with a crystallization process of LHT at 80 °C for 6 h showed photocatalytic activity much higher than a commercial product of visible light photocatalyst. Structure analysis of the visible light photocatalysts indicates the importance of prevention of the Au NPs aggregation in the crystallization processes for enhancement of photocatalytic activity.

JAXA protein crystallization in space: ongoing improvements for growing high-quality crystals

PubMed Central

Takahashi, Sachiko; Ohta, Kazunori; Furubayashi, Naoki; Yan, Bin; Koga, Misako; Wada, Yoshio; Yamada, Mitsugu; Inaka, Koji; Tanaka, Hiroaki; Miyoshi, Hiroshi; Kobayashi, Tomoyuki; Kamigaichi, Shigeki

2013-01-01

The Japan Aerospace Exploration Agency (JAXA) started a high-quality protein crystal growth project, now called JAXA PCG, on the International Space Station (ISS) in 2002. Using the counter-diffusion technique, 14 sessions of experiments have been performed as of 2012 with 580 proteins crystallized in total. Over the course of these experiments, a user-friendly interface framework for high accessibility has been constructed and crystallization techniques improved; devices to maximize the use of the microgravity environment have been designed, resulting in some high-resolution crystal growth. If crystallization conditions were carefully fixed in ground-based experiments, high-quality protein crystals grew in microgravity in many experiments on the ISS, especially when a highly homogeneous protein sample and a viscous crystallization solution were employed. In this article, the current status of JAXA PCG is discussed, and a rational approach to high-quality protein crystal growth in microgravity based on numerical analyses is explained. PMID:24121350

An evaluation of adhesive sample holders for advanced crystallographic experiments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mazzorana, Marco; Sanchez-Weatherby, Juan, E-mail: juan.sanchez-weatherby@diamond.ac.uk; Sandy, James

Commercially available adhesives have been evaluated for crystal mounting when undertaking complex macromolecular crystallography experiments. Here, their use as tools for advanced sample mounting and cryoprotection is assessed and their suitability for room-temperature data-collection and humidity-controlled studies is investigated. The hydration state of macromolecular crystals often affects their overall order and, ultimately, the quality of the X-ray diffraction pattern that they produce. Post-crystallization techniques that alter the solvent content of a crystal may induce rearrangement within the three-dimensional array making up the crystal, possibly resulting in more ordered packing. The hydration state of a crystal can be manipulated by exposingmore » it to a stream of air at controlled relative humidity in which the crystal can equilibrate. This approach provides a way of exploring crystal hydration space to assess the diffraction capabilities of existing crystals. A key requirement of these experiments is to expose the crystal directly to the dehydrating environment by having the minimum amount of residual mother liquor around it. This is usually achieved by placing the crystal on a flat porous support (Kapton mesh) and removing excess liquid by wicking. Here, an alternative approach is considered whereby crystals are harvested using adhesives that capture naked crystals directly from their crystallization drop, reducing the process to a one-step procedure. The impact of using adhesives to ease the harvesting of different types of crystals is presented together with their contribution to background scattering and their usefulness in dehydration experiments. It is concluded that adhesive supports represent a valuable tool for mounting macromolecular crystals to be used in humidity-controlled experiments and to improve signal-to-noise ratios in diffraction experiments, and how they can protect crystals from modifications in the sample environment is discussed.« less

The inhibition of tetrahydrofuran clathrate-hydrate formation with antifreeze protein

NASA Astrophysics Data System (ADS)

Zeng, H.; Wilson, L. D.; Walker, V. K.; Ripmeester, J. A.

2003-01-01

The effect of Type I fish antifreeze protein (AFP) from the winter flounder, Pleuronectes americanus (Walbaum), (WfAFP) on the formation of tetrahydrofuran (THF) clathrate hydrate was studied by observing changes in THF crystal morphology and determining the induction time for nucleation. AFP retarded THF clathrate-hydrate growth at the tested temperatures and modified the THF clathrate-hydrate crystal morphology from octahedral to plate-like. AFP appears to be even more effective than the kinetic inhibitor, polyvinylpyrrolidone (PVP). Recombinant AFP from an insect, a spruce budworm, Choristoneura fumiferana (Clem.), moth, (Cf) was also tested for inhibition activity by observation of the THF-hydrate-crystal-growth habit. Like WfAFP, CfAFP appeared to show adsorption on multiple THF-hydrate-crystal faces. A protein with no antifreeze activity, cytochrome C, was used as a control and it neither changed the morphology of the THF clathrate-hydrate crystals, nor retarded the formation of the hydrate. Preliminary experiments on the inhibition activity of WfAFP on a natural gas hydrate assessed induction time and the amount of propane gas consumed. Similar to the observations for THF, the data indicated that WfAFP inhibited propane-hydrate growth. Taken together, these results support our hypothesis that AFPs can inhibit clathrate-hydrate growth and as well, offer promise for the understanding of the inhibition mechanism.

UV-Visible Absorption Spectroscopy Enhanced X-ray Crystallography at Synchrotron and X-ray Free Electron Laser Sources.

PubMed

Cohen, Aina E; Doukov, Tzanko; Soltis, Michael S

2016-01-01

This review describes the use of single crystal UV-Visible Absorption micro-Spectrophotometry (UV-Vis AS) to enhance the design and execution of X-ray crystallography experiments for structural investigations of reaction intermediates of redox active and photosensitive proteins. Considerations for UV-Vis AS measurements at the synchrotron and associated instrumentation are described. UV-Vis AS is useful to verify the intermediate state of an enzyme and to monitor the progression of reactions within crystals. Radiation induced redox changes within protein crystals may be monitored to devise effective diffraction data collection strategies. An overview of the specific effects of radiation damage on macromolecular crystals is presented along with data collection strategies that minimize these effects by combining data from multiple crystals used at the synchrotron and with the X-ray free electron laser.

Science Notes.

ERIC Educational Resources Information Center

Piearce, Trevor; And Others

1988-01-01

Provides explanations of 15 experiments, laboratory activities, demonstrations, and lessons for use in instruction. Includes information on Daphnia, wild garlic, crystals, gas chromatographs, bleaches, alcohols, reactivity series, chemistry formula, electronic keyboards and waveforms, interference and diffraction gravity, Moire fringe patterns,…

Influence of two different template removal methods on the micromorphology, crystal structure, and photocatalytic activity of hollow CdS nanospheres

NASA Astrophysics Data System (ADS)

Wang, Han; Jin, Tingting; Zheng, Xing; Jiang, Bo; Zhu, Chaosheng; Yuan, Xiangdong; Zheng, Jingtang; Wu, Mingbo

2016-11-01

Hollow cadmium sulfide (CdS) nanospheres of about 260 nm average diameters and about 30 nm shell thickness can be easily synthesized via a sonochemical process, in which polystyrene (PS) nanoparticles were employed as templates. In order to remove the PS templates, both etching and calcination were applied in this paper. The influence of the two different template removal methods on the surface micromorphology, crystal structure, and photocatalytic activity of hollow CdS nanospheres was carefully performed a comparative study. Results of X-ray diffraction, scanning electron microscopy, transmission electron microscopy, energy dispersive X-ray, FT-IR, thermogravimetric analysis, Brunauer-Emmett-Teller, diffused reflectance spectra, and decolorization experiments showed that the different template removal methods exhibited a significant influence on the surface micromorphology, crystal structure, and photocatalytic activity of hollow CdS nanospheres. The CdS hollow nanospheres as-prepared by etching had pure cubic sphalerite structure, higher -OH content, less defects and exhibited good photocatalytic activity for rhodamine-B, Methylene Blue and methyl orange under UV-vis light irradiation. However, CdS hollow nanospheres obtained by calcination with a hexagonal crystal structure, less -OH content, more defects have shown worse photocatalytic activity. This indicated that surface micromorphology and crystalline phase were mainly factors influencing photocatalytic activity of hollow CdS nanospheres.

High-throughput crystallization screening.

PubMed

Skarina, Tatiana; Xu, Xiaohui; Evdokimova, Elena; Savchenko, Alexei

2014-01-01

Protein structure determination by X-ray crystallography is dependent on obtaining a single protein crystal suitable for diffraction data collection. Due to this requirement, protein crystallization represents a key step in protein structure determination. The conditions for protein crystallization have to be determined empirically for each protein, making this step also a bottleneck in the structure determination process. Typical protein crystallization practice involves parallel setup and monitoring of a considerable number of individual protein crystallization experiments (also called crystallization trials). In these trials the aliquots of purified protein are mixed with a range of solutions composed of a precipitating agent, buffer, and sometimes an additive that have been previously successful in prompting protein crystallization. The individual chemical conditions in which a particular protein shows signs of crystallization are used as a starting point for further crystallization experiments. The goal is optimizing the formation of individual protein crystals of sufficient size and quality to make them suitable for diffraction data collection. Thus the composition of the primary crystallization screen is critical for successful crystallization.Systematic analysis of crystallization experiments carried out on several hundred proteins as part of large-scale structural genomics efforts allowed the optimization of the protein crystallization protocol and identification of a minimal set of 96 crystallization solutions (the "TRAP" screen) that, in our experience, led to crystallization of the maximum number of proteins.

An evaluation of adhesive sample holders for advanced crystallographic experiments

PubMed Central

Mazzorana, Marco; Sanchez-Weatherby, Juan; Sandy, James; Lobley, Carina M. C.; Sorensen, Thomas

2014-01-01

The hydration state of macromolecular crystals often affects their overall order and, ultimately, the quality of the X-ray diffraction pattern that they produce. Post-crystallization techniques that alter the solvent content of a crystal may induce rearrangement within the three-dimensional array making up the crystal, possibly resulting in more ordered packing. The hydration state of a crystal can be manipulated by exposing it to a stream of air at controlled relative humidity in which the crystal can equilibrate. This approach provides a way of exploring crystal hydration space to assess the diffraction capabilities of existing crystals. A key requirement of these experiments is to expose the crystal directly to the dehydrating environment by having the minimum amount of residual mother liquor around it. This is usually achieved by placing the crystal on a flat porous support (Kapton mesh) and removing excess liquid by wicking. Here, an alternative approach is considered whereby crystals are harvested using adhesives that capture naked crystals directly from their crystallization drop, reducing the process to a one-step procedure. The impact of using adhesives to ease the harvesting of different types of crystals is presented together with their contribution to background scattering and their usefulness in dehydration experiments. It is concluded that adhesive supports represent a valuable tool for mounting macromolecular crystals to be used in humidity-controlled experiments and to improve signal-to-noise ratios in diffraction experiments, and how they can protect crystals from modifications in the sample environment is discussed. PMID:25195752

Crystal-rich lava dome extrusion during vesiculation: An experimental study

NASA Astrophysics Data System (ADS)

Pistone, Mattia; Whittington, Alan G.; Andrews, Benjamin J.; Cottrell, Elizabeth

2017-11-01

Lava dome-forming eruptions represent a common eruptive style and a major hazard at numerous active volcanoes worldwide. The extrusion mechanics of crystal-rich lava domes and the influence of volatiles on the transition from viscous to brittle behaviour during lava dome extrusion remain unclear. Understanding how gas exsolution and crystallinity control effusive versus explosive eruption behaviour is essential. Here, we present new experimental results on the rheology of synthesised, crystal-rich (50 to 80 vol% quartz crystals), hydrous (4.2 wt% H2O in the glass) dacite samples, which vesiculate from 5 to 27 vol% gas bubbles at high temperatures (from glass transition temperature to 797 °C) during deformation conducted in a parallel plate viscometer (constant stress at 0.63-0.64 MPa, and variable strain-rates ranging from 8.32·10- 8 to 3.58·10- 5 s- 1). The experiments reproduce certain aspects of lava dome deformation in volcanic conduits during vesiculation of the residual melt, instigated in the experiments by increasing temperature. During gas exsolution (i.e. nucleation and growth of gas-pressurised bubbles) and volume inflation, we find that the rheological lubrication of the system during deformation is strongly dictated by the initial crystallinity. At crystal contents < 60 vol%, gas bubbles form and coalesce during expansion and viscous deformation, favouring strain localisation and gas permeability within shear bands, which control the overall sample rheology. At crystallinities of 60 to 70 vol%, gas exsolution generates pressurisation (i.e. pore pressure increase) within the bubbles trapped in the solid crystal clusters, and embryonic formation of microscopic fractures through melt and crystals drives the system to a brittle behaviour. At higher crystallinity (80 vol%) vesiculation leads to large pressurisation, which then triggers extensive brittle fragmentation. Through macroscopic fractures, outgassing determines the rheological stalling of the system. In the light of these results we propose a rheological description of crystal-rich lava dome mechanics. The contrasting experimental behaviours at different crystallinities have implications for the style of slow-ascending dome-forming eruptions. All other factors being equal, our experiments suggest that crystal-poor magmas will undergo efficient outgassing, reducing the potential for an explosive eruption. Conversely, crystal-rich magmas may experience limited outgassing and larger gas overpressures during vesiculation, therefore increasing the potential for an explosive eruption.

Structure determination of uracil-DNA N-glycosylase from Deinococcus radiodurans in complex with DNA.

PubMed

Pedersen, Hege Lynum; Johnson, Kenneth A; McVey, Colin E; Leiros, Ingar; Moe, Elin

2015-10-01

Uracil-DNA N-glycosylase (UNG) is a DNA-repair enzyme in the base-excision repair (BER) pathway which removes uracil from DNA. Here, the crystal structure of UNG from the extremophilic bacterium Deinococcus radiodurans (DrUNG) in complex with DNA is reported at a resolution of 1.35 Å. Prior to the crystallization experiments, the affinity between DrUNG and different DNA oligonucleotides was tested by electrophoretic mobility shift assays (EMSAs). As a result of this analysis, two 16 nt double-stranded DNAs were chosen for the co-crystallization experiments, one of which (16 nt AU) resulted in well diffracting crystals. The DNA in the co-crystal structure contained an abasic site (substrate product) flipped into the active site of the enzyme, with no uracil in the active-site pocket. Despite the high resolution, it was not possible to fit all of the terminal nucleotides of the DNA complex into electron density owing to disorder caused by a lack of stabilizing interactions. However, the DNA which was in contact with the enzyme, close to the active site, was well ordered and allowed detailed analysis of the enzyme-DNA interaction. The complex revealed that the interaction between DrUNG and DNA is similar to that in the previously determined crystal structure of human UNG (hUNG) in complex with DNA [Slupphaug et al. (1996). Nature (London), 384, 87-92]. Substitutions in a (here defined) variable part of the leucine loop result in a shorter loop (eight residues instead of nine) in DrUNG compared with hUNG; regardless of this, it seems to fulfil its role and generate a stabilizing force with the minor groove upon flipping out of the damaged base into the active site. The structure also provides a rationale for the previously observed high catalytic efficiency of DrUNG caused by high substrate affinity by demonstrating an increased number of long-range electrostatic interactions between the enzyme and the DNA. Interestingly, specific interactions between residues in the N-terminus of a symmetry-related molecule and the complementary DNA strand facing away from the active site were also observed which seem to stabilize the enzyme-DNA complex. However, the significance of this observation remains to be investigated. The results provide new insights into the current knowledge about DNA damage recognition and repair by uracil-DNA glycosylases.

Crystallization and preliminary X-ray diffraction data of β-galactosidase from Aspergillus niger.

PubMed

Rico-Díaz, Agustín; Vizoso Vázquez, Ángel; Cerdán, M Esperanza; Becerra, Manuel; Sanz-Aparicio, Julia

2014-11-01

β-Galactosidase from Aspergillus niger (An-β-Gal), belonging to the family 35 glycoside hydrolases, hydrolyzes the β-galactosidase linkages in lactose and other galactosides. It is extensively used in industry owing to its high hydrolytic activity and safety. The enzyme has been expressed in yeasts and purified by immobilized metal-ion affinity chromatography for crystallization experiments. The recombinant An-β-Gal, deglycosylated to avoid heterogeneity of the sample, has a molecular mass of 109 kDa. Rod-shaped crystals grew using PEG 3350 as the main precipitant agent. A diffraction data set was collected to 1.8 Å resolution.

Adsorption of Crystal Violet on Activated Carbon Prepared from Coal Flotation Concentrate

NASA Astrophysics Data System (ADS)

Aydogmus, Ramazan; Depci, Tolga; Sarikaya, Musa; Riza Kul, Ali; Onal, Yunus

2016-10-01

The objective of this study is firstly to investigate the floatability properties of Zilan- Van coal after microwave irradiation and secondly to produce activated carbon from flotation concentrate in order to remove Crystal Violet (CV) from waste water. The flotation experiments showed that microwave heating at 0.9 kW power level for 60 sec exposure time enhanced the hydrophobicity and increased the flotation yield. The activated carbon with remarkable surface area (696 m2/g) was produced from the flotation concentrate and used to adsorb CV from aqueous solution in a batch reactor at different temperature. The adsorption properties of CV onto the activated carbon are discussed in terms of the adsorption isotherms (Langmuir and Freundlich) and found that the experimental results best fitted by the Langmuir model.

An Experiment with Manifold Purposes: The Chemical Reactivity of Crystal Defects upon Crystal Dissolution.

ERIC Educational Resources Information Center

Lazzarini, Annaluisa Fantola; Lazzarini, Ennio

1983-01-01

Background information and procedures are provided for an experiment designed to introduce (1) crystal defects and their reactivity upon crystal dissolution; (2) hydrates electron and its reactivity; (3) application of radiochemical method of analysis; and (4) the technique of competitive kinetics. Suggested readings and additional experiments are…

[A prediction model for the activity of insecticidal crystal proteins from Bacillus thuringiensis based on support vector machine].

PubMed

Lin, Yi; Cai, Fu-Ying; Zhang, Guang-Ya

2007-01-01

A quantitative structure-property relationship (QSPR) model in terms of amino acid composition and the activity of Bacillus thuringiensis insecticidal crystal proteins was established. Support vector machine (SVM) is a novel general machine-learning tool based on the structural risk minimization principle that exhibits good generalization when fault samples are few; it is especially suitable for classification, forecasting, and estimation in cases where small amounts of samples are involved such as fault diagnosis; however, some parameters of SVM are selected based on the experience of the operator, which has led to decreased efficiency of SVM in practical application. The uniform design (UD) method was applied to optimize the running parameters of SVM. It was found that the average accuracy rate approached 73% when the penalty factor was 0.01, the epsilon 0.2, the gamma 0.05, and the range 0.5. The results indicated that UD might be used an effective method to optimize the parameters of SVM and SVM and could be used as an alternative powerful modeling tool for QSPR studies of the activity of Bacillus thuringiensis (Bt) insecticidal crystal proteins. Therefore, a novel method for predicting the insecticidal activity of Bt insecticidal crystal proteins was proposed by the authors of this study.

Dynamical Properties of a Living Nematic

NASA Astrophysics Data System (ADS)

Genkin, Mikhail

The systems, which are made of a large number or interacting particles, or agents that convert the energy stored in the environment into mechanical motion, are called active systems, or active matter. The examples of active matter include both living and synthetic systems. The size of agents varies significantly: bird flocks and fish schools represent macroscopic active systems, while suspensions of living organisms or artificial colloidal particles are examples of microscopic ones. In this work, I studied one of the simplest realization of active matter termed living (or active) nematics, that can be conceived by mixing swimming bacteria and nematic liquid crystal. Using modeling, numerical simulations and experiments I studied various dynamical properties of active nematics. This work hints into new methods of control and manipulation of active matter. Active nematic exhibits complex spatiotemporal behavior manifested by formation, proliferation, and annihilation of topological defects. A new computational 2D model coupling nematic liquid crystal and swimming bacteria dynamics have been proposed. We investigated the developed system of partial differential equations analytically and integrated it numerically using the highly efficient parallel GPU code. The integration results are in a very good agreement with other theoretical and experimental studies. In addition, our model revealed a number of testable phenomena. The major model prediction (bacteria accumulation in positive and depletion in negative topological defects) was tested by a dedicated experiment. We extended our model to study active nematics in a biphasic state, where nematic and isotropic phases coexist. Typically this coexistence is manifested by formation of tactoids - isotropic elongated regions surrounded by nematic phase, or nematic regions surrounded by isotropic phase. Using numerical integration, we revealed fundamental properties of such systems. Our main model outcome - spontaneous negative charging of isotropic-nematic interfaces - was confirmed by the experiment. The provided modeling and experimental results are in a very good qualitative and quantitative agreement. At last, we studied living nematics experimentally. We worked with swimming bacteria Bacillus subtilis suspended in disodium cromoglycate (DSCG) liquid crystal. Using cylindrical confinement, we were able to observe quantization of nematics' bending instability. Our experimental results revealed a complex interplay between bacteria self-propulsion and nematics' elasticity in the presence of cylindrical confinements of different sizes.

Investigating the origins of double photopeaks in CsI:Tl samples through activator mapping

NASA Astrophysics Data System (ADS)

Onken, Drew R.; Gridin, Sergii; Williams, Richard T.; Williams, Charles B.; Donati, George L.; Gayshan, Vadim; Vasyukov, Sergey; Gektin, Alex

2018-06-01

Careful examination of the origins of double photopeaks in CsI:Tl provides a foundation for exploring the relationship between activator homogeneity and photopeak resolution in scintillators. In rare cases, certain CsI:Tl crystals exhibit a second photopeak in the pulse-height spectrum. A combination of optical mapping and ICP-MS measurements reveals the presence of two distinct regions with differing Tl concentrations in these crystals. The oscillator strength of the 299 nm absorption A-band of Tl in CsI was measured to be 0.0526 ± 0.0008; this parameter can be used to quantify activator concentration from the optical absorption. Using published measurements of luminescence intensity versus Tl concentration, the distributions of Tl measured from optical absorption maps of the samples were reconstructed into photopeaks in good agreement with experiment. The distribution of Tl concentrations in these particular crystals allowed examining luminescence pulse shape as a function of Tl concentration.

Oilfield scales: controls on precipitation and crystal morphology of barite (barium sulphate)

NASA Astrophysics Data System (ADS)

Stark, A. I. R.; Wogelius, R. A.; Vaughan, D. J.

2003-04-01

The precipitation and subsequent build up of barite (barium sulphate) inside extraction tubing presents a costly problem for off shore oil wells which use seawater to mobilize oil during hydrocarbon recovery. Mixing of reservoir formation water containing Ba2+ ions and seawater containing SO_42- ions results in barite precipitation within the reservoir well-bore region and piping. Great effort has been expended in designing strategies to minimize scale formation but details of the reaction mechanism and sensitivity to thermodynamic variables are poorly constrained. Furthermore, few detailed studies have been carried out under simulated field conditions. Hence an experimental programme was designed to study barite formation under environmentally relevant conditions with control of several system variables during the precipitation reaction. Synthetic sea-water and formation-water brines containing sodium sulphate and barium chloride, respectively, were mixed to induce BaSO_4 precipitation. Experiments were carried out at high temperature (100^oC) and high pressure (500 bars) in double rocking autoclave bombs. Barite formation as a function of the addition of calcium, magnesium, and a generic phosphonate based scale inhibitor was investigated whilst maintaining constant pH, temperature and ionic strength (0.5159). Additional experiments were performed at ambient conditions for comparison. Data concerning nucleation, growth rates, and crystal morphology were obtained. ICP-AES data from the supernatant product solutions showed considerable variation in quantity of barium sulphate precipitated as a function of the listed experimental variables. For example, ESEM analysis of barium sulphate crystals showed a dramatic shift in crystal habit from the typical tabular habit produced in control experiments; experiments performed in the presence of foreign cations produced more equant crystals, while those experiments completed in the presence of the phosphonate scale inhibitor produced precipitates with distorted anhedral shapes. Based on these preliminary results, further experiments which monitor rate and morphology as a function of Ba/Ca ratio, ionic strength, and ion activity product for barite will also be completed.

The Underground Laboratory in South Korea : facilities and experiments

NASA Astrophysics Data System (ADS)

Kim, Yeongduk

2017-01-01

We have developed underground physics programs for last 15 years in South Korea. The scientific and technical motivation for this initiative was the lack of local facility of a large accelerator in Korea. Thanks to the large underground electric power generator in Yangyang area, we could construct a deep underground laboratory (Yangyang Laboratory, Y2L) and has performed some pioneering experiments for dark matter search and double beta decay experiments. Since year of 2013, a new research center in the Institute for Basic Science (IBS), Center for Underground Physics (CUP), is approved by the government and Y2L laboratory is managed by CUP. Due to the limited space in Y2L, we are proposing to construct a new deep underground laboratory where we can host larger scale experiments of next generation. The site is in an active iron mine, and will be made in 1100 meter underground with a space of about 2000 m2 by the end of 2019. I will describe the status and future plan for this underground laboratory. CUP has two main experimental programs. (1) Identification of dark matter : The annual modulation signal of DAMA/LIBRA experiment has been contradictory to many other experiments such as XENON100, LUX, and Super CDMS. Yale University and CUP (COSINE-100) experimentalists agreed to do an experiment together at the Y2L and recently commissioned a 100kg scale low background NaI(Tl) crystal experiment. In future, we will develop NaI(Tl) crystals with lower internal backgrounds and try to run identical detectors at both north and south hemisphere. Low mass WIMP search is also planned with a development of low temperature sensors coupled with highly scintillating crystals. (2) Neutrinoless double beta decay search : The mass of the lightest neutrino and the Majorana nature of the neutrinos are not determined yet. Neutrinoless double beta decay experiment can answer both of the questions directly, and ultra-low backgrounds and excellent energy resolution are critical to discover this ultra rare phenomena. AMoRE (Advanced Mo-based Rare phenomena Experiment) is a state-of-art experiment based on low temperature MMC sensor and ultra pure molybdate crystals containing highly enriched isotopes. With 200 kg of molybdate crystals running 3 years, It's sensitivity goal is reaching 1027 years of half-life and down to 15-30 meV neutrino mass. AMoRE-pilot experiment with 1.5 kg of enriched Mo-100 crystals is running at Y2L now. In addition to the two main physics program, CUP is doing NEOS short baseline neutrino experiment and also develops new experiments for new parameter search for dark photons, WIMPs, and double beta decay experiments.

On the development of two characteristically different crystal morphology in SiO(2)-MgO-Al (2)O (3)-K (2)O-B (2)O (3)-F glass-ceramic system.

PubMed

Roy, Shibayan; Basu, Bikramjit

2009-01-01

The present work demonstrates how crystals with two different characteristic morphologies can be formed in SiO(2)-MgO-Al(2)O(3)-K(2)O-B(2)O(3)-F glass-ceramic system by adopting two sets of heat treatment experiments. In our study, single stage heat treatment experiments were performed at 1,000 degrees C for varying holding time of 8-24 h with 4 h time interval and as a function of temperature in the range of 1,000-1,120 degrees C with 40 degrees C temperature interval. The constant heating rate of 10 degrees C/min was employed for both sets of experiments. The microstructural changes were investigated using Fourier transformed infrared spectroscopy (FT-IR), SEM-EDS and XRD. For temperature variation batches, the microstructure is characterized by interlocked, randomly oriented mica plates ('house-of-cards' morphology). An important and new observation of complex crystal morphology is made in the samples heat treated at 1,000 degrees C for varying holding times. Such morphology appears to be the results of composite spherulitic-dendritic like growth of mica rods radiating from a central nucleus. The possible mechanism for such characteristic crystal growth morphology is discussed with reference to a nucleation-growth kinetics based model. The activation energy for crystal nucleation and Avrami index are computed to be 388 kJ/mol and 1.3 respectively, assuming Johnson-Mehl-Avrami model of crystallization. Another important result is that a maximum of around 70% of spherulitic-dendritic like crystal morphology can be obtained after heat treatment at 1,000 degrees C for 24 h, while a lower amount (approximately 58%) of interlocked plate like mica crystals is formed after heat treatment at 1,040 degrees C for 4 h.

Characterization of the Protein Crystal Growth Apparatus for Microgravity Aboard the Space Station

NASA Technical Reports Server (NTRS)

Kundrot, Craig E.; Roeber, D.; Achari, A.; Stinson, Thomas N. (Technical Monitor)

2002-01-01

We have conducted experiments to determine the equilibration rates of some major precipitants used in protein crystallography aboard the International Space Station (ISS). The solutions were placed in the Protein Crystallization Apparatus for Microgravity (PCAM) which mimic Cryschem sitting drop trays. The trays were placed in cylinders. These cylinders were placed inside a Single locker Thermal Enclosure System (STES), and were activated for different durations during the flight. Bumpers pressed against elastomers seal drops in a deactivated state during pre-flight and prior to transfer to the ISS. Activation occurs while in flight on the ISS by releasing the bumpers allowing the drops to be exposed to the reservoir. PCAM was flown to the ISS on STS 100, Flight 6A, on April 19, 2001. Six series of equilibration experiments were tested for each precipitant with a small amount of Green Fluorescent Protein (GFP). Cylinder 10 was never activated, 7 was activated for 40 days, 8 was activated for 20 days, 9 was activated for 10 days, 11 was activated for 4 days and 12 was activated for 2 days. Upon the return to Earth by STS 104 on July 24,2001 the samples were transferred to Marshall Space Flight Center. The samples were then brought to the lab and the volumes of each sample were measured.

Antioxidative succinobucol-sterol conjugates: Crystal structures and pseudosymmetry in the crystals

NASA Astrophysics Data System (ADS)

Ikonen, Satu; Jurček, Ondřej; Wimmer, Zdeněk; Drašar, Pavel; Kolehmainen, Erkki

2012-03-01

An extensive study to attach succinobucol to sterols has provided conjugates which comprise two pharmaceutically important compounds into one entity where the components are expected to have a synergistic effect. The motivation to design these novel conjugates was the need to broaden the armamentarium of current agents used in the treatment of atherosclerotic diseases and type 2 diabetes. In desire for detailed information of these compounds in solid state, which also have an influence to their physiological activity, systematic crystallization experiments were performed and as a result, X-ray quality single crystals were obtained from four succinobucol-sterol conjugates. All of these compounds crystallized in space group P1 with two or four molecules in an asymmetric unit and the crystallographically independent molecules were found to be related by pseudosymmetry (i.e. by pseudoinversion in 1-3 and by pseudoinversion plus pseudotranslation in 4).

Thermal, optical, mechanical and electrical properties of a novel NLO active L-phenylalanine L-phenylalaninium perchlorate single crystals

NASA Astrophysics Data System (ADS)

Cyrac Peter, A.; Vimalan, M.; Sagayaraj, P.; Madhavan, J.

2010-01-01

Single crystals of L-phenylalanine L-phenylalaninium perchlorate (LPAPCl), a semiorganic nonlinear (NLO) material have been successfully grown up to a size of 14 mm×5 mm×3 mm. The lattice parameters of the grown crystals are determined by single crystal XRD. The UV-Vis-NIR spectrum of LPAPCl show less optical absorption in the entire visible region. Nonlinear optical study reveals that the SHG efficiency of LPAPCl is nearly 1.4 times that of KDP. The laser damage density is found to be 7.4 GW/cm 2. The crystals are subjected to microhardness studies and the variation of the microhardness with the applied load is studied. The response of dielectric constant in the frequency region of 50 Hz to 5 MHz has been investigated. AC and DC conductivity and photoconductivity experiments are also carried out and the results are discussed.

Precision Crystal Calorimeters in High Energy Physics

ScienceCinema

Ren-Yuan Zhu

2017-12-09

Precision crystal calorimeters traditionally play an important role in high energy physics experiments. In the last two decades, it faces a challenge to maintain its precision in a hostile radiation environment. This paper reviews the performance of crystal calorimeters constructed for high energy physics experiments and the progress achieved in understanding crystal’s radiation damage as well as in developing high quality scintillating crystals for particle physics. Potential applications of new generation scintillating crystals of high density and high light yield, such as LSO and LYSO, in particle physics experiments is also discussed.

Crystal-rich lava dome extrusion during vesiculation: an experimental study

NASA Astrophysics Data System (ADS)

Pistone, M.; Whittington, A. G.; Andrews, B. J.; Cottrell, E.

2016-12-01

Lava dome-forming eruptions represent a common eruptive style and a major hazard on numerous active volcanoes worldwide. The influence of volatiles on the rheological mechanics of lava dome extrusion remains unclear. Here we present new experimental results on the rheology of synthesized, crystal-rich (50 to 80 vol% quartz crystals), hydrous (4.2 wt% H2O in the glass) dacites, which vesiculate from 5 to 27 vol% gas bubbles at high temperatures (483 to 797 °C) during deformation conducted in a parallel plate viscometer (constant stress at 0.64 MPa, and variable strain-rates ranging from 8.32•10-8 to 3.58•10-5 s-1). The experiments replicated lava dome deformation in volcanic conduits during vesiculation of the residual melt, instigated in the experiments by increasing temperature. During gas exsolution we find that the rheological lubrication of the system during deformation is strongly dictated by the imposed initial crystallinity. At low crystal content (< 60 vol%) strain localization within shear bands, composed of melt and gas bubbles that likely interconnect, controls the overall sample rheology. At high crystallinity (60 to 70 vol%) gas pressurization (i.e. pore pressure increase) within crystal clusters and embryonic formation of microscopic fractures drive the system to a brittle behavior. At higher crystallinity (80 vol%) gas pressurization triggers brittle fragmentation through macroscopic fractures, which sustain outgassing and determines the viscous death of the system. The contrasting behaviors at different crystallinities have direct impact on the style of volcanic eruptions. Outgassing induced by deformation and bubble coalescence reduces the system pressurization and the potential for an explosive eruption. Conversely, high crystallinity lava domes experience limited loss of exsolved gas during deformation, permitting the achievement of large overpressures prior to fragmentation, favoring likely explosive eruptions. These findings provide a dataset that might be used to constrain the physical properties of natural lava domes at active volcanoes and show how crystallinity and corresponding gas pressurization control dome growth rate and consequent eruption style.

Purification, Crystallization, and Preliminary X-ray Analysis of Native Canavalin

NASA Technical Reports Server (NTRS)

Pusey, Marc; Dowell, Jennifer; Ng, Joseph; Gavira, Jose A.

2003-01-01

The protein canavalin is a 7S vicilin, from the Jack Bean, Canavalis ensfomis. Canavalin is described as a seed storage protein, an energy source for a developing seed, as no other known activity or function has been found. The protein was first isolated and crystallized by Sumner and Howell (J. Biol. Chem. 113, 607-610, 1936). Canavalin spontaneously crystallizes after proteolytic cleavage at neutral pH, which removes residues 1-46, 224-245, and 325-330 and produces peptides of approximately 25, 13, and 12 kDa. Preliminary gel filtration experiments indicated the presence of nucleic acid with the uncleaved protein. We developed a dual column procedure, ion exchange followed by hydroxy apatite chromatography, that effectively removes the nucleic acid and yields an essentially pure uncut canavalin preparation with an OD 280/260 ratio of approximately 1.9-2.0. Standard crystallization screens using this material gave a number of positive results having a common requirement for alcohols and Mg(2+) ion, with crystals typically appearing within a day or less. Optimization experiments to date have shown that we can obtain crystals from pH 6.5 to pH 8.2, using MPD from 5 to 20% and 0.05 to 0.2M Mg(2+) (sulfate or acetate). The crystals are of space group P2(sub 1)2(sub 1)2(sub 1), unit cell dimensions, and a complete data set to 1.5 Angstroms, resolution has now been collected at a synchrotron source. Most importantly, the crystals are not twinned, a persistent problem with the most commonly obtained rhombohedral form of proteolytically cleaved canavalin.

Synthesis, crystal structure, Hirshfeld surfaces analysis and anti-ischemic activity of cinnamide derivatives

NASA Astrophysics Data System (ADS)

Zhong, Jian-gang; Han, Jia-pei; Li, Xiao-feng; Xu, Yi; Zhong, Yan; Wu, Bin

2018-02-01

Two cinnamide derivatives, namely, (E)-1-(4-(bis(4-methylphenyl)- methyl)piperazin-1-yl)-3-(3,4-diethoxyphenyl)prop-2-en-1-one (5) and (E)-1-(4-(bis- (4-fluorophenyl)methyl)piperazin-1-yl)-3-(4-methoxyphenyl)prop-2-en-1-one (6), have been synthesized and characterized by IR spectra, High resolution mass spectra, 1H NMR spectra, 13C NMR spectra. The compound 5 is a novel compound and has never been reported in the literature. Their crystal structures were studied by single-crystal X-ray diffraction. They all crystallize in the monoclinic system. The single-crystal X-ray revealed that compound 5 has infinite X-shaped 1-D polymeric chains structure and compound 6 has a layered 3-D structure by intermolecular interactions. Hirshfeld surface analysis demonstrated the presence of H⋯H, O⋯H, C⋯H, F⋯H, Csbnd H⋯π and π⋯π intermolecular interactions. In addition, the MTT assay results indicated that the compounds 5 and 6 display effective activities against neurotoxicity which is induced by glutamine in PC12 cells. The in vivo experiment indicated that the compound 6 has a good protective effect on cerebral infarction.

Laboratory studies of crystal growth in magma

NASA Astrophysics Data System (ADS)

Hammer, J. E.; Welsch, B. T.; First, E.; Shea, T.

2012-12-01

The proportions, compositions, and interrelationships among crystalline phases and glasses in volcanic rocks cryptically record pre-eruptive intensive conditions, the timing of changes in crystallization environment, and the devolatilization history of eruptive ascent. These parameters are recognized as important monitoring tools at active volcanoes and interpreting geologic events at prehistoric and remote eruptions, thus motivating our attempts to understand the information preserved in crystals through an experimental appoach. We are performing laboratory experiments in mafic, felsic, and intermediate composition magmas to study the mechanisms of crystal growth in thermochemical environments relevant to volcanic environments. We target features common to natural crystals in igneous rocks for our experimental studies of rapid crystal growth phenomena: (1) Surface curvature. Do curved interfaces and spongy cores represent evidence of dissolution (i.e., are they corrosion features), or do they record the transition from dendritic to polyhedral morphology? (2) Trapped melt inclusions. Do trapped liquids represent bulk (i.e., far-field) liquids, boundary layer liquids, or something intermediate, depending on individual species diffusivity? What sequence of crystal growth rates leads to preservation of sealed melt inclusions? (3) Subgrain boundaries. Natural phenocrysts commonly exhibit tabular subgrain regions distinguished by small angle lattice misorientations or "dislocation lamellae" and undulatory extinction. Might these crystal defects be produced as dendrites undergo ripening? (4) Clusters. Contacting clusters of polymineralic crystals are the building blocks of cumulates, and are ubiquitous features of mafic volcanic rocks. Are plagioclase and clinopyroxene aligned crystallographically, suggesting an epitaxial (surface energy) relationship? (5) Log-normal size distribution. What synthetic cooling histories produce "natural" distributions of crystal sizes, and are phenocrystic textures uniquely attributed to staged cooling? In addition, we seek to explore the limitations of the experimental approach. Which aspects of natural crystallization sequences are adequately reproduced in experimental charges, and which are compromised by the obligatory reduced temporal and spatial scales of crystal growth experiments? What are the implications of synthetic starting materials and thermal pre-treatments for nucleation, growth, heterophase equilibria, and textural maturation?

Protein crystal growth in a microgravity environment

NASA Technical Reports Server (NTRS)

Bugg, Charles E.

1988-01-01

Protein crystal growth is a major experimental problem and is the bottleneck in widespread applications of protein crystallography. Research efforts now being pursued and sponsored by NASA are making fundamental contributions to the understanding of the science of protein crystal growth. Microgravity environments offer the possibility of performing new types of experiments that may produce a better understanding of protein crystal growth processes and may permit growth environments that are more favorable for obtaining high quality protein crystals. A series of protein crystal growth experiments using the space shuttle was initiated. The first phase of these experiments was focused on the development of micro-methods for protein crystal growth by vapor diffusion techniques, using a space version of the hanging drop method. The preliminary space experiments were used to evolve prototype hardware that will form the basis for a more advanced system that can be used to evaluate effects of gravity on protein crystal growth.

GEODE 2: Manufacturing large area format cadmium-mercury-telluride crystals in a microgravity environment. Pressure sensor proof of concept

NASA Astrophysics Data System (ADS)

Gale, M. R.; Beattie, D. A.

In the GEODE 1 experiment, a semiconductor Cd-Hg telluride crystal was grown in the MASER1 sounding rocket. It was shown that bulk-quench Cd-Hg telluride crystallization in a microgravity environment results in a more homogeneous crystal structure than can be achieved terrestrially. In the GEODE 2 program, the wall thickness of the quartz ampoule containing the crystal will be reduced to improve the heat transfer characteristics during crystallization. Ampoule explosion must be prevented by active control of the pressure surrounding the weaker, thin-walled ampoule to match that inside the furnace. A prototype pressure sensor that uses the absorption of ultraviolet light by Hg vapor has been built and tested. Pressures from 4 to 40 atmospheres have been measured with a resolution better than 0.35 atmospheres over the entire range. The feasibility of the pressure measurement technique has been demonstrated, although some design improvements are required in order to make measurements more repeatable.

Embeded photonic crystal at the interface of p-GaN and Ag reflector to improve light extraction of GaN-based flip-chip light-emitting diode

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhen, Aigong; Ma, Ping, E-mail: maping@semi.ac.cn; Zhang, Yonghui

2014-12-22

In this experiment, a flip-chip light-emitting diode with photonic crystal was fabricated at the interface of p-GaN and Ag reflector via nanospheres lithography technique. In this structure, photonic crystal could couple with the guide-light efficiently by reason of the little distance between photonic crystal and active region. The light output power of light emitting diode with embedded photonic crystal was 1.42 times larger than that of planar flip-chip light-emitting diode. Moreover, the embedded photonic crystal structure makes the far-field divergence angle decreased by 18° without spectra shift. The three-dimensional finite difference time domain simulation results show that photonic crystal couldmore » improve the light extraction, and enhance the light absorption caused by Ag reflector simultaneously, because of the roughed surface. The depth of photonic crystal is the key parameter affecting the light extraction and absorption. Light extraction efficiency increases with the depth photonic crystal structure rapidly, and reaches the maximum at the depth 80 nm, beyond which light extraction decrease drastically.« less

Detailed analysis of Honeywell In-Space Accelerometer data - STS-32. [crystal microstructure response to different types of residual acceleration

NASA Technical Reports Server (NTRS)

Rogers, Melissa J. B.; Alexander, J. I. D.; Schoess, Jeff

1993-01-01

The Honeywell In-Space Accelerometer (HISA) system collected data in the mid-deck area of the Shuttle Columbia during the flight of STS-32, January 1990. The resulting data were to be used to investigate the response of crystal microstructure to different types of residual acceleration. The HISA is designed to detect and record transient and oscillatory accelerations. The sampling and electronics package stored averaged accelerations over two sampling periods; two sampling rates were available: 1 Hz and 50 Hz. Analysis of the HISA data followed the CMMR Acceleration Data Processing Guide, considering in-house computer modelling of a float-zone indium crystal growth experiment. Characteristic examples of HISA data showing the response to the primary reaction control system, Orbiter Maneuvering System operations, and crew treadmill activity are presented. Various orbiter structural modes are excited by these and other activities.

Cleavage of nicotinamide adenine dinucleotide by the ribosome-inactivating protein from Momordica charantia.

PubMed

Vinkovic, M; Dunn, G; Wood, G E; Husain, J; Wood, S P; Gill, R

2015-09-01

The interaction of momordin, a type 1 ribosome-inactivating protein from Momordica charantia, with NADP(+) and NADPH has been investigated by X-ray diffraction analysis of complexes generated by co-crystallization and crystal soaking. It is known that the proteins of this family readily cleave the adenine-ribose bond of adenosine and related nucleotides in the crystal, leaving the product, adenine, bound to the enzyme active site. Surprisingly, the nicotinamide-ribose bond of oxidized NADP(+) is cleaved, leaving nicotinamide bound in the active site in the same position but in a slightly different orientation to that of the five-membered ring of adenine. No binding or cleavage of NADPH was observed at pH 7.4 in these experiments. These observations are in accord with current views of the enzyme mechanism and may contribute to ongoing searches for effective inhibitors.

Carboxylic acids in crystallization of macromolecules: learning from successful crystallization experiments.

PubMed

Offermann, Lesa R; He, John Z; Mank, Nicholas J; Booth, William T; Chruszcz, Maksymilian

2014-03-01

The production of macromolecular crystals suitable for structural analysis is one of the most important and limiting steps in the structure determination process. Often, preliminary crystallization trials are performed using hundreds of empirically selected conditions. Carboxylic acids and/or their salts are one of the most popular components of these empirically derived crystallization conditions. Our findings indicate that almost 40 % of entries deposited to the Protein Data Bank (PDB) reporting crystallization conditions contain at least one carboxylic acid. In order to analyze the role of carboxylic acids in macromolecular crystallization, a large-scale analysis of the successful crystallization experiments reported to the PDB was performed. The PDB is currently the largest source of crystallization data, however it is not easily searchable. These complications are due to a combination of a free text format, which is used to capture information on the crystallization experiments, and the inconsistent naming of chemicals used in crystallization experiments. Despite these difficulties, our approach allows for the extraction of over 47,000 crystallization conditions from the PDB. Initially, the selected conditions were investigated to determine which carboxylic acids or their salts are most often present in crystallization solutions. From this group, selected sets of crystallization conditions were analyzed in detail, assessing parameters such as concentration, pH, and precipitant used. Our findings will lead to the design of new crystallization screens focused around carboxylic acids.

Chiral Crystallization of Ethylenediamine Sulfate

ERIC Educational Resources Information Center

Koby, Lawrence; Ningappa, Jyothi B.; Dakesssian, Maria; Cuccia, Louis A.

2005-01-01

The optimal conditions for the crystallization of achiral ethylenediamine sulfate into large chiral crystals that are ideal for polarimetry studies and observation using Polaroid sheets are presented. This experiment is an ideal undergraduate experiment, which clearly demonstrates the chiral crystallization of an achiral molecule.

Preliminary investigations of protein crystal growth using the Space Shuttle

NASA Technical Reports Server (NTRS)

Delucas, L. J.; Suddath, F. L.; Snyder, R.; Naumann, R.; Broom, M. B.; Pusey, M.; Yost, V.; Herren, B .; Carter, D.

1986-01-01

Four preliminary Shuttle experiments are described which have been used to develop prototype hardware for a more advanced system that will evaluate effects of gravity on protein crystal growth. The first phase of these experiments has centered on the development of micromethods for protein crystal growth by vapor-diffusion techniques (using a space version of the hanging-drop method) and on dialysis using microdialysis cells. Results suggest that the elimination of density-driven sedimentation can effect crystal morphology. In the dialysis experiment, space-grown crystals of concanavalin B were three times longer and 1/3 the thickness of earth-grown crystals.

The plug-based nanovolume Microcapillary Protein Crystallization System (MPCS)

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gerdts, Cory J.; Elliott, Mark; Lovell, Scott

2012-02-08

The Microcapillary Protein Crystallization System (MPCS) embodies a new semi-automated plug-based crystallization technology which enables nanolitre-volume screening of crystallization conditions in a plasticware format that allows crystals to be easily removed for traditional cryoprotection and X-ray diffraction data collection. Protein crystals grown in these plastic devices can be directly subjected to in situ X-ray diffraction studies. The MPCS integrates the formulation of crystallization cocktails with the preparation of the crystallization experiments. Within microfluidic Teflon tubing or the microfluidic circuitry of a plastic CrystalCard, {approx}10-20 nl volume droplets are generated, each representing a microbatch-style crystallization experiment with a different chemical composition.more » The entire protein sample is utilized in crystallization experiments. Sparse-matrix screening and chemical gradient screening can be combined in one comprehensive 'hybrid' crystallization trial. The technology lends itself well to optimization by high-granularity gradient screening using optimization reagents such as precipitation agents, ligands or cryoprotectants.« less

Scintillation properties of selected oxide monocrystals activated with Ce and Pr

NASA Astrophysics Data System (ADS)

Wojtowicz, Andrzej J.; Drozdowski, Winicjusz; Wisniewski, Dariusz; Lefaucheur, Jean-Luc; Galazka, Zbigniew; Gou, Zhenhui; Lukasiewicz, Tadeusz; Kisielewski, Jaroslaw

2006-01-01

In the last 10-15 years there has been a significant effort toward development of new, more efficient and faster materials for detection of ionizing radiation. A growing demand for better scintillator crystals for detection of 511 keV gamma particles has been due mostly to recent advances in modern imaging systems employing positron emitting radionuclides for medical diagnostics in neurology, oncology and cardiology. While older imaging systems were almost exclusively based on BGO and NaI:Tl crystals the new systems, e.g., ECAT Accel, developed by Siemens/CTI, are based on recently discovered and developed LSO (Lu 2SiO 5:Ce, Ce-activated lutetium oxyorthosilicate) crystals. Interestingly, despite very good properties of LSO, there still is a strong drive toward development of new scintillator crystals that would show even better performance and characteristics. In this presentation we shall review spectroscopic and scintillator characterization of new complex oxide crystals, namely LSO, LYSO, YAG, LuAP (LuAlO 3, lutetium aluminate perovskite) and LuYAP activated with Ce and Pr. The LSO:Ce crystals have been grown by CTI Inc (USA), LYSO:Ce, LuAP:Ce and LuYAP:Ce crystals have been grown by Photonic Materials Ltd., Scotland (PML is the only company providing large LuAP:Ce crystals on a commercial scale), while YAG:Pr and LuAP:Pr crystals have been grown by Institute of Electronic Materials Technology (Poland). All these crystals have been characterized at Institute of Physics, N. Copernicus University (Poland). We will review and compare results of measurements of radioluminescence, VUV spectroscopy, scintillation light yields, scintillation time profiles and low temperature thermoluminescence performed on these crystals. We will demonstrate that all experiments clearly indicate that there is a significant room for improvement of LuAP, LuYAP and YAG. While both Ce-activated LSO and LYSO perform very well, we also note that LuYAP:Ce, LuAP:Ce and YAG:Pr offer some advantages and, after a likely improvement of some parameters, may also present a viable and desired alternative in applications that require high counting rates or better time resolution. Unfortunately, LuAP:Pr, although the fastest among all the materials studied, may be seriously limited in its achievable light yield by inherent physical processes that are responsible for nonradiative quenching of scintillation light in this material.

Friction and wear behavior of single-crystal silicon carbide in sliding contact with various metals

NASA Technical Reports Server (NTRS)

Miyoshi, K.; Buckley, D. H.

1978-01-01

Sliding friction experiments were conducted with single-crystal silicon carbide in contact with various metals. Results indicate the coefficient of friction is related to the relative chemical activity of the metals. The more active the metal, the higher the coefficient of friction. All the metals examined transferred to silicon carbide. The chemical activity of the metal and its shear modulus may play important roles in metal transfer, the form of the wear debris and the surface roughness of the metal wear scar. The more active the metal, and the less resistance to shear, the greater the transfer to silicon carbide and the rougher the wear scar on the surface of the metal. Hexagon shaped cracking and fracturing formed by cleavage of both prismatic and basal planes is observed on the silicon carbide surface.

Solution Growth and Characterization of Single Crystals on Earth and in Microgravity

NASA Technical Reports Server (NTRS)

Aggarwal, M. D.; Currie, J. R.; Penn, B. G.; Batra, A. K.; Lal, R. B.

2007-01-01

Crystal growth has been of interest to physicists and engineers for a long time because of their unique properties. Single crystals are utilized in such diverse applications as pharmaceuticals, computers, infrared detectors, frequency measurements, piezoelectric devices, a variety of high-technology devices, and sensors. Solution crystal growth is one of the important techniques to grow a variety of crystals when the material decomposes at the melting point and a suitable solvent is available to make a saturated solution at a desired temperature. In this Technical Memorandum (TM) an attempt is made to give the fundamentals of growing crystals from solution including improved designs of various crystallizers. Since the same solution crystal growth technique could not be used in microgravity, the authors proposed a new cooled-sting technique to grow crystals in space. The authors experience from conducting two Space Shuttle solution crystal growth experiments are also detailed in this TM and the complexity of solution growth experiments to grow crystals in space are also discussed. These happen to be some of the early experiments performed in space, and various lessons learned are described. A brief discussion of protein crystal growth that shares basic principles of the solution growth technique is given, along with some flight hardware information for growth in microgravity.

Growth and Characteristics of Bulk Single Crystals Grown from Solution on Earth and in Microgravity

NASA Technical Reports Server (NTRS)

Aggarwal, M. D.; Batra, A. K.; Lal, R. B.; Penn, Benjamin G.; Frazier, Donald O.

2011-01-01

The growth of crystals has been of interest to physicists and engineers for a long time because of their unique properties. Single crystals are utilized in such diverse applications as pharmaceuticals, computers, infrared detectors, frequency measurements, piezoelectric devices, a variety of high technology devices and sensors. Solution crystal growth is one of the important techniques to grow a variety of crystals when the material decomposes at the melting point and a suitable solvent is available to make a saturated solution at a desired temperature. In this chapter an attempt is made to give some fundamentals of growing crystals from solution including improved designs of various crystallizers. Since the same solution crystal growth technique could not be used in microgravity, authors had proposed a new cooled sting technique to grow crystals in space. Authors? experiences of conducting two space shuttle experiments relating to solution crystal growth are also detailed in this work. The complexity of these solution growth experiments to grow crystals in space are discussed. These happen to be some of the early experiments performed in space, and various lessons learned are described. A brief discussion of protein crystal growth that also shares basic principles of solution growth technique is given along with some flight hardware information for its growth in microgravity.

Follow up on the crystal growth experiments of the LDEF

NASA Technical Reports Server (NTRS)

Nielsen, K. F.; Lind, M. D.

1993-01-01

The results of the 4 solution growth experiments on the LDEF have been published elsewhere. Both the crystals of CaCO3, which were large and well shaped, and the much smaller TTF-TCNQ crystals showed unusual morphological behavior. The follow up on these experiments was begun in 1981, when ESA initiated a 'Concept Definition Study' on a large, 150 kg, Solution Growth Facility (SGF) to be included in the payload of EURECA-1, the European Retrievable Carrier. This carrier was a continuation of the European Spacelab and at that time planned for launch in 1987. The long delay of the LDEF retrieval and of subsequent missions brought about reflections both on the concept of crystal growth in space and on the choice of crystallization materials that had been made for the LDEF. Already before the LDEF retrieval, research on TTF-TCNQ had been stopped, and a planned growth experiment with TTF-TCNQ on the SGF/EURECA had been cancelled. The target of the SGF investigation is now more fundamental in nature. None of the crystals to be grown here are, like TTF-TCNQ, in particular demand by science or industry, and the crystals only serve the purpose of model crystals. The real purpose of the investigation is to study the growth behavior. One of the experiments, the Soret Coefficient Measurement experiment is not growing crystals at all, but has it as its sole purpose to obtain accurate information on thermal diffusion, a process of importance in crystal growth from solution.

Thermal and convection analyses of the dendrite remelting rocket experiment; Experiment 74-21 in the space processing rocket program

NASA Technical Reports Server (NTRS)

Grodzka, P. G.; Pond, J. E.; Spradley, J. W.; Johnson, M. H.

1976-01-01

The Dendrite Remelting Rocket Experiment was performed aboard a Black Brant VC Sounding Rocket during a period which gravity levels of approximately 0.00001 g prevailed. The experiment consisted of cooling an aqueous ammonium chloride solution in a manner such that crystallization of ammonium chloride crystals proceeded throughout a three minute period of zero-g. The crystallization process during flight was recorded on 35 mm panatomic-x film. A number of ground crystallizations were similarly recorded for comparison purposes. The convective and thermal conditions in aqueous and metallic liquid systems were assessed under conditions of the flight experiment to help establish the relevance of the rocket experiment to metals casting phenomena. The results indicate that aqueous or metallic convective velocities in the Dendrite Remelting Rocket Experiment cell are of insignificant magnitudes at the 0.0001 to 0.00001 g levels of the experiment. The crystallization phenomena observed in the Rocket Experiment, therefore, may be indicative of how metals will solidify in low-g.

Crystal Nucleation Using Surface-Energy-Modified Glass Substrates.

PubMed

Nordquist, Kyle A; Schaab, Kevin M; Sha, Jierui; Bond, Andrew H

2017-08-02

Systematic surface energy modifications to glass substrates can induce nucleation and improve crystallization outcomes for small molecule active pharmaceutical ingredients (APIs) and proteins. A comparatively broad probe for function is presented in which various APIs, proteins, organic solvents, aqueous media, surface energy motifs, crystallization methods, form factors, and flat and convex surface energy modifications were examined. Replicate studies ( n ≥ 6) have demonstrated an average reduction in crystallization onset times of 52(4)% (alternatively 52 ± 4%) for acetylsalicylic acid from 91% isopropyl alcohol using two very different techniques: bulk cooling to 0 °C using flat surface energy modifications or microdomain cooling to 4 °C from the interior of a glass capillary having convex surface energy modifications that were immersed in the solution. For thaumatin and bovine pancreatic trypsin, a 32(2)% reduction in crystallization onset times was demonstrated in vapor diffusion experiments ( n ≥ 15). Nucleation site arrays have been engineered onto form factors frequently used in crystallization screening, including microscope slides, vials, and 96- and 384-well high-throughput screening plates. Nucleation using surface energy modifications on the vessels that contain the solutes to be crystallized adds a layer of useful variables to crystallization studies without requiring significant changes to workflows or instrumentation.

Protein crystal growth results from the United States Microgravity Laboratory-1 mission

NASA Technical Reports Server (NTRS)

Delucas, Lawrence J.; Moore, K. M.; Vanderwoerd, M.; Bray, T. L.; Smith, C.; Carson, M.; Narayana, S. V. L.; Rosenblum, W. M.; Carter, D.; Clark, A. D, Jr.

1994-01-01

Protein crystal growth experiments have been performed by this laboratory on 18 Space Shuttle missions since April, 1985. In addition, a number of microgravity experiments also have been performed and reported by other investigators. These Space Shuttle missions have been used to grow crystals of a variety of proteins using vapor diffusion, liquid diffusion, and temperature-induced crystallization techniques. The United States Microgravity Laboratory - 1 mission (USML-1, June 25 - July 9, 1992) was a Spacelab mission dedicated to experiments involved in materials processing. New protein crystal growth hardware was developed to allow in orbit examination of initial crystal growth results, the knowledge from which was used on subsequent days to prepare new crystal growth experiments. In addition, new seeding hardware and techniques were tested as well as techniques that would prepare crystals for analysis by x-ray diffraction, a capability projected for the planned Space Station. Hardware that was specifically developed for the USML-1 mission will be discussed along with the experimental results from this mission.

Linking Plagioclase Zoning Patterns to Active Magma Processes

NASA Astrophysics Data System (ADS)

Izbekov, P. E.; Nicolaysen, K. P.; Neill, O. K.; Shcherbakov, V.; Plechov, P.; Eichelberger, J. C.

2015-12-01

Plagioclase, one of the most common and abundant mineral phases in volcanic products, will vary in composition in response to changes in temperature, pressure, composition of the ambient silicate melt, and melt H2O concentration. Changes in these parameters may cause dissolution or growth of plagioclase crystals, forming characteristic textural and compositional variations (zoning patterns), the complete core-to-rim sequence of which describes events experienced by an individual crystal from its nucleation to the last moments of its growth. Plagioclase crystals in a typical volcanic rock may look drastically dissimilar despite their spatial proximity and the fact that they have erupted together. Although they shared last moments of their growth during magma ascent and eruption, their prior experiences could be very different, as plagioclase crystals often come from different domains of the same magma system. Distinguishing similar zoning patterns, correlating them across the entire population of plagioclase crystals, and linking these patterns to specific perturbations in the magmatic system may provide additional perspective on the variety, extent, and timing of magma processes at active volcanic systems. Examples of magma processes, which may be distinguished based on plagioclase zoning patterns, include (1) cooling due to heat loss, (2) heating and/or pressure build up due to an input of new magmatic material, (3) pressure drop in response to magma system depressurization, and (4) crystal transfer between different magma domains/bodies. This review will include contrasting examples of zoning patters from recent eruptions of Karymsky, Bezymianny, and Tolbachik Volcanoes in Kamchatka, Augustine and Cleveland Volcanoes in Alaska, as well as from the drilling into an active magma body at Krafla, Iceland.

Maximizing Macromolecule Crystal Size for Neutron Diffraction Experiments

NASA Technical Reports Server (NTRS)

Judge, R. A.; Kephart, R.; Leardi, R.; Myles, D. A.; Snell, E. H.; vanderWoerd, M.; Curreri, Peter A. (Technical Monitor)

2002-01-01

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.

Experimental Demonstration of Isomorphism.

ERIC Educational Resources Information Center

Kamenicek, J.; Melicharek, M.

2000-01-01

Describes some simple experiments related to the properties of crystals. Illustrates isomorphism using single crystals of alum. Presents experiments for determining how various mixture compositions affect the growth of salt crystals. (WRM)

Apollo-Soyuz pamphlet no. 2: X-rays, gamma-rays. [experimental design

NASA Technical Reports Server (NTRS)

Page, L. W.; From, T. P.

1977-01-01

The nature of high energy radiation and its penetration through earth's atmosphere is examined with emphasis on X-rays, gamma rays, and cosmic radiation and the instruments used in their detection. The history of radio astronomy and the capabilities of the Uhuru satellite are summarized. The ASTP soft X-ray experiment (MA-048) designed to study the spectra in the range from 0.1 to 10 keV and survey the background over a large section of the sky is described, as well as the determination of SMC C-1 as an X-ray pulsar. The crystal activation experiment (MA-151) used to measure the radioactive isotopes created by cosmic rays in crystals used for gamma ray detectors is also discussed.

Protein crystal growth in microgravity

NASA Technical Reports Server (NTRS)

Rosenblum, William M.; Delucas, Lawrence J.; Wilson, William W.

1989-01-01

Major advances have been made in several of the experimental aspects of protein crystallography, leaving protein crystallization as one of the few remaining bottlenecks. As a result, it has become important that the science of protein crystal growth is better understood and that improved methods for protein crystallization are developed. Preliminary experiments with both small molecules and proteins indicate that microgravity may beneficially affect crystal growth. For this reason, a series of protein crystal growth experiments using the Space Shuttle was initiated. The preliminary space experiments were used to evolve prototype hardware that will form the basis for a more advanced system that can be used to evaluate effects of gravity on protein crystal growth. Various optical techniques are being utilized to monitor the crystal growth process from the incipient or nucleation stage and throughout the growth phase. The eventual goal of these studies is to develop a system which utilizes optical monitoring for dynamic control of the crystallization process.

Synthesis of gadolinium doped titanium(IV) oxide and their photocatalytic activity to decrease chemical oxygen demand (COD) value of water pollutants

NASA Astrophysics Data System (ADS)

Eddy, Diana Rakhmawaty; Dwiyanti, Dina; Rahayu, Iman; Hastiawan, Iwan; Bahti, Husein H.

2017-05-01

Pesticides are widely used for the control of plant disease. Unfortunately they are highly toxic to terraneous and aquatic life; this is a particular problem in agricultural areas. TiO2 is widely used for pesticide control because of its photocatalytic activity, but it still has inadequacy in its wide band gap. Alternatively, the wide band gap of TiO2 could be narrowed by modification with rare earth element such as gadolinium, so the photocatalytic activity of TiO2could be significantly enhanced. The purpose of this experiment is to synthesize Gd/TiO2 and its application to reduce COD of water pollutants such as carbosulfan pesticide. This experiment is done by doping gadolinium oxide into titanium tetra isopropoxide by sol-gel method. The crystal structure is characterized by using XRD, shown anatase successfully obtained with the smallest crystallite size is 37.655 nm, indicated optimum calcination time is 4 hours. SEM-EDX result shown morphology of crystal is big aggregates. Photocatalytic activity is tested to carbosulfan pesticide, obtained the COD percent decreases up to 87.88%.

STS-107 Flight Day 9 Highlights

NASA Technical Reports Server (NTRS)

2003-01-01

This video shows the activities of the STS-107 crew (Rick Husband, Commander; William McCool, Pilot; Kalpana Chawla, David Brown, Michael Anderson, Laurel Clark, Mission Specialists; Ilan Ramon, Payload Specialist) during flight day 9 of the Columbia orbiter's final flight. The primary activities of flight day 9 are spaceborne experiments. The video shows a commercial experiment on roses, a partial view of Africa from Libya to the Horn of Africa through the MEIDEX (Mediterranean Israeli Dust Experiment), and the FAST (Facility for Absorption and Surface Tension) experiment. The STARS (Space Technology and Research Students) international student experiments are shown. The preliminary results of these experiments on the effects of microgravity on silkworms, spiders, crystal growth, fish embryos, carpenter bees, and ants are discussed. The video includes a view of southern Spain and the Mediterranean Sea.

Operation condition for continuous anti-solvent crystallization of CBZ-SAC cocrystal considering deposition risk of undesired crystals

NASA Astrophysics Data System (ADS)

Nishimaru, Momoko; Nakasa, Miku; Kudo, Shoji; Takiyama, Hiroshi

2017-07-01

Crystallization operation of cocrystal production has deposition risk of undesired crystals. Simultaneously, continuous manufacturing processes are focused on. In this study, conditions for continuous cocrystallization considering risk reduction of undesired crystals deposition were investigated on the view point of thermodynamics and kinetics. The anti-solvent cocrystallization was carried out in four-component system of carbamazepine, saccharin, methanol and water. From the preliminary batch experiment, the relationships among undesired crystal deposition, solution composition decided by mixing ratio of solutions, and residence time for the crystals were considered, and then the conditions of continuous experiment were decided. Under these conditions, the continuous experiment was carried out. The XRD patterns of obtained crystals in the continuous experiment showed that desired cocrystals were obtained without undesired crystals. This experimental result was evaluated by using multi-component phase diagrams from the view point of the operation point's movement. From the evaluation, it was found that there is a certain operation condition which the operation point is fixed with time in the specific domain without the deposition risk of undesired single component crystals. It means the possibility of continuous production of cocrystals without deposition risk of undesired crystals was confirmed by using multi-component phase diagrams.

Formation of co-crystals: Kinetic and thermodynamic aspects

NASA Astrophysics Data System (ADS)

Gagnière, E.; Mangin, D.; Puel, F.; Rivoire, A.; Monnier, O.; Garcia, E.; Klein, J. P.

2009-04-01

Co-crystallisation is a recent method of great interest for the pharmaceutical industry, since pharmaceutical co-crystals represent useful materials for drug products. In this study, an active pharmaceutical ingredient (carbamazepine (CBZ)) co-crystallized with a vitamin (nicotinamide (NCT)) was chosen as a model substance. This work was focused on the construction of a phase diagram for the system CBZ/NCT, split in six domains for kinetic reasons (the different solid phases which might appear during the crystallisation) and in four domains according to thermodynamic aspects (the stable final phase obtained). Although co-crystals are not ionic compounds, the supersaturation of co-crystals can be evaluated by considering the solubility product. Batch crystallisation operations were carried out in a stirred vessel equipped with an in situ video probe. This latter device was a powerful analysis tool to monitor the CBZ/NCT co-crystals and single CBZ crystals since these two crystalline phases grown in ethanol exhibited needle and platelet habits. As concerns kinetics, the different solid phases which might appear during the experiments were observed and competed against each others. In accordance with thermodynamics, the stable solid form was obtained at the end of the operation. Finally some preliminary results indicate that the nucleation of co-crystals may be favoured by the presence of CBZ crystals. Epitaxial relationships between CBZ/NCT co-crystals and CBZ crystals were suspected.

The role of mass transport in protein crystallization.

PubMed

García-Ruiz, Juan Manuel; Otálora, Fermín; García-Caballero, Alfonso

2016-02-01

Mass transport takes place within the mesoscopic to macroscopic scale range and plays a key role in crystal growth that may affect the result of the crystallization experiment. The influence of mass transport is different depending on the crystallization technique employed, essentially because each technique reaches supersaturation in its own unique way. In the case of batch experiments, there are some complex phenomena that take place at the interface between solutions upon mixing. These transport instabilities may drastically affect the reproducibility of crystallization experiments, and different outcomes may be obtained depending on whether or not the drop is homogenized. In diffusion experiments with aqueous solutions, evaporation leads to fascinating transport phenomena. When a drop starts to evaporate, there is an increase in concentration near the interface between the drop and the air until a nucleation event eventually takes place. Upon growth, the weight of the floating crystal overcomes the surface tension and the crystal falls to the bottom of the drop. The very growth of the crystal then triggers convective flow and inhomogeneities in supersaturation values in the drop owing to buoyancy of the lighter concentration-depleted solution surrounding the crystal. Finally, the counter-diffusion technique works if, and only if, diffusive mass transport is assured. The technique relies on the propagation of a supersaturation wave that moves across the elongated protein chamber and is the result of the coupling of reaction (crystallization) and diffusion. The goal of this review is to convince protein crystal growers that in spite of the small volume of the typical protein crystallization setup, transport plays a key role in the crystal quality, size and phase in both screening and optimization experiments.

Shock and Microstructural Characterization of the α-ω Phase Transition in Titanium Crystals

NASA Astrophysics Data System (ADS)

Morrow, Benjamin M.; Rigg, Paulo A.; Jones, David R.; Addessio, Francis L.; Trujillo, Carl P.; Saavedra, Ramon A.; Martinez, Daniel T.; Cerreta, Ellen K.

2017-12-01

A multicrystal comprised of a small number of large crystals of high-purity titanium and a [0001] oriented high-purity single crystal titanium sample were shock loaded using gas gun plate impact experiments. Tests were performed at stresses above the α {-}ω phase transition stress (for high-purity polycrystalline specimens) to observe the behavior of oriented crystals under similar conditions. Post-mortem characterization of the shocked microstructure was conducted on the single crystal sample to measure textures, and quantify phases and twinning. The apparent activation of plastic and transformation mechanisms was dependent upon crystal orientation. Specifically, the [0001] crystal showed a higher Hugoniot elastic limit than the [10\\bar{1}0] or [3\\bar{1}\\bar{4}4] orientations. The slope of velocity as a function of time was lower in the [0001] orientation than the other orientations during plastic deformation, indicating sluggish transformation kinetics for the α to ω phase transition for the [0001] oriented crystal. Microtexture measurements of a recovered [0001] oriented single crystal revealed the presence of retained ω phase after unloading, with orientations of the constituent phase fractions indicative of the forward α → ω transition, rather than the reverse ω → α transition, suggesting that the material never achieved a state of 100% ω phase.

The Biological Macromolecule Crystallization Database and NASA Protein Crystal Growth Archive

PubMed Central

Gilliland, Gary L.; Tung, Michael; Ladner, Jane

1996-01-01

The NIST/NASA/CARB Biological Macromolecule Crystallization Database (BMCD), NIST Standard Reference Database 21, contains crystal data and crystallization conditions for biological macromolecules. The database entries include data abstracted from published crystallographic reports. Each entry consists of information describing the biological macromolecule crystallized and crystal data and the crystallization conditions for each crystal form. The BMCD serves as the NASA Protein Crystal Growth Archive in that it contains protocols and results of crystallization experiments undertaken in microgravity (space). These database entries report the results, whether successful or not, from NASA-sponsored protein crystal growth experiments in microgravity and from microgravity crystallization studies sponsored by other international organizations. The BMCD was designed as a tool to assist x-ray crystallographers in the development of protocols to crystallize biological macromolecules, those that have previously been crystallized, and those that have not been crystallized. PMID:11542472

Synchronization of pairs of nanosecond pulses from a laser with two gain crystals pumped with two different sources.

PubMed

Staufert, Daniel; Cudney, Roger S

2018-05-10

We report a laser that emits two Q-switched pulses, one at 1.047 μm and the other at 1.064 μm, generated by a Nd:YLF and a Nd:YVO 4 , respectively. The crystals are pumped by two fiber-coupled diode lasers (808 nm and 880 nm); the delay between the pulses can be controlled by adjusting the power of the pumps. Two kinds of Q-switching techniques are reported, passive (Cr:YAG saturable absorber) and active (electro-optic modulator). We model both the active and passive Q switching and make a comparison between numerical simulations and experiments. We show experimentally and theoretically that in both cases the pulses can be synchronized; however, the stability of the synchronization (sensitivity to pump power fluctuations) is better for active than for passive Q switching. We also report that under certain experimental conditions a third wavelength is obtained, 1156 nm, which corresponds to the first Stokes shift of the 1047 nm pulse produced by stimulated Raman scattering from the Nd:YVO 4 crystal.

Liquid crystal mediated active nano-plasmonic based on the formation of hybrid plasmonic-photonic modes

NASA Astrophysics Data System (ADS)

Mehrzad, Hossein; Mohajerani, Ezeddin

2018-02-01

The present study aims to demonstrate how active hybrid nano-plasmonic modes become excited due to the coupling of localized plasmonic resonance and Fabry-Perot (FP) optical modes. The proposed structure includes an integration of a micro-cavity filled with liquid crystals with high anisotropy and a layer of gold nanoislands (NIs). The optical absorption of NI is controllably discretized to the narrow-width modes, called "hybrid modes (HM)," due to the interplay between FP and plasmonic modes. HM could demonstrate a strongly intensified and diminished absorption, compared to the absorption of the bare gold layer. Based on the active plasmonic experiments, the HM boosted the figure of merit related to activation capability up to 40 times and subsequently experienced impressive spectral shifts, leading to very wavelength-selective changes. The theoretical simulation of the HM is provided to suggest relevant insights into the experimental results.

Three-Dimensional Stress Fields and Slip Systems for Single Crystal Superalloy Notched Specimens

NASA Technical Reports Server (NTRS)

Magnan, Shannon M.; Throckmorton, David (Technical Monitor)

2002-01-01

Single crystal superalloys have become increasingly popular for turbine blade and vane applications due to their high strength, and creep and fatigue resistance at elevated temperatures. The crystallographic orientation of a single crystal material greatly affects its material properties, including elastic modulus, shear modulus, and ductility. These directional properties, along with the type of loading and temperature, dictate an anisotropic response in the yield strength, creep resistance, creep rupture ductility, fatigue resistance, etc. A significant amount of research has been conducted to determine the material properties in the <001> orientation, yet the material properties deviating from the <001> orientation have not been assessed for all cases. Based on the desired application and design criteria, a crystal orientation is selected to yield the maximum properties. Currently, single crystal manufacturing is able to control the primary crystallographic orientation within 15 of the target orientation, which is an acceptable deviation to meet both performance and cost guidelines; the secondary orientation is rarely specified. A common experiment is the standard load-controlled tensile test, in which specimens with different orientations can be loaded to observe the material response. The deformation behavior of single-crystal materials under tension and compression is known to be a function of not only material orientation, but also of varying microdeformation (i.e. dislocation) mechanisms. The underlying dislocation motion causes deformation via slip, and affects the activation of specific slip systems based on load and orientation. The slip can be analyzed by observing the visible traces left on the surface of the specimen from the slip activity within the single crystal material. The goal of this thesis was to predict the slip systems activated in three-dimensional stress fields of a notched tensile specimen, as a function of crystal orientation, using finite element analysis without addressing microstructural deformation mechanisms that govern their activation. Out of three orientations tested, the specimen with a [110] load orientation and a [001] growth direction had the lowest maximum resolved shear stress; this specimen orientation appears to be the best design candidate for a tensile application.

Crystal Growth and Scintillation Properties of Eu2+ doped Cs4CaI6 and Cs4SrI6

NASA Astrophysics Data System (ADS)

Stand, L.; Zhuravleva, M.; Chakoumakos, B.; Johnson, J.; Loyd, M.; Wu, Y.; Koschan, M.; Melcher, C. L.

2018-03-01

In this work we present the crystal growth and scintillation properties of two new ternarymetal halide scintillators activated with divalent europium, Cs4CaI6 and Cs4SrI6. Single crystals of each compound were grown in evacuated quartz ampoules via the vertical Bridgman technique using a two-zone transparent furnace. Single crystal X-ray diffraction experiments showed that both crystals have a trigonal (R-3c) structure, with a density of 3.99 g/cm3 and 4.03 g/cm3. The radioluminescence and photoluminescence measurements showed typical luminescence properties due to the 5d-4f radiative transitions in Eu2+. At this early stage of development Cs4SrI6:Eu and Cs4CaI6:Eu have shown very promising scintillation properties, with light yields and energy resolutions of 62,300 ph/MeV and 3.3%, and 51,800 photons/MeV and 3.6% at 662 keV, respectively.

Comparative in vitro studies on disodium EDTA effect with and without Proteus mirabilis on the crystallization of carbonate apatite and struvite

NASA Astrophysics Data System (ADS)

Prywer, Jolanta; Olszynski, Marcin; Torzewska, Agnieszka; Mielniczek-Brzóska, Ewa

2014-06-01

Effect of disodium EDTA (salt of ethylenediamine tetraacetic acid) on the crystallization of struvite and carbonate apatite was studied. To evaluate such an effect we performed an experiment of struvite and carbonate apatite growth from artificial urine. The crystallization process was induced by Proteus mirabilis to mimic the real urinary tract infection, which usually leads to urinary stone formation. The results demonstrate that disodium EDTA exhibits the effect against P. mirabilis retarding the activity of urease - an enzyme produced by these microorganisms. The spectrophotometric results demonstrate that, with and without P. mirabilis, the addition of disodium EDTA increases the induction time and decreases the growth efficiency compared to the baseline (without disodium EDTA). These results are discussed from the standpoint of speciation of complexes formed in the solution of artificial urine in the presence of disodium EDTA. The size of struvite crystals was found to decrease in the presence of disodium EDTA. However, struvite crystals are larger in the presence of bacteria while the crystal morphology and habit remain unchanged.

Comparative Analysis of Thaumatin Crystals Grown on Earth and in Microgravity. Experiment 23

NASA Technical Reports Server (NTRS)

Ng, Joseph D.; Lorber, Bernard; Giege, Richard; Koszelak, Stanley; Day, John; Greenwood, Aaron; McPherson, Alexander

1998-01-01

The protein thaumatin was studied as a model macromolecule for crystallization in microgravity environment experiments conducted on two U.S. Space Shuttle missions (second United States Microgravity Laboratory (USML-2) and Life and Microgravity Spacelab (LMS)). In this investigation we evaluated and compared the quality of space- and Earth-grown thaumatin crystals using x-ray diffraction analysis and characterized them according to crystal size, diffraction resolution limit, and mosaicity. Two different approaches for growing thaumatin crystals in the microgravity environment, dialysis and liquid-liquid diffusion, were employed as a joint experiment by our two investigative teams. Thaumatin crystals grown under a microgravity environment were generally larger in volume with fewer total crystals. They diffracted to significantly higher resolution and with improved diffraction properties as judged by relative Wilson plots. The mosaicity for space-grown crystals was significantly less than for those grown on Earth. Increasing concentrations of protein in the crystallization chambers under microgravity lead to larger crystals. The data presented here lend further support to the idea that protein crystals of improved quality can be obtained in a microgravity environment.

Crystal Growth Furnace - An overview of the system configuration and planned experiments on the First United States Microgravity Laboratory mission

NASA Technical Reports Server (NTRS)

Srinivas, R.; Schaefer, D. A.

1992-01-01

The Crystal Growth Furnace (CGF) system configuration for the First United States Microgravity Laboratory (USML-1) mission is reviewed, and the planned on-orbit experiments are briefly described. The CGF is configured to accommodate four scientific experiments involving crystal growth which are based on the classical Bridgman method and CVT method, including vapor transport crystal growth of mercury cadmium telluride; crystal growth of mercury zinc telluride by directional solidification; seeded Bridgman growth of zinc-doped cadmium telluride; and Bridgman growth of selenium-doped gallium arsenide.

Protein-crystal growth experiment (planned)

NASA Technical Reports Server (NTRS)

Fujita, S.; Asano, K.; Hashitani, T.; Kitakohji, T.; Nemoto, H.; Kitamura, S.

1988-01-01

To evaluate the effectiveness of a microgravity environment on protein crystal growth, a system was developed using 5 cubic feet Get Away Special payload canister. In the experiment, protein (myoglobin) will be simultaneously crystallized from an aqueous solution in 16 crystallization units using three types of crystallization methods, i.e., batch, vapor diffusion, and free interface diffusion. Each unit has two compartments: one for the protein solution and the other for the ammonium sulfate solution. Compartments are separated by thick acrylic or thin stainless steel plates. Crystallization will be started by sliding out the plates, then will be periodically recorded up to 120 hours by a still camera. The temperature will be passively controlled by a phase transition thermal storage component and recorded in IC memory throughout the experiment. Microgravity environment can then be evaluated for protein crystal growth by comparing crystallization in space with that on Earth.

Scintillation light detectors with Neganov Luke amplification

NASA Astrophysics Data System (ADS)

Isaila, C.; Boslau, O.; Coppi, C.; Feilitzsch, F. v.; Goldstraß, P.; Jagemann, T.; Jochum, J.; Kemmer, J.; Lachenmaier, T.; Lanfranchi, J.-C.; Pahlke, A.; Potzel, W.; Rau, W.; Stark, M.; Wernicke, D.; Westphal, W.

2006-04-01

For an active suppression of the gamma and electron background in the Cryogenic Rare Event Search with Superconducting Thermometers (CRESST) dark matter experiment both phonons and scintillation light generated in a CaWO 4 crystal are detected simultaneously. The phonon signal is read out by a transition edge sensor (TES) on the CaWO 4 crystal. For light detection a silicon absorber equipped with a TES is employed. An efficient background discrimination requires very sensitive light detectors. The threshold can be improved by applying an electric field to the silicon crystal leading to an amplification of the thermal signal due to the Neganov-Luke effect. Measurements showing the improved sensitivity of the light detectors as well as future steps for reducing the observed extra noise will be presented.

Results of the TTF-TCNQ- and the calcium carbonate-crystallization on the Long Duration Exposure Facility

NASA Technical Reports Server (NTRS)

Nielsen, Kjeld Flemming; Lind, M. David

1991-01-01

Experiment AO139A on the Long Duration Exposure Facility (LDEF) carried four large containers into orbit for five years with crystal growth solutions for lead sulfide, calcium carbonate, and tetra thiafulvalene- tetra cyanoquino methane (TTF-TCNQ). The LDEF was in excellent condition after the long orbital stay, and although the temperature data was lost, the experiment program had been working since the valves in all containers were opened. All four experiments produced crystals; however, they were of varying quality. The calcium carbonate crystals had the best appearance. The TTF-TCNQ crystals were packed together near the valve openings of the container. When taken apart, the single crystals showed some unusual morphological properties. X-ray investigations as well as conductivity measurements on the long duration space grown TTF-TCNQ crystals are presented, and pictures of the calcium carbonate are shown. Comparisons are made with previous space solution growth experiments on the European Spacelab Mission and the Apollo-Soyuz Test Project.

Trends in the precipitation and crystallization behavior of supersaturated aqueous solutions of poorly water-soluble drugs assessed using synchrotron radiation.

PubMed

Raina, Shweta A; Van Eerdenbrugh, Bernard; Alonzo, David E; Mo, Huaping; Zhang, Geoff G Z; Gao, Yi; Taylor, Lynne S

2015-06-01

Amorphous materials are high-energy solids that can potentially enhance the bioavailability of poorly soluble compounds. A major impediment to their widespread use as a formulation platform is the tendency of amorphous materials to crystallize. The aim of this study was to evaluate the relative crystallization tendency of six structural analogues belonging to the dihydropyridine class, in an aqueous environment in the absence and presence of polymers, using wide-angle X-ray scattering synchrotron radiation and polarized light microscopy. The crystallization behavior of precipitates generated from supersaturated solutions of the active pharmaceutical ingredients was found to be highly variable ranging from immediate to several hours in the absence of polymers. Polymers with intermediate hydrophilicity/hydrophobicity were found to substantially delay crystallization, whereas strongly hydrophilic or hydrophobic polymers were largely ineffective. Nuclear magnetic resonance spectroscopy experiments supported the supposition that polymers need to have affinity for both the drug-rich precipitate and the aqueous phase in order to be effective crystallization inhibitors. This study highlights the variability in the crystallization tendency of different compounds and provides insight into the mechanism of inhibition by polymeric additives. © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Amino Acid-Assisted Incorporation of Dye Molecules within Calcite Crystals.

PubMed

Marzec, Bartosz; Green, David C; Holden, Mark A; Coté, Alexander S; Ihli, Johannes; Khalid, Saba; Kulak, Alexander; Walker, Daniel; Tang, Chiu; Duffy, Dorothy M; Kim, Yi-Yeoun; Meldrum, Fiona C

2018-05-23

Biomineralisation processes invariably occur in the presence of multiple organic additives, which act in combination to give exceptional control over structures and properties. However, few synthetic studies have investigated the cooperative effects of soluble additives. This work addresses this challenge and focuses on the combined effects of amino acids and coloured dye molecules. The experiments demonstrate that strongly coloured calcite crystals only form in the presence of Brilliant Blue R (BBR) and four of the seventeen soluble amino acids, as compared with almost colourless crystals using the dye alone. The active amino acids are identified as those which themselves effectively occlude in calcite, suggesting a mechanism where they can act as chaperones for individual molecules or even aggregates of dyes molecules. These results provide new insight into crystal-additive interactions and suggest a novel strategy for generating materials with target properties. © 2018 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Flux synthesis of regular Bi4TaO8Cl square nanoplates exhibiting dominant exposure surfaces of {001} crystal facets for photocatalytic reduction of CO2 to methane.

PubMed

Li, Liang; Han, Qiutong; Tang, Lanqin; Zhang, Yuan; Li, Ping; Zhou, Yong; Zou, Zhigang

2018-01-25

Herein, orthorhombic regular Bi 4 TaO 8 Cl square nanoplates with an edge length of about 500 nm and a thickness of about 100 nm were successfully synthesized using a facile molten salt route. The as-prepared square nanoplates have been proven to be of {001} crystal facets as two dominantly exposed surfaces. The density functional theory calculation and photo-deposition of noble metal experiment demonstrate the electron and hole separation on different crystal facets and reveal that {001} crystal facets are in favor of the reduction reaction. Since the square nanoplate structure exhibits dominant exposure surfaces of the {001} facets, the molten salt route-based samples basically possess an obviously higher photocatalytic activity than those prepared by the solid state reaction (SSR) method. This study may provide inspiration for fabricating efficient photocatalysts.

KENNEDY SPACE CENTER, FLA. - The crystals visible in this laboratory dish were part of an experiment carried on mission STS-107. Several experiments were found during the search for Columbia debris. Included in the Commercial ITA Biomedical Experiments payload on mission STS-107 are urokinase cancer research, microencapsulation of drugs, the Growth of Bacterial Biofilm on Surfaces during Spaceflight (GOBBSS), and tin crystal formation.

NASA Image and Video Library

2003-05-07

KENNEDY SPACE CENTER, FLA. - The crystals visible in this laboratory dish were part of an experiment carried on mission STS-107. Several experiments were found during the search for Columbia debris. Included in the Commercial ITA Biomedical Experiments payload on mission STS-107 are urokinase cancer research, microencapsulation of drugs, the Growth of Bacterial Biofilm on Surfaces during Spaceflight (GOBBSS), and tin crystal formation.

Fluid Physics and Macromolecular Crystal Growth in Microgravity

NASA Technical Reports Server (NTRS)

Helliwell, John R.; Snell, Edward H.; Chayen, Naomi E.; Judge, Russell A.; Boggon, Titus J.; Pusey, M. L.; Rose, M. Franklin (Technical Monitor)

2000-01-01

The first protein crystallization experiment in microgravity was launched in April, 1981 and used Germany's Technologische Experimente unter Schwerelosigkeit (TEXUS 3) sounding rocket. The protein P-galactosidase (molecular weight 465Kda) was chosen as the sample with a liquid-liquid diffusion growth method. A sliding device brought the protein, buffer and salt solution into contact when microgravity was reached. The sounding rocket gave six minutes of microgravity time with a cine camera and schlieren optics used to monitor the experiment, a single growth cell. In microgravity a strictly laminar diffusion process was observed in contrast to the turbulent convection seen on the ground. Several single crystals, approx 100micron in length, were formed in the flight which were of inferior but of comparable visual quality to those grown on the ground over several days. A second experiment using the same protocol but with solutions cooled to -8C (kept liquid with glycerol antifreeze) again showed laminar diffusion. The science of macromolecular structural crystallography involves crystallization of the macromolecule followed by use of the crystal for X-ray diffraction experiments to determine the three dimensional structure of the macromolecule. Neutron protein crystallography is employed for elucidation of H/D exchange and for improved definition of the bound solvent (D20). The structural information enables an understanding of how the molecule functions with important potential for rational drug design, improved efficiency of industrial enzymes and agricultural chemical development. The removal of turbulent convection and sedimentation in microgravity, and the assumption that higher quality crystals will be produced, has given rise to the growing number of crystallization experiments now flown. Many experiments can be flown in a small volume with simple, largely automated, equipment - an ideal combination for a microgravity experiment. The term "protein crystal growth" is often historically used to describe these microgravity experiments. This is somewhat inaccurate as the field involves the study of many varied biological molecules including viruses, proteins, DNA, RNA and complexes of those structures. For this reason we use the term macromolecular crystal growth. In this chapter we review a series of diagnostic microgravity crystal growth experiments carried out principally using the European Space Agency (ESA) Advanced Protein Crystallization Facility (APCF). We also review related research, both experimental and theoretical, on the aspects of microgravity fluid physics that affect microgravity protein crystal growth. Our experiments have revealed some surprises that were not initially expected. We discuss them here in the context of practical lessons learnt and how to maximize the limited microgravity opportunities available.

Decades of Data: Extracting Trends from Microgravity Crystallization History

NASA Technical Reports Server (NTRS)

Judge, Russell A.; Snell, Edward H.; Kephart, Richard; vanderWoerd, Mark; Curreri, Peter A. (Technical Monitor)

2002-01-01

The reduced acceleration environment of an orbiting spacecraft has been posited as an ideal environment for biological crystal growth since buoyancy driven convection and sedimentation are greatly reduced. Since the first sounding rocket flight in 1981 many crystallization experiments have flown with some showing improvement and others not. To further explore macromolecule crystal improvement in microgravity we have accumulated data from published reports and reports submitted by individual investigators to NASA, forming a database called BIOSEArCH (Biological Space Experiment Archive of Crystallization History). To date it contains information from 63 missions including, the Space Shuttle program, unmanned satellites, the Russian Space Station MIR and sounding rocket experiments, containing reports for more than 736 macromolecule experiments. While it is not at this point in time a comprehensive record of all flight crystallization experimental results, there is however sufficient information for emerging trends to be identified. These trends will be highlighted.

Friction and wear of single-crystal manganese-zinc ferrite

NASA Technical Reports Server (NTRS)

Miyoshi, K.; Buckley, D. H.

1979-01-01

Sliding friction experiments were conducted with single crystal manganese-zinc ferrite in contact with itself and with transition metals. Results indicate mating highest atomic density directions (110) on matched crystallographic planes exhibit the lowest coefficient of friction, indicating that direction is important in the friction behavior of ferrite. Matched parallel high atomic density planes and crystallographic directions at the interface exhibit low coefficients of friction. The coefficients of friction for ferrite in contact with various metals are related to the relative chemical activity of these metals. The more active the metal, the higher the coefficient of friction. Cracking and the formation of hexagon- and rectangular-shaped platelet wear debris due to cleavages of (110) planes are observed on the ferrite surfaces as a result of sliding.

Kinetic Study of Adsorption Processes in Solution: An Undergraduate Physical Chemistry Experiment.

ERIC Educational Resources Information Center

Casado, Julio; And Others

1985-01-01

Background information, apparatus needed, procedures used, and results obtained are provided for a simple kinetic method for the monitoring of adsorption processes. The method, which involved adsorption of crystal violet onto activated carbon, is suitable for classroom and/or research purposes. (JN)

Linking Plagioclase Zoning Patterns to Active Magma Processes

NASA Astrophysics Data System (ADS)

Izbekov, P. E.; Nicolaysen, K. P.; Neill, O. K.; Shcherbakov, V.; Eichelberger, J. C.; Plechov, P.

2016-12-01

Plagioclase, one of the most common and abundant mineral phases in volcanic products, will vary in composition in response to changes in temperature, pressure, composition of the ambient silicate melt, and melt H2O concentration. Changes in these parameters may cause dissolution or growth of plagioclase crystals, forming characteristic textural and compositional variations (zoning patterns), the complete core-to-rim sequence of which describes events experienced by an individual crystal from its nucleation to the last moments of its growth. Plagioclase crystals in a typical volcanic rock may look drastically dissimilar despite their spatial proximity and the fact that they have erupted together. Although they shared last moments of their growth during magma ascent and eruption, their prior experiences could be very different, as plagioclase crystals often come from different domains of the same magma system. Distinguishing similar zoning patterns, correlating them across the entire population of plagioclase crystals, and linking these patterns to specific perturbations in the magmatic system may provide additional perspective on the variety, extent, and timing of magma processes at active volcanic systems. Examples of magma processes, which may be distinguished based on plagioclase zoning patterns, include (1) cooling due to heat loss, (2) heating and/or pressure build up due to an input of new magmatic material, (3) pressure drop in response to magma system depressurization, and (4) crystal transfer between different magma domains/bodies. This review will include contrasting examples of zoning patters from recent eruptions of Augustine and Cleveland Volcanoes in Alaska, Sakurajima Volcano in Japan, Karymsky, Bezymianny, and Tolbachik Volcanoes in Kamchatka, as well as from the drilling into an active magma body at Krafla, Iceland.

Biosygnatures on olivines in search of past life on Mars

NASA Astrophysics Data System (ADS)

Jakus, Natalia; Manecki, Maciej; Faehnrich, Karol; Młynarska, Maria; Słupski, Paweł

2017-04-01

Biosignatures indicate past and present activity of living organisms. Only inorganic biosignatures, e.g. results of interactions between the minerals and the microorganisms in Martian soils could resist harsh environmental conditions on Mars. However, it may be difficult to distinguish the traces of the organism activities from the effects of "natural" chemical and physical processes. In this study, an acidiophilic, chemoautotrophic, iron-oxidizing bacteria Acidithiobacillus ferrooxidans were incubated with magnesium-iron silicate (olivine) crystals to identify the potential development of biogenic textures on the surface. The Mg-rich olivines were separated from the gabbro rock (Trodos, Cyprus). The isometric crystals were up to 2 mm in size. All the grains were cleaned in ultrasonic bath and fixed on the epoxy stubs. This enabled the observation of the very same surfaces before and after the experiments allowing inspection of natural etch pits and weathering patterns present before inoculation as well as the forms resulting from the experiments. The stubs with the olivines were sterilized with ethanol prior to the experiments. Bacteria were isolated from old pyrite mine in Klucze near Olkusz (Southern Poland). A liquid media K9 was used through the experiments (Silverman and Ludgren, 1959). The experiments were run in triplicates. Olivine grains were placed in the inoculated medium and incubated for 7 days at 28 C. An abiotic experiment was run as control. Additionally, the experiments in modified (iron deficient) medium were designed to stimulate potential active scavenging for Fe by bacteria-mediated dissolution. In the Fe-deficient medium, the negligible amount of iron was present only to initiate the bacteria growth: the only source of Fe was the olivine grain throughout the experiment. After 7 days of incubation the olivine grains were removed and air-dried. The alterations of the crystals by both, purely inorganic and biologically mediated dissolution were investigated with the use of scanning electron microscopy (SEM) with EDS microanalyzer. Any alteration of mineral surface resulting from mineral-microbes interaction was considered as a biosignature. In the standard Fe-rich K9 medium, occasional precipitation of the sulfate phase was observed. There is no evidence for the microbial control on this process. Formation of etch pits was observed in both, Fe-rich and Fe-deficient experiments, in the presence and in the absence of bacteria. The dissolution patterns were indistinguishable. Therefore, the experiments resulting in formation of the biofilm will be designed in future. SILVERMAN M.P., LUNDGREN D.G., 1959. Studies on the chemoautotrophic iron bacterium Ferrobacillus ferrooxidans. An improved medium and a harvesting procedure for securing high cell yields.

Investigation of crystal growth in zero gravity environment and investigation of metallic whiskers

NASA Technical Reports Server (NTRS)

Davis, J. H.; Lal, R. B.; Walter, H. U.; Castle, J. G., Jr.

1972-01-01

Theoretical and experimental work reported relates to the effects of near-zero gravity on growths of crystals and metallic whiskers during Skylab and Apollo flight experiments. Studies on growth and characterization of candidate materials for flight experiments cover indium-bismuth compounds, bismuth single crystals, gallium arsenide films and single crystals, and cadmium whiskers.

Preparative Protein Production from Inclusion Bodies and Crystallization: A Seven-Week Biochemistry Sequence

PubMed Central

Peterson, Megan J.; Snyder, W. Kalani; Westerman, Shelley; McFarland, Benjamin J.

2011-01-01

We describe how to produce and purify proteins from E. coli inclusion bodies by adapting versatile, preparative-scale techniques to the undergraduate laboratory schedule. This seven-week sequence of experiments fits into an annual cycle of research activity in biochemistry courses. Recombinant proteins are expressed as inclusion bodies, which are collected, washed, then solubilized in urea. Stepwise dialysis to dilute urea over the course of a week produces refolded protein. Column chromatography is used to purify protein into fractions, which are then analyzed with gel electrophoresis and concentration assays. Students culminate the project by designing crystallization trials in sitting-drop trays. Student evaluation of the experience has been positive, listing 5–12 new techniques learned, which are transferrable to graduate research in academia and industry. PMID:21691428

First array of enriched Zn$$^{82}$$Se bolometers to search for double beta decay

DOE PAGES

Artusa, D. R.; Balzoni, A.; Beeman, J. W.; ...

2016-07-01

The R&D activity performed during the last years proved the potential of ZnSe scintillating bolometers to the search for neutrino-less double beta decay, motivating the realization of the first large-mass experiment based on this technology: CUPID-0. The isotopic enrichment in 82Se, the Zn 82Se crystals growth, as well as the light detectors production have been accomplished, and the experiment is now in construction at Laboratori Nazionali del Gran Sasso (Italy). In this paper we present the results obtained testing the first three Zn 82Se crystals operated as scintillating bolometers, and we prove that their performance in terms of energy resolution,more » background rejection capability and intrinsic radio-purity complies with the requirements of CUPID-o.« less

Automation in biological crystallization.

PubMed

Stewart, Patrick Shaw; Mueller-Dieckmann, Jochen

2014-06-01

Crystallization remains the bottleneck in the crystallographic process leading from a gene to a three-dimensional model of the encoded protein or RNA. Automation of the individual steps of a crystallization experiment, from the preparation of crystallization cocktails for initial or optimization screens to the imaging of the experiments, has been the response to address this issue. Today, large high-throughput crystallization facilities, many of them open to the general user community, are capable of setting up thousands of crystallization trials per day. It is thus possible to test multiple constructs of each target for their ability to form crystals on a production-line basis. This has improved success rates and made crystallization much more convenient. High-throughput crystallization, however, cannot relieve users of the task of producing samples of high quality. Moreover, the time gained from eliminating manual preparations must now be invested in the careful evaluation of the increased number of experiments. The latter requires a sophisticated data and laboratory information-management system. A review of the current state of automation at the individual steps of crystallization with specific attention to the automation of optimization is given.

Automation in biological crystallization

PubMed Central

Shaw Stewart, Patrick; Mueller-Dieckmann, Jochen

2014-01-01

Crystallization remains the bottleneck in the crystallographic process leading from a gene to a three-dimensional model of the encoded protein or RNA. Automation of the individual steps of a crystallization experiment, from the preparation of crystallization cocktails for initial or optimization screens to the imaging of the experiments, has been the response to address this issue. Today, large high-throughput crystallization facilities, many of them open to the general user community, are capable of setting up thousands of crystallization trials per day. It is thus possible to test multiple constructs of each target for their ability to form crystals on a production-line basis. This has improved success rates and made crystallization much more convenient. High-throughput crystallization, however, cannot relieve users of the task of producing samples of high quality. Moreover, the time gained from eliminating manual preparations must now be invested in the careful evaluation of the increased number of experiments. The latter requires a sophisticated data and laboratory information-management system. A review of the current state of automation at the individual steps of crystallization with specific attention to the automation of optimization is given. PMID:24915074

New Insights on the Rheology of Olivine Deformed under Lithospheric Temperature Conditions

NASA Astrophysics Data System (ADS)

Cordier, P.; Demouchy, S. A.; Mussi, A.; Tommasi, A.

2014-12-01

Rheology of mantle rocks at lithospheric temperatures remains poorly constrained, since most experimental studies on creep mechanisms of olivine single crystals ((MgFe)2SiO4, Pbnm) and polycrystalline olivine aggregates were performed at high-temperatures (T >> 1200oC). In this study, we report results from deformation experiments on oriented single crystals of San Carlos olivine and polycrystalline olivine aggregate at temperatures relevant of the uppermost mantle (ranging from 800o to 1090oC) in tri-axial compression. The experiments were carried out at a confining pressure of 300 MPa in a high-resolution gas-medium mechanical testing apparatus at various constant strain rates (from 7 x 10-6 s-1 to 1 x 10-4 s-1). Mechanical tests show that mantle lithosphere is actually weaker than previously inferred from the extrapolation of high-temperature experiments. In this study, we present characterization of dislocation microstructures based on transmission electron microscopy and electron tomography. It is shown that below 1000°C, dislocation activity is restricted to [001] glide with a strong predominance of {110} as glide planes. We observe recovery mechanisms which suggest that the mechanical properties observed in laboratory experiments represent an upper bound for the actual behavior of olivine under lithospheric mantle conditions. Moreover, the drastic reduction in slip system activity observed questions the ability of deforming olivine aggregates in the ductile regime at such temperatures. We show that ductility is preserved thanks to the activation of alternative deformation mechanisms in grain boundaries involving disclinations.

Demonstration of Crystal Structure.

ERIC Educational Resources Information Center

Neville, Joseph P.

1985-01-01

Describes an experiment where equal parts of copper and aluminum are heated then cooled to show extremely large crystals. Suggestions are given for changing the orientation of crystals by varying cooling rates. Students are more receptive to concepts of microstructure after seeing this experiment. (DH)

Synthesis, crystal structures, molecular docking, and in vitro biological activities evaluation of transition metal complexes with 4-(3,4-dichlorophenyl) piperazine-1-carboxylic acid

NASA Astrophysics Data System (ADS)

Chen, Zhi-Jian; Chen, Ya-Na; Xu, Chun-Na; Zhao, Shan-Shan; Cao, Qi-Yue; Qian, Shao-Song; Qin, Jie; Zhu, Hai-Liang

2016-08-01

Three novel mononuclear complexes, [MⅡ(L)2·2H2O], (M = Cu, Ni or Cd; HL = 4-(3,4-dichlorophenyl)piperazine-1-carboxylic acid)were synthesized and structurally determined by single-crystal X-ray diffraction. Molecular docking study preliminarily revealed that complex 1 had potential urease inhibitory activity. In accordance with the result of calculation, in vitro tests of the inhibitory activities of complexes 1-3 against jack bean urease showed complex 1 (IC50 = 8.17 ± 0.91 μM) had better inhibitory activities than the positive reference acetohydroxamic acid (AHA) (IC50 = 26.99 ± 1.43 μM), while complexes 2 and 3 showed no inhibitory activities., kinetics study was carried out to explore the mechanism of the inhibiting of the enzyme, and the result indicated that complex 1 was a competitive inhibitor of urease. Albumin binding experiment and in vitro toxicity evaluation of complex 1 were implemented to explore its Pharmacological properties.

Design of activated serine-containing catalytic triads with atomic level accuracy

PubMed Central

Rajagopalan, Sridharan; Wang, Chu; Yu, Kai; Kuzin, Alexandre P.; Richter, Florian; Lew, Scott; Miklos, Aleksandr E.; Matthews, Megan L.; Seetharaman, Jayaraman; Su, Min; Hunt, John. F.; Cravatt, Benjamin F.; Baker, David

2014-01-01

A challenge in the computational design of enzymes is that multiple properties must be simultaneously optimized -- substrate-binding, transition state stabilization, and product release -- and this has limited the absolute activity of successful designs. Here, we focus on a single critical property of many enzymes: the nucleophilicity of an active site residue that initiates catalysis. We design proteins with idealized serine-containing catalytic triads, and assess their nucleophilicity directly in native biological systems using activity-based organophosphate probes. Crystal structures of the most successful designs show unprecedented agreement with computational models, including extensive hydrogen bonding networks between the catalytic triad (or quartet) residues, and mutagenesis experiments demonstrate that these networks are critical for serine activation and organophosphate-reactivity. Following optimization by yeast-display, the designs react with organophosphate probes at rates comparable to natural serine hydrolases. Co-crystal structures with diisopropyl fluorophosphate bound to the serine nucleophile suggest the designs could provide the basis for a new class of organophosphate captures agents. PMID:24705591

Space Shuttle mission: STS-67

NASA Technical Reports Server (NTRS)

1995-01-01

The Space Shuttle Endeavor, scheduled to launch March 2, 1995 from NASA's Kennedy Space Center, will conduct NASA's longest Shuttle flight prior to date. The mission, designated STS-67, has a number of experiments and payloads, which the crew, commanded by Stephen S. Oswald, will have to oversee. This NASA press kit for the mission contains a general background (general press release, media services information, quick-look facts page, shuttle abort modes, summary timeline, payload and vehicle weights, orbital summary, and crew responsibilities); cargo bay payloads and activities (Astro 2, Get Away Special Experiments); in-cabin payloads (Commercial Minimum Descent Altitude Instrumentation Technology Associates Experiments, protein crystal growth experiments, Middeck Active Control Experiment, and Shuttle Amateur Radio Experiment); and the STS-67 crew biographies. The payloads and experiments are described and summarized to give an overview of the goals, objectives, apparatuses, procedures, sponsoring parties, and the assigned crew members to carry out the tasks.

Spacelab J experiment descriptions

NASA Technical Reports Server (NTRS)

Miller, Teresa Y. (Editor)

1993-01-01

Brief descriptions of the experiment investigations for the Spacelab J Mission which was launched from the Kennedy Space Center aboard the Endeavour in Sept. 1992 are presented. Experiments cover the following: semiconductor crystals; single crystals; superconducting composite materials; crystal growth; bubble behavior in weightlessness; microgravity environment; health monitoring of Payload Specialists; cultured plant cells; effect of low gravity on calcium metabolism and bone formation; and circadian rhythm.

Improving axion detection sensitivity in high purity germanium detector based experiments

NASA Astrophysics Data System (ADS)

Xu, Wenqin; Elliott, Steven

2015-04-01

Thanks to their excellent energy resolution and low energy threshold, high purity germanium (HPGe) crystals are widely used in low background experiments searching for neutrinoless double beta decay, e.g. the MAJORANA DEMONSTRATOR and the GERDA experiments, and low mass dark matter, e.g. the CDMS and the EDELWEISS experiments. A particularly interesting candidate for low mass dark matter is the axion, which arises from the Peccei-Quinn solution to the strong CP problem and has been searched for in many experiments. Due to axion-photon coupling, the postulated solar axions could coherently convert to photons via the Primakeoff effect in periodic crystal lattices, such as those found in HPGe crystals. The conversion rate depends on the angle between axions and crystal lattices, so the knowledge of HPGe crystal axis is important. In this talk, we will present our efforts to improve the HPGe experimental sensitivity to axions by considering the axis orientations in multiple HPGe crystals simultaneously. We acknowledge the support of the U.S. Department of Energy through the LANL/LDRD Program.

Quality Assurance on Undoped CsI Crystals for the Mu2e Experiment

NASA Astrophysics Data System (ADS)

Atanov, N.; Baranov, V.; Budagov, J.; Davydov, Yu. I.; Glagolev, V.; Tereshchenko, V.; Usubov, Z.; Cervelli, F.; Di Falco, S.; Donati, S.; Morescalchi, L.; Pedreschi, E.; Pezzullo, G.; Raffaelli, F.; Spinella, F.; Colao, F.; Cordelli, M.; Corradi, G.; Diociaiuti, E.; Donghia, R.; Giovannella, S.; Happacher, F.; Martini, M.; Miscetti, S.; Ricci, M.; Saputi, A.; Sarra, I.; Echenard, B.; Hitlin, D. G.; Hu, C.; Miyashita, T.; Porter, F.; Zhang, L.; Zhu, R.-Y.; Grancagnolo, F.; Tassielli, G.; Murat, P.

2018-02-01

The Mu2e experiment is constructing a calorimeter consisting of 1,348 undoped CsI crystals in two disks. Each crystal has a dimension of 34 x 34 x 200 mm, and is readout by a large area silicon PMT array. A series of technical specifications was defined according to physics requirements. Preproduction CsI crystals were procured from three firms: Amcrys, Saint-Gobain and Shanghai Institute of Ceramics. We report the quality assurance on crystal's scintillation properties and their radiation hardness against ionization dose and neutrons. With a fast decay time of 30 ns and a light output of more than 100 p.e./MeV measured with a bi-alkali PMT, undoped CsI crystals provide a cost-effective solution for the Mu2e experiment.

SKYLAB (SL)-3 - EXPERIMENT HARDWARE

NASA Image and Video Library

1973-11-08

S74-19677 (April 1974) --- This crystal of Germanium Selenide (GeSe) was grown under weightless conditions in an electric furnace aboard the Skylab space station. Experiment M556, Vapor Growth of IV-VI Compounds, was conducted as a comparative test of GeSe crystals grown on Earth and those grown in a weightless environment. Skylab postflight results indicate that crystals grown in a zero-gravity situation demonstrate greater growth and better composite structure than those grown in ground-bases laboratories. The GeSe crystal shown here is 20 millimeters long, the largest crystal ever grown on Earth or in space. Principal Investigator for Experiment M556 is Dr. Harry Wiedemaier, Rensselaer Polytechnic Institute, Troy, New York. (See NASA photograph S74-19676 for an example of an Earth-grown Germanium Selenide crystal.) Photo credit: NASA

Crystal structure, phytochemical study and enzyme inhibition activity of Ajaconine and Delectinine

NASA Astrophysics Data System (ADS)

Ahmad, Shujaat; Ahmad, Hanif; Khan, Hidayat Ullah; Shahzad, Adnan; Khan, Ezzat; Ali Shah, Syed Adnan; Ali, Mumtaz; Wadud, Abdul; Ghufran, Mehreen; Naz, Humera; Ahmad, Manzoor

2016-11-01

The Crystal structure, comparative DFT study and phytochemical investigation of atisine type C-20 diterpenoid alkaloid ajaconine (1) and lycoctonine type C-19 diterpenoid alkaloid delectinine (2) is reported here. These compounds were isolated from Delphinium chitralense. Both the natural products 1 and 2 crystallize in orthorhombic crystal system with identical space group of P212121. The geometric parameters of both compounds were calculated with the help of DFT using B3LYP/6-31+G (p) basis set and HOMO-LUMO energies, optimized band gaps, global hardness, ionization potential, electron affinity and global electrophilicity are calculated. The compounds 1 and 2 were screened for acetyl cholinesterase and butyryl cholinesterase inhibition activities in a dose dependent manner followed by molecular docking to explore the possible inhibitory mechanism of ajaconine (1) and delectinine (2). The IC50 values of tested compounds against AChE were observed as 12.61 μM (compound 1) and 5.04 μM (compound 2). The same experiments were performed for inhibition of BChE and IC50 was observed to be 10.18 μM (1) and 9.21 μM (2). Promising inhibition activity was shown by both the compounds against AChE and BChE in comparison with standard drugs available in the market such as allanzanthane and galanthamine. The inhibition efficiency of both the natural products was determined in a dose dependent manner.

An experimental study of pyroxene crystallization during rapid cooling in a thermal gradient; applications to komatiites and chondrites

NASA Astrophysics Data System (ADS)

Bouquain, S.; Arndt, N. T.; Faure, F.; Libourel, G.

2013-03-01

To investigate the crystallization of pyroxene in spinifex-textured komatiites and in chondrites we undertook a series of experiments in which compositions in the CMAS system were cooling rapidly in a thermal gradient. Cooling rates were generally between 5 to 10 °C h-1 but some runs were made at 100-200 °C h-1; thermal gradients were between 10 and 20 °C cm-1. These conditions reproduced those at various levels in the crust of komatiitic lava flow. The starting composition was chosen to have pigeonite on the liquidus and a majority of the experiments crystallized zoned pigeonite-diopside crystals like those in komatiite lavas. A~conspicuous aspect of the experimental results was their lack of reproduceability. Some experiments crystallized forsterite whereas others that were run under similar conditions crystallized two pyroxenes and no forsterite; some experiments were totally glassy but others totally crystallized to pyroxene. The degree of supercooling at the onset of pyroxene crystallization was variable, from less than 25 °C to more than 110 °C. We attribute these results to the difficulty of nucleation of pyroxene. In some cases forsterite crystallized metastably and modified the liquid composition to inhibit pyroxene crystallization; in others no nucleation took place until a large degree of supercooling was achieved, then pyroxene crystallized rapidly. Pigeonite crystallized under a wide range of conditions, at cooling rates from 3 to 100 °C h-1. The notion that this mineral only forms at low cooling rates is not correct.

Studies on the in vitro and in vivo antiurolithic activity of Holarrhena antidysenterica.

PubMed

Khan, Aslam; Khan, Saeed R; Gilani, Anwar H

2012-12-01

Holarrhena antidysenterica has a traditional use in the treatment of urolithiasis, therefore, its crude extract has been investigated for possible antiurolithic effect. The crude aqueous-methanolic extract of Holarrhena antidysenterica (Ha.Cr) was studied using the in vitro and in vivo methods. In the in vitro experiments, Ha.Cr demonstrated a concentration-dependent (0.25-4 mg/ml) inhibitory effect on the slope of aggregation. It decreased the size of crystals and transformed the calcium oxalate monohydrate (COM) to calcium oxalate dehydrate (COD) crystals, in calcium oxalate metastable solutions. It also showed concentration-dependent antioxidant effect against 2,2-diphenyl-1-picrylhydrazyl (DPPH) free radicals and lipid peroxidation induced in rat kidney tissue homogenate. Ha.Cr (0.3 mg/ml) reduced (p < 0.05) the cell toxicity and LDH release in renal epithelial cells (MDCK) exposed to oxalate (0.5 mM) and COM (66 μg/cm(2)) crystals. In male Wistar rats, receiving 0.75 % ethylene glycol (EG) for 21 days along with 1 % ammonium chloride (AC) in drinking water, Ha.Cr treatment (30-100 mg/kg) prevented the toxic changes caused by lithogenic agents; EG and AC, like loss of body weight, polyurea, oxaluria, raised serum urea and creatinine levels and crystal deposition in kidneys compared to their respective controls. These data indicate that Holarrhena antidysenterica possesses antiurolithic activity, possibly mediated through the inhibition of CaOx crystal aggregation, antioxidant and renal epithelial cell protective activities and may provide base for designing future studies to establish its efficacy and safety for clinical use.

Ag-ligand modified tungstovandates and their efficient catalysis degradation properties for methylene blue

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zheng, Ran; Zhang, Huixia; Liu, Yunping

Two polytungstovandates [Ag(mbpy){sub 2}][Ag{sub 2}(mbpy){sub 3}][VW{sub 5}O{sub 19}]·H{sub 2}O (1) and [Ag(mbpy)]{sub 2}[Ag(mbpy){sub 2}]{sub 4}[VW{sub 12}O{sub 40}] (2) (mbpy =4,4′-dimethyl-2,2′-bipyridyl), had been hydrothermally synthesized and characterized by IR, TG, and single-crystal X-ray diffraction techniques. Single-crystal structural analysis revealed that the polyanionic clusters in two compounds are different: Lindqvist-type in 1 and α-Keggin-type in 2, respectively, while the cationic moieties in them are Ag-mbpy units. The experiments showed that this kind of hybrid crystal materials possesses more efficiently catalytic performance for the degradation of organic dye methylene blue (MB) in water solution under the UV irradiation. The significant degradation rate ofmore » MB can reach 89.9%, 94.9% by crystals 1 and 2 (40 mg) in the course of about 5 min. - Graphical abstract: Two Ag-ligand modified polytungstovandates had been synthesized and characterized, which were active in the catalytic degradation of organic dye methylene blue under the UV irradiation. - Highlights: • Two Ag-ligand modified tungstovandates were synthesized and characterized. • Weak interactions play important roles in constructing crystal frameworks. • Compounds are active to catalyze the degradation of methylene blue.« less

Morphology and formation mechanism in precipitation of calcite induced by Curvibacter lanceolatus strain HJ-1

NASA Astrophysics Data System (ADS)

Zhang, Chonghong; Li, Fuchun; Lv, Jiejie

2017-11-01

Precipitation of calcium carbobate induced by microbial activities is common occurrence in controlled solution, but the formation mechanism and morphology in precipitation of calcite in solution systems is unclear, and the role of microbes is disputed. Here, culture experiment was performed for 50 days using the Curvibacter lanceolatus strain HJ-1 in a M2 culture medium, and the phase composition and morphology of the precipitates were characterized by the X-ray diffraction (XRD), Fourier transform infrared (FT-IR), and scanning electron microscopy (SEM) techniques. We show that the precipitation processes in our experiment lead to unusual morphologies of crystals corresponding to different growth stages, and the morphologies of the precipitated crystal aggregates ranging from the main rod-, cross-, star-, cauliflower-like morphologies to spherulitic structure. The complex and unusual morphologies of the precipitated calcite by strain HJ-1 may provide a reference point for better understanding the biomineralization mechanism of calcite, moreover, morphological transition of minerals revealed that the multi-ply crystals-aggregation mechanism for calcite growth in crystallisation media.

First results from the PROTEIN experiment on board the International Space Station

NASA Astrophysics Data System (ADS)

Decanniere, Klaas; Potthast, Lothar; Pletser, Vladimir; Maes, Dominique; Otalora, Fermin; Gavira, Jose A.; Pati, Luis David; Lautenschlager, Peter; Bosch, Robert

On March 15 2009 Space Shuttle Discovery was launched, carrying the Process Unit of the Protein Crystallization Diagnostics Facility (PCDF) to the International Space Station. It contained the PROTEIN experiment, aiming at the in-situ observation of nucleation and crystal growth behaviour of proteins. After installation in the European Drawer Rack (EDR) and connection to the PCDF Electronics Unit, experiment runs were performed continuously for 4 months. It was the first time that protein crystallization experiments could be modified on-orbit in near real-time, based on data received on ground. The data included pseudo-dark field microscope images, interferograms, and Dynamic Light Scattering data. The Process Unit with space grown crystals was returned to ground on July 31 2009. Results for the model protein glucose isomerase (Glucy) from Streptomyces rubiginosus crystallized with ammonium sulfate will be reported concerning nucleation and the growth from Protein and Impurities Depletion Zones (PDZs). In addition, results of x-ray analyses for space-grown crystals will be given.

Humidity control and hydrophilic glue coating applied to mounted protein crystals improves X-ray diffraction experiments

PubMed Central

Baba, Seiki; Hoshino, Takeshi; Ito, Len; Kumasaka, Takashi

2013-01-01

Protein crystals are fragile, and it is sometimes difficult to find conditions suitable for handling and cryocooling the crystals before conducting X-ray diffraction experiments. To overcome this issue, a protein crystal-mounting method has been developed that involves a water-soluble polymer and controlled humid air that can adjust the moisture content of a mounted crystal. By coating crystals with polymer glue and exposing them to controlled humid air, the crystals were stable at room temperature and were cryocooled under optimized humidity. Moreover, the glue-coated crystals reproducibly showed gradual transformations of their lattice constants in response to a change in humidity; thus, using this method, a series of isomorphous crystals can be prepared. This technique is valuable when working on fragile protein crystals, including membrane proteins, and will also be useful for multi-crystal data collection. PMID:23999307

The use of workflows in the design and implementation of complex experiments in macromolecular crystallography.

PubMed

Brockhauser, Sandor; Svensson, Olof; Bowler, Matthew W; Nanao, Max; Gordon, Elspeth; Leal, Ricardo M F; Popov, Alexander; Gerring, Matthew; McCarthy, Andrew A; Gotz, Andy

2012-08-01

The automation of beam delivery, sample handling and data analysis, together with increasing photon flux, diminishing focal spot size and the appearance of fast-readout detectors on synchrotron beamlines, have changed the way that many macromolecular crystallography experiments are planned and executed. Screening for the best diffracting crystal, or even the best diffracting part of a selected crystal, has been enabled by the development of microfocus beams, precise goniometers and fast-readout detectors that all require rapid feedback from the initial processing of images in order to be effective. All of these advances require the coupling of data feedback to the experimental control system and depend on immediate online data-analysis results during the experiment. To facilitate this, a Data Analysis WorkBench (DAWB) for the flexible creation of complex automated protocols has been developed. Here, example workflows designed and implemented using DAWB are presented for enhanced multi-step crystal characterizations, experiments involving crystal reorientation with kappa goniometers, crystal-burning experiments for empirically determining the radiation sensitivity of a crystal system and the application of mesh scans to find the best location of a crystal to obtain the highest diffraction quality. Beamline users interact with the prepared workflows through a specific brick within the beamline-control GUI MXCuBE.

Crystal structure, Hirshfeld surfaces and DFT computation of NLO active (2E)-2-(ethoxycarbonyl)-3-[(1-methoxy-1-oxo-3-phenylpropan-2-yl)amino] prop-2-enoic acid.

PubMed

Venkatesan, Perumal; Thamotharan, Subbiah; Ilangovan, Andivelu; Liang, Hongze; Sundius, Tom

2016-01-15

Nonlinear optical (NLO) activity of the compound (2E)-2-(ethoxycarbonyl)-3-[(1-methoxy-1-oxo-3-phenylpropan-2-yl)amino] prop-2-enoic acid is investigated experimentally and theoretically using X-ray crystallography and quantum chemical calculations. The NLO activity is confirmed by both powder Second Harmonic Generation (SHG) experiment and first hyper polarizability calculation. The title compound displays 8 fold excess of SHG activity when compared with the standard compound KDP. The gas phase geometry optimization and vibrational frequencies calculations are performed using density functional theory (DFT) incorporated in B3LYP with 6-311G++(d,p) basis set. The title compound crystallizes in non-centrosymmetric space group P21. Moreover, the crystal structure is primarily stabilized through intramolecular N-H···O and O-H···O hydrogen bonds and intermolecular C-H···O and C-H···π interactions. These intermolecular interactions are analyzed and quantified using Hirshfeld surface analysis and PIXEL method. The detailed vibrational assignments are performed on the basis of the potential energy distributions (PED) of the vibrational modes. Copyright © 2015 Elsevier B.V. All rights reserved.

Microgravity: Teacher's guide with activities for physical science

NASA Technical Reports Server (NTRS)

Vogt, Gregory L.; Wargo, Michael J.; Rosenberg, Carla B. (Editor)

1995-01-01

This guide is an educational tool for teachers of grades 5 through 12. It is an introduction to microgravity and its application to spaceborne laboratory experiments. Specific payloads and missions are mentioned with limited detail, including Spacelab, the International Microgravity Laboratory, and the United States Microgravity Laboratory. Activities for students demonstrate chemistry, mathematics, and physics applications of microgravity. Activity objectives include: modeling how satellites orbit Earth; demonstrating that free fall eliminates the local effects of gravity; measuring the acceleration environments created by different motions; using a plasma sheet to observe acceleration forces that are experienced on board a space vehicle; demonstrating how mass can be measured in microgravity; feeling how inertia affects acceleration; observing the gravity-driven fluid flow that is caused by differences in solution density; studying surface tension and the fluid flows caused by differences in surface tension; illustrating the effects of gravity on the burning rate of candles; observing candle flame properties in free fall; measuring the contact angle of a fluid; illustrating the effects of gravity and surface tension on fiber pulling; observing crystal growth phenomena in a 1-g environment; investigating temperature effects on crystal growth; and observing crystal nucleation and growth rate during directional solidification. Each activity includes a background section, procedure, and follow-up questions.

Rapid crystallization during recycling of basaltic andesite tephra: timescales determined by reheating experiments

PubMed Central

Deardorff, Nicholas; Cashman, Katharine

2017-01-01

Microcrystalline inclusions within microlite-poor matrix are surprisingly common in low intensity eruptions around the world, yet their origin is poorly understood. Inclusions are commonly interpreted as evidence of crystallization along conduit margins. Alternatively, these clasts may be recycled from low level eruptions where they recrystallize by heating within the vent. We conducted a series of experiments heating basaltic andesite lapilli from temperatures below the glass transition (~690 °C) to above inferred eruption temperatures (>1150 °C) for durations of 2 to >60 minutes. At 690 °C < T < 800 °C, crystallization is evident after heating for ~20 minutes; at T > 800 °C, crystallization occurs in <5 minutes. At T ≥ 900 °C, all samples recrystallize extensively in 2–10 minutes, with pyroxenes, Fe-oxides, and plagioclase. Experimental crystallization textures closely resemble those observed in natural microcrystalline inclusions. Comparison of inclusion textures in lapilli from the active submarine volcano NW Rota-1, Mariana arc and subaerial volcano Stromboli suggest that characteristic signatures of clast recycling are different in the two environments. Specifically, chlorine assimilation provides key evidence of recycling in submarine samples, while bands of oxides bordering microcrystalline inclusions are unique to subaerial environments. Correct identification of recycling at basaltic vents will improve (lower) estimates of mass eruption rate and help to refine interpretations of eruption dynamics. PMID:28402339

Processing materials in space - The history and the future

NASA Technical Reports Server (NTRS)

Chassay, Roger; Carswell, Bill

1987-01-01

The development of materials processing in space, and some of the Soyuz, Apollo, Skylab, and Shuttle orbital materials experiments are reviewed. Consideration is given to protein crystal growth, electrophoresis, low-gravity isoelectric focusing, phase partitioning, a monodisperse latex reactor, semiconductor crystal growth, solution crystal growth, the triglycine sulfate experiment, vapor crystal growth experiments, the mercuric iodide experiment, electronic and electrooptical materials, organic thin films and crystalline solids, deep undercooling of metals and alloys, magnetic materials, immiscible materials, metal solidification research, reluctant glass-forming materials, and containerless glass formation. The space processing apparatuses and ground facilities, for materials processing are described. Future facilities for commercial research, development, and manufacturing in space are proposed.

Friction and wear of single-crystal and polycrystalline maganese-zinc ferrite in contact with various metals

NASA Technical Reports Server (NTRS)

Miyoshi, K.; Buckley, D. H.

1977-01-01

Sliding friction experiments were conducted with single-crystal (SCF) and hot-pressed polycrystalline (HPF) manganese-zinc ferrite in contact with various metals. Results indicate that the coefficients of friction for SCF and HPF are related to the relative chemical activity of those metals in high vacuum. The more active the metal, the higher the coefficient of friction. The coefficients of friction for both SCF and HPF were the same and much higher in vacuum than in argon at atmospheric pressure. All the metals tested transferred to the surface of both SCF and HPF in sliding. Both SCF and HPF exhibited cracking and fracture with sliding. Cracking in SCF is dependent on crystallographic characteristics. In HPF, cracking depends on the orientation of the individual crystallites.

Immersion Freezing of Total Ambient Aerosols and Ice Residuals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Kulkarni, Gourihar

This laboratory study reports pre-activation measurements of the size-selected un-activated ambient or total aerosols at the temperature range from -26 to -34°C using two continuous-flow diffusion chamber style ice nucleation chambers. Two different experiments (A and B) were performed in immersion freezing mode. In experiment A, frozen fraction of total aerosol was measured, whereas in experiment B frozen fraction of ice residuals (IR) obtained through sublimation of nucleated ice crystals was measured. Frozen fractions at respective temperatures from experiment B were observed to be higher than A, and therefore it was concluded that ambient particles show pre-activation phenomenon. Furthermore, single-particlemore » elemental composition analyses of the total aerosols showed that majority of the particles are dust particles coated by organic matter. In general, this study suggests that such internally mixed complex total aerosols are efficient ice nucleating particles (INPs) and motivates further research to examine the physio-chemical properties of IR particles to explain the phenomenon of pre-activation.« less

Synthesis and Physical Properties of Liquid Crystals: An Interdisciplinary Experiment

ERIC Educational Resources Information Center

Van Hecke, Gerald R.; Karukstis, Kerry K.; Hanhan Li; Hendargo, Hansford C.; Cosand, Andrew J.; Fox, Marja M.

2005-01-01

A study involves multiple chemistry and physics concepts applied to a state of matter that has biological relevance. An experiment involving the synthesis and physical properties of liquid crystals illustrates the interdisciplinary nature of liquid crystal research and the practical devices derived from such research.

Quality Assurance on Undoped CsI Crystals for the Mu2e Experiment

DOE PAGES

Atanov, N.; Baranov, V.; Budagov, J.; ...

2017-12-21

The Mu2e experiment is constructing a calorimeter consisting of 1,348 undoped CsI crystals in two disks. Each crystal has a dimension of 34 x 34 x 200 mm 3, and is readout by a large area silicon PMT array. A series of technical specifications was defined according to physics requirements. Preproduction CsI crystals were procured from three firms: Amcrys, Saint-Gobain and Shanghai Institute of Ceramics. We report the quality assurance on crystal's scintillation properties and their radiation hardness against ionization dose and neutrons. With a fast decay time of 30 ns and a light output of more than 100 p.e./MeVmore » measured with a bi-alkali PMT, undoped CsI crystals provide a cost-effective solution for the Mu2e experiment.« less

Quality Assurance on Undoped CsI Crystals for the Mu2e Experiment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Atanov, N.; Baranov, V.; Budagov, J.

The Mu2e experiment is constructing a calorimeter consisting of 1,348 undoped CsI crystals in two disks. Each crystal has a dimension of 34 x 34 x 200 mm 3, and is readout by a large area silicon PMT array. A series of technical specifications was defined according to physics requirements. Preproduction CsI crystals were procured from three firms: Amcrys, Saint-Gobain and Shanghai Institute of Ceramics. We report the quality assurance on crystal's scintillation properties and their radiation hardness against ionization dose and neutrons. With a fast decay time of 30 ns and a light output of more than 100 p.e./MeVmore » measured with a bi-alkali PMT, undoped CsI crystals provide a cost-effective solution for the Mu2e experiment.« less

Nanoscale effects of silica particle supports on the formation and properties of TiO2 nanocatalysts

NASA Astrophysics Data System (ADS)

Li, Aize; Jin, Yuhui; Muggli, Darrin; Pierce, David T.; Aranwela, Hemantha; Marasinghe, Gaya K.; Knutson, Theodore; Brockman, Greg; Zhao, Julia Xiaojun

2013-06-01

Small TiO2 crystals in the anatase phase are in high demand as photocatalysts. Stable TiO2 crystals in the anatase phase were obtained using a silica nanoparticle as a support. The focus of this study was to investigate the nanoscale effect of the silica support on the formation and properties of small anatase crystals. The experiments were carried out using powder X-ray diffraction, differential thermal analysis, transmission electron microscopy, and energy dispersion spectroscopy. The results showed that the size of the silica support played a crucial role in crystallization of TiO2 and regulation of TiO2 properties, including phase transition, crystal size, thermodynamic property and catalytic activity. A nanoscale curvature model of the spherical silica support was proposed to explain these size effects. Finally, the developed TiO2 catalysts were applied to the oxidation of methanol using a high-throughput photochemical reactor. The size effect of the silica supports on the TiO2 catalytic efficiency was demonstrated using this system.

Computational model for living nematic

NASA Astrophysics Data System (ADS)

Genkin, Mikhail; Sokolov, Andrey; Lavrentovich, Oleg; Aranson, Igor

A realization of an active system has been conceived by combining swimming bacteria and a lyotropic nematic liquid crystal. Here, by coupling the well-established and validated model of nematic liquid crystals with the bacterial dynamics we developed a computational model describing intricate properties of such a living nematic. In faithful agreement with the experiment, the model reproduces the onset of periodic undulation of the nematic director and consequent proliferation of topological defects with the increase in bacterial concentration. It yields testable prediction on the accumulation and transport of bacteria in the cores of +1/2 topological defects and depletion of bacteria in the cores of -1/2 defects. Our new experiment on motile bacteria suspended in a free-standing liquid crystalline film fully confirmed this prediction. This effect can be used to capture and manipulation of small amounts of bacteria.

Gentle, fast and effective crystal soaking by acoustic dispensing

PubMed Central

Ng, Jia Tsing; Talon, Romain; Nekrosiute, Karolina; Krojer, Tobias; Douangamath, Alice; Brandao-Neto, Jose; Pearce, Nicholas M.; von Delft, Frank

2017-01-01

The steady expansion in the capacity of modern beamlines for high-throughput data collection, enabled by increasing X-ray brightness, capacity of robotics and detector speeds, has pushed the bottleneck upstream towards sample preparation. Even in ligand-binding studies using crystal soaking, the experiment best able to exploit beamline capacity, a primary limitation is the need for gentle and nontrivial soaking regimens such as stepwise concentration increases, even for robust and well characterized crystals. Here, the use of acoustic droplet ejection for the soaking of protein crystals with small molecules is described, and it is shown that it is both gentle on crystals and allows very high throughput, with 1000 unique soaks easily performed in under 10 min. In addition to having very low compound consumption (tens of nanolitres per sample), the positional precision of acoustic droplet ejection enables the targeted placement of the compound/solvent away from crystals and towards drop edges, allowing gradual diffusion of solvent across the drop. This ensures both an improvement in the reproducibility of X-ray diffraction and increased solvent tolerance of the crystals, thus enabling higher effective compound-soaking concentrations. The technique is detailed here with examples from the protein target JMJD2D, a histone lysine demethylase with roles in cancer and the focus of active structure-based drug-design efforts. PMID:28291760

Ground Based Experiments in Support of Microgravity Research Results-Vapor Growth of Organic Nonlinear Optical Thin Film

NASA Technical Reports Server (NTRS)

Zugrav, M. Ittu; Carswell, William E.; Haulenbeek, Glen B.; Wessling, Francis C.

2001-01-01

This work is specifically focused on explaining previous results obtained for the crystal growth of an organic material in a reduced gravity environment. On STS-59, in April 1994, two experiments were conducted with N,N-dimethyl-p-(2,2-dicyanovinyl) aniline (DCVA), a promising nonlinear optical (NLO) material. The space experiments were set to reproduce laboratory experiments that yielded small, bulk crystals of DCVA. The results of the flight experiment, however, were surprising. Rather than producing a bulk single crystal, the result was the production of two high quality, single crystalline thin films. This result was even more intriguing when it is considered that thin films are more desirable for NLO applications than are bulk single crystals. Repeated attempts on the ground to reproduce these results were fruitless. A second set of flight experiments was conducted on STS-69 in September 1995. This time eight DCVA experiments were flown, with each of seven experiments containing a slight change from the first reference experiment. The reference experiment was programmed with growth conditions identical to those of the STS-59 mission. The slight variations in each of the other seven were an attempt to understand what particular parameter was responsible for the preference of thin film growth over bulk crystal growth in microgravity. Once again the results were surprising. In all eight cases thin films were grown again, albeit with varying quality. So now we were faced with a phenomenon that not only takes place in microgravity, but also is very robust, resisting all attempts to force the growth of bulk single crystals.

Shuttle Mission STS-50: Orbital Processing of High-Quality CdTe Compound Semiconductors Experiment: Final Flight Sample Characterization Report

NASA Technical Reports Server (NTRS)

Larson, David J.; Casagrande, Luis G.; DiMarzio, Don; Alexander, J. Iwan D.; Carlson, Fred; Lee, Taipo; Dudley, Michael; Raghathamachar, Balaji

1998-01-01

The Orbital Processing of High-Quality Doped and Alloyed CdTe Compound Semiconductors program was initiated to investigate, quantitatively, the influences of gravitationally dependent phenomena on the growth and quality of bulk compound semiconductors. The objective was to improve crystal quality (both structural and compositional) and to better understand and control the variables within the crystal growth production process. The empirical effort entailed the development of a terrestrial (one-g) experiment baseline for quantitative comparison with microgravity (mu-g) results. This effort was supported by the development of high-fidelity process models of heat transfer, fluid flow and solute redistribution, and thermo-mechanical stress occurring in the furnace, safety cartridge, ampoule, and crystal throughout the melting, seeding, crystal growth, and post-solidification processing. In addition, the sensitivity of the orbital experiments was analyzed with respect to the residual microgravity (mu-g) environment, both steady state and g-jitter. CdZnTe crystals were grown in one-g and in mu-g. Crystals processed terrestrially were grown at the NASA Ground Control Experiments Laboratory (GCEL) and at Grumman Aerospace Corporation (now Northrop Grumman Corporation). Two mu-g crystals were grown in the Crystal Growth Furnace (CGF) during the First United States Microgravity Laboratory Mission (USML-1), STS-50, June 24 - July 9, 1992.

Growth of InSb and InI Crystals on Earth and in Microgravity

NASA Technical Reports Server (NTRS)

Ostrogorsky, A. G.; Churilov, A.; Volz, M. P.; Riabov, V.; Van den Berg, L.

2015-01-01

During the past 40 years, dozens of semiconductor crystal growth experiments have been conducted in space laboratories. The subsequent analysis of the space-grown crystals revealed (i) that weak convection existed in virtually all melt-growth experiments, (ii) de-wetting significantly reduced the level of stress-induced defects, and (iii) particularly encouraging results were obtained in vapor-growth experiments. In 2002, following a decade of ground based research in growing doped Ge and GaSb crystals, a series of crystal growth experiments was performed at the ISS, within the SUBSA (Solidification Using a Baffle in Sealed Ampoules) investigation. Te- and Zn-doped InSb crystals were grown from the melt. The specially designed furnace provided a side-view of the melt and precise seeding measurement of the growth rate. At present, under sponsorship of CASIS (Center for the Advancement of Science in Space, www.iss-casis.org), we are conducting ground-based experiments with indium mono-iodide (InI) in preparation for the "SUBSA II" ISS investigation, planned for 2017. The experiments include: i) Horizontal Bridgman (HB) growth and ii) Vapor Transport (VT) growth. Finite element modeling will also be conducted, to optimize the design of the flight ampoules, for vapor and melt growth.

An experimental study of pyroxene crystallization during rapid cooling in a thermal gradient: application to komatiites

NASA Astrophysics Data System (ADS)

Bouquain, S.; Arndt, N. T.; Faure, F.; Libourel, G.

2014-07-01

To investigate the crystallization of pyroxene in spinifex-textured komatiites, we undertook a series of experiments in which compositions in the CaO-MgO-Al2O3-SiO2 CMAS system were cooled rapidly in a thermal gradient. Cooling rates were generally between 5 and 10 °C h-1, but some runs were made at 100-200 °C h-1; thermal gradients were between 10 and 20 °C cm-1. These conditions reproduced those at various depths in the crust of komatiite lava flow. The starting composition was chosen to have pigeonite on the liquidus, and most of the experimental charges crystallized zoned pigeonite-diopside crystals like those in komatiite lavas. An intriguing aspect of the experimental results was their lack of reproducibility. Some experiments crystallized forsterite, whereas others that were run under similar conditions crystallized two pyroxenes and no forsterite; some experiments were totally glassy, but others crystallized entirely to pyroxene. The degree of supercooling at the onset of pyroxene crystallization was variable, from less than 25 °C to more than 110 °C. We attribute these results to the difficulty of nucleation of pyroxene under the conditions of the experiments. In some cases forsterite crystallized metastably and modified the liquid composition to inhibit pyroxene crystallization; in others no nucleation took place until a large degree of supercooling was achieved, and then pyroxene crystallized rapidly. Pigeonite crystallized under a wide range of conditions, at cooling rates from 3 to 100 °C h-1. The notion that this mineral only forms at low cooling rates is not correct.

Crystalline heterogeneities and instabilities in thermally convecting magma chamber

NASA Astrophysics Data System (ADS)

Culha, C.; Suckale, J.; Qin, Z.

2016-12-01

A volcanic vent can supply different densities of crystals over an eruption time period. This has been seen in Hawai'i's Kilauea Iki 1959 eruption; however it is not common for all Kilauea or basaltic eruptions. We ask the question: Under what conditions can homogenous magma chamber cultivate crystalline heterogeneities? In some laboratory experiments and numerical simulations, a horizontal variation is observed. The region where crystals reside is identified as a retention zone: convection velocity balances settling velocity. Simulations and experiments that observe retention zones assume crystals do not alter the convection in the fluid. However, a comparison of experiments and simulations of convecting magma with crystals suggest that large crystal volume densities and crystal sizes alter fluid flow considerably. We introduce a computational method that fully resolves the crystalline phase. To simulate basaltic magma chambers in thermal convection, we built a numerical solver of the Navier-Stoke's equation, continuity equation, and energy equation. The modeled magma is assumed to be a viscous, incompressible fluid with a liquid and solid phase. Crystals are spherical, rigid bodies. We create Rayleigh-Taylor instability through a cool top layer and hot bottom layer and update magma density while keeping crystal temperature and size constant. Our method provides a detailed picture of magma chambers, which we compare to other models and experiments to identify when and how crystals alter magma chamber convection. Alterations include stratification, differential settling and instabilities. These characteristics are dependent on viscosity, convection vigor, crystal volume density and crystal characteristics. We reveal that a volumetric crystal density variation may occur over an eruption time period, if right conditions are met to form stratifications and instabilities in magma chambers. These conditions are realistic for Kilauea Iki's 1959 eruption.

Investigation of microgravity effects on solidification phenomena of selected materials

NASA Technical Reports Server (NTRS)

Maag, Carl R.; Hansen, Patricia A.

1992-01-01

A Get Away Special (GAS) experiment payload to investigate microgravity effects on solidification phenomena of selected experimental samples has been designed for flight. It is intended that the first flight of the assembly will (1) study the p-n junction characteristics for advancing semiconductor device applications, (2) study the effects of gravity-driven convection on the growth of HgCd crystals, (3) compare the textures of the sample which crystallizes in microgravity with those found in chondrite meteorites, and (4) modify glass optical characteristics through divalent oxygen exchange. The space flight experiment consists of many small furnaces. While the experiment payload is in the low gravity environment of orbital flight, the payload controller will sequentially activate the furnaces to heat samples to their melt state and then allow cooling to resolidification in a controlled fashion. The materials processed in the microgravity environment of space will be compared to the same materials processed on earth in a one-gravity environment. This paper discusses the design of all subassemblies (furnance, electronics, and power systems) in the experiment. A complete description of the experimental materials is also presented.

Experiment and density functional theory analyses of GdTaO4 single crystal

NASA Astrophysics Data System (ADS)

Ding, Shoujun; Kinross, Ashlie; Wang, Xiaofei; Yang, Huajun; Zhang, Qingli; Liu, Wenpeng; Sun, Dunlu

2018-05-01

GdTaO4 is a type of excellent materials that can be used as scintillation, laser matrix as well as self-activated phosphor has generated significant interest. Whereas its band structure, electronic structure and optical properties are still need elucidation. To solve this intriguing problem, high-quality GdTaO4 single crystal (M-type) was grown successfully using Czochralski method. Its structure as well as optical properties was determined in experiment. Moreover, a systematic theoretical calculation based on the density function theory methods were performed on M-type and M‧-type GdTaO4 and their band structure, density of state as well as optical properties were obtained. Combine with the performed experiment results, the calculated results were proved with high reliability. Hence, the calculated results obtained in this work could provide a deep understanding of GdTaO4 material, which also useful for the further investigation on GdTaO4 material.

A Physical Chemistry Experiment in Polymer Crystallization Kinetics

ERIC Educational Resources Information Center

Singfield, Kathy L.; Chisholm, Roderick A.; King, Thomas L.

2012-01-01

A laboratory experiment currently used in an undergraduate physical chemistry lab to investigate the rates of crystallization of a polymer is described. Specifically, the radial growth rates of typical disc-shaped crystals, called spherulites, growing between microscope glass slides are measured and the data are treated according to polymer…

Zeolite crystal growth in space - What has been learned

NASA Technical Reports Server (NTRS)

Sacco, A., Jr.; Thompson, R. W.; Dixon, A. G.

1993-01-01

Three zeolite crystal growth experiments developed at WPI have been performed in space in last twelve months. One experiment, GAS-1, illustrated that to grow large, crystallographically uniform crystals in space, the precursor solutions should be mixed in microgravity. Another experiment evaluated the optimum mixing protocol for solutions that chemically interact ('gel') on contact. These results were utilized in setting the protocol for mixing nineteen zeolite solutions that were then processed and yielded zeolites A, X and mordenite. All solutions in which the nucleation event was influenced produced larger, more 'uniform' crystals than did identical solutions processed on earth.

Fast and scalable purification of a therapeutic full-length antibody based on process crystallization.

PubMed

Smejkal, Benjamin; Agrawal, Neeraj J; Helk, Bernhard; Schulz, Henk; Giffard, Marion; Mechelke, Matthias; Ortner, Franziska; Heckmeier, Philipp; Trout, Bernhardt L; Hekmat, Dariusch

2013-09-01

The potential of process crystallization for purification of a therapeutic monoclonal IgG1 antibody was studied. The purified antibody was crystallized in non-agitated micro-batch experiments for the first time. A direct crystallization from clarified CHO cell culture harvest was inhibited by high salt concentrations. The salt concentration of the harvest was reduced by a simple pretreatment step. The crystallization process from pretreated harvest was successfully transferred to stirred tanks and scaled-up from the mL-scale to the 1 L-scale for the first time. The crystallization yield after 24 h was 88-90%. A high purity of 98.5% was reached after a single recrystallization step. A 17-fold host cell protein reduction was achieved and DNA content was reduced below the detection limit. High biological activity of the therapeutic antibody was maintained during the crystallization, dissolving, and recrystallization steps. Crystallization was also performed with impure solutions from intermediate steps of a standard monoclonal antibody purification process. It was shown that process crystallization has a strong potential to replace Protein A chromatography. Fast dissolution of the crystals was possible. Furthermore, it was shown that crystallization can be used as a concentrating step and can replace several ultra-/diafiltration steps. Molecular modeling suggested that a negative electrostatic region with interspersed exposed hydrophobic residues on the Fv domain of this antibody is responsible for the high crystallization propensity. As a result, process crystallization, following the identification of highly crystallizable antibodies using molecular modeling tools, can be recognized as an efficient, scalable, fast, and inexpensive alternative to key steps of a standard purification process for therapeutic antibodies. Copyright © 2013 Wiley Periodicals, Inc.

Growing protein crystals in microgravity - The NASA Microgravity Science and Applications Division (MSAD) Protein Crystal Growth (PCG) program

NASA Technical Reports Server (NTRS)

Herren, B.

1992-01-01

In collaboration with a medical researcher at the University of Alabama at Birmingham, NASA's Marshall Space Flight Center in Huntsville, Alabama, under the sponsorship of the Microgravity Science and Applications Division (MSAD) at NASA Headquarters, is continuing a series of space experiments in protein crystal growth which could lead to innovative new drugs as well as basic science data on protein molecular structures. From 1985 through 1992, Protein Crystal Growth (PCG) experiments will have been flown on the Space Shuttle a total of 14 times. The first four hand-held experiments were used to test hardware concepts; later flights incorporated these concepts for vapor diffusion protein crystal growth with temperature control. This article provides an overview of the PCG program: its evolution, objectives, and plans for future experiments on NASA's Space Shuttle and Space Station Freedom.

Quantifying Aluminum Crystal Size Part 2: The Model-Development Sequence

ERIC Educational Resources Information Center

Hjalmarson, Margret; Diefes-Dux, Heidi A.; Bowman, Keith; Zawojewski, Judith S.

2006-01-01

We have designed model-development sequences using a common context to provide authentic problem-solving experiences for first-year students. The model-development sequence takes a model-eliciting activity a step further by engaging students in the exploration and adaptation of a mathematical model (e.g., procedure, algorithm, method) for solving…

Preparative Protein Production from Inclusion Bodies and Crystallization: A Seven-Week Biochemistry Sequence

ERIC Educational Resources Information Center

Peterson, Megan J.; Snyder, W. Kalani; Westerman, Shelley; McFarland, Benjamin J.

2011-01-01

We describe how to produce and purify proteins from "Escherichia coli" inclusion bodies by adapting versatile, preparative-scale techniques to the undergraduate laboratory schedule. This 7-week sequence of experiments fits into an annual cycle of research activity in biochemistry courses. Recombinant proteins are expressed as inclusion bodies,…

Toward Fully in Silico Melting Point Prediction Using Molecular Simulations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang, Y; Maginn, EJ

2013-03-01

Melting point is one of the most fundamental and practically important properties of a compound. Molecular computation of melting points. However, all of these methods simulation methods have been developed for the accurate need an experimental crystal structure as input, which means that such calculations are not really predictive since the melting point can be measured easily in experiments once a crystal structure is known. On the other hand, crystal structure prediction (CSP) has become an active field and significant progress has been made, although challenges still exist. One of the main challenges is the existence of many crystal structuresmore » (polymorphs) that are very close in energy. Thermal effects and kinetic factors make the situation even more complicated, such that it is still not trivial to predict experimental crystal structures. In this work, we exploit the fact that free energy differences are often small between crystal structures. We show that accurate melting point predictions can be made by using a reasonable crystal structure from CSP as a starting point for a free energy-based melting point calculation. The key is that most crystal structures predicted by CSP have free energies that are close to that of the experimental structure. The proposed method was tested on two rigid molecules and the results suggest that a fully in silico melting point prediction method is possible.« less

Deformation behavior of HCP titanium alloy: Experiment and Crystal plasticity modeling

DOE PAGES

Wronski, M.; Arul Kumar, Mariyappan; Capolungo, Laurent; ...

2018-03-02

The deformation behavior of commercially pure titanium is studied using experiments and a crystal plasticity model. Compression tests along the rolling, transverse, and normal-directions, and tensile tests along the rolling and transverse directions are performed at room temperature to study the activation of slip and twinning in the hexagonal closed packed titanium. A detailed EBSD based statistical analysis of the microstructure is performed to develop statistics of both {10-12} tensile and {11-22} compression twins. A simple Monte Carlo (MC) twin variant selection criterion is proposed within the framework of the visco-plastic self-consistent (VPSC) model with a dislocation density (DD) basedmore » law used to describe dislocation hardening. In the model, plasticity is accommodated by prismatic, basal and pyramidal slip modes, and {10-12} tensile and {11-22} compression twinning modes. Thus, the VPSC-MC model successfully captures the experimentally observed activation of low Schmid factor twin variants for both tensile and compression twins modes. The model also predicts macroscopic stress-strain response, texture evolution and twin volume fraction that are in agreement with experimental observations.« less

Deformation behavior of HCP titanium alloy: Experiment and Crystal plasticity modeling

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wronski, M.; Arul Kumar, Mariyappan; Capolungo, Laurent

The deformation behavior of commercially pure titanium is studied using experiments and a crystal plasticity model. Compression tests along the rolling, transverse, and normal-directions, and tensile tests along the rolling and transverse directions are performed at room temperature to study the activation of slip and twinning in the hexagonal closed packed titanium. A detailed EBSD based statistical analysis of the microstructure is performed to develop statistics of both {10-12} tensile and {11-22} compression twins. A simple Monte Carlo (MC) twin variant selection criterion is proposed within the framework of the visco-plastic self-consistent (VPSC) model with a dislocation density (DD) basedmore » law used to describe dislocation hardening. In the model, plasticity is accommodated by prismatic, basal and pyramidal slip modes, and {10-12} tensile and {11-22} compression twinning modes. Thus, the VPSC-MC model successfully captures the experimentally observed activation of low Schmid factor twin variants for both tensile and compression twins modes. The model also predicts macroscopic stress-strain response, texture evolution and twin volume fraction that are in agreement with experimental observations.« less

Nanomechanical control of optical field and quality factor in photonic crystal structures

NASA Astrophysics Data System (ADS)

Cotrufo, Michele; Midolo, Leonardo; Zobenica, Žarko; Petruzzella, Maurangelo; van Otten, Frank W. M.; Fiore, Andrea

2018-03-01

Actively controlling the properties of localized optical modes is crucial for cavity quantum electrodynamics experiments. While several methods to tune the optical frequency have been demonstrated, the possibility of controlling the shape of the modes has scarcely been investigated. Yet an active manipulation of the mode pattern would allow direct control of the mode volume and the quality factor and therefore of the radiative processes. In this work, we propose and demonstrate a nano-optoelectromechanical device in which a mechanical displacement affects the spatial pattern of the electromagnetic field. The device is based on a double-membrane photonic crystal waveguide which, upon bending, creates a spatial modulation of the effective refractive index, resulting in an effective potential well or antiwell for the optical modes. The change in the field pattern drastically affects the optical losses: large modulations of the quality factors and dissipative coupling rates larger than 1 GHz/nm are predicted by calculations and confirmed by experiments. This concept opens new avenues in solid-state cavity quantum electrodynamics in which the field, instead of the frequency, is coupled to the mechanical motion.

Surrogate Seeds For Growth Of Crystals

NASA Technical Reports Server (NTRS)

Shlichta, Paul J.

1989-01-01

Larger crystals of higher quality grown. Alternative method for starting growth of crystal involves use of seed crystal of different material instead of same material as solution. Intended for growing single-crystal proteins for experiments but applicable in general to growth of crystals from solutions and to growth of semiconductor or other crystals from melts.

Phoenito experiments: combining the strengths of commercial crystallization automation.

PubMed

Newman, Janet; Pham, Tam M; Peat, Thomas S

2008-11-01

The use of crystallization robots for initial screening in macromolecular crystallization is well established. This paper describes how four general optimization techniques, growth-rate modulation, fine screening, seeding and additive screening, have been adapted for automation in a medium-throughput crystallization service facility. The use of automation for more challenging optimization experiments is discussed, as is a novel way of using both the Mosquito and the Phoenix nano-dispensing robots during the setup of a single crystallization plate. This dual-dispenser technique plays to the strengths of both machines.

Phoenito experiments: combining the strengths of commercial crystallization automation

PubMed Central

Newman, Janet; Pham, Tam M.; Peat, Thomas S.

2008-01-01

The use of crystallization robots for initial screening in macromolecular crystallization is well established. This paper describes how four general optimization techniques, growth-rate modulation, fine screening, seeding and additive screening, have been adapted for automation in a medium-throughput crystallization service facility. The use of automation for more challenging optimization experiments is discussed, as is a novel way of using both the Mosquito and the Phoenix nano-dispensing robots during the setup of a single crystallization plate. This dual-dispenser technique plays to the strengths of both machines. PMID:18997323

Microgravity

NASA Image and Video Library

2001-01-24

Experiments with colloidal solutions of plastic microspheres suspended in a liquid serve as models of how molecules interact and form crystals. For the Dynamics of Colloidal Disorder-Order Transition (CDOT) experiment, Paul Chaikin of Princeton University has identified effects that are attributable to Earth's gravity and demonstrated that experiments are needed in the microgravity of orbit. Space experiments have produced unexpected dendritic (snowflake-like) structures. To date, the largest hard sphere crystal grown is a 3 mm single crystal grown at the cool end of a ground sample. At least two more additional flight experiments are plarned aboard the International Space Station. This image is from a video downlink.

Concentration and structure inhomogeneities in GaSb(Si) single crystals grown at different heat and mass transfer conditions

NASA Astrophysics Data System (ADS)

Serebryakov, Yu. A.; Prokhorov, I. A.; Vlasov, V. N.; Korobeynikova, E. N.; Zakharov, B. G.; Shul'pina, I. L.; Marchenko, M. P.; Fryazinov, I. V.

2007-06-01

Results of ground-based experiments on crystallization of gallium antimonide on the POLIZON facility carried out within the framework of space experiment preparation aboard FOTON satellite are submitted. Technical and technological opportunities of suppression of disturbing factors for improvement of quality of grown crystals in space are substantiated. Features of formation of concentration and structure inhomogeneities in GaSb:Si crystals grown under non-stationary and stationary convection conditions are investigated. Experimental data about structure and dopant distribution inhomogeneities are discussed taking into account results of numerical researches of GaSb:Si crystallization. Also earlier received results of modeling of GaSb:Te crystallization under close temperature conditions are used. Correlation between computational and experimental data is shown. The data on intensity of flows close to crystallization front are received at which non-stationary or stationary conditions of crystallization are realized. The forecast for space conditions is made. The influence of a rotating magnetic field on convection in melt for application in space experiment projected is investigated.

Modeling of dislocation dynamics in germanium Czochralski growth

NASA Astrophysics Data System (ADS)

Artemyev, V. V.; Smirnov, A. D.; Kalaev, V. V.; Mamedov, V. M.; Sidko, A. P.; Podkopaev, O. I.; Kravtsova, E. D.; Shimansky, A. F.

2017-06-01

Obtaining very high-purity germanium crystals with low dislocation density is a practically difficult problem, which requires knowledge and experience in growth processes. Dislocation density is one of the most important parameters defining the quality of germanium crystal. In this paper, we have performed experimental study of dislocation density during 4-in. germanium crystal growth using the Czochralski method and comprehensive unsteady modeling of the same crystal growth processes, taking into account global heat transfer, melt flow and melt/crystal interface shape evolution. Thermal stresses in the crystal and their relaxation with generation of dislocations within the Alexander-Haasen model have been calculated simultaneously with crystallization dynamics. Comparison to experimental data showed reasonable agreement for the temperature, interface shape and dislocation density in the crystal between calculation and experiment.

Study of the cosmogenic activation in NaI(Tl) crystals within the ANAIS experiment

NASA Astrophysics Data System (ADS)

Villar, P.; Amaré, J.; Cebrián, S.; Coarasa, I.; García, E.; Martínez, M.; Oliván, M. A.; Ortigoza, Y.; Ortiz de Solórzano, A.; Puimedón, J.; Sarsa, M. L.; Villar, J. A.

2018-03-01

The direct detection of galactic dark matter particles requires ultra-low background conditions. NaI(Tl) crystals are applied in the search for these dark matter particles through their interactions in the detector by measuring the scintillation signal produced. The production of long-lived isotopes in materials due to the exposure to cosmic rays on Earth’s surface can be an hazard for these ultra-low background demanding experiments, typically performed underground. Therefore, production rates of cosmogenic isotopes in all the materials present in the experimental set-up, as well as the corresponding cosmic rays exposure history, must be both well-known in order to assess the relevance of this effect in the achievable sensitivity of a given experiment. Here, analysis of the cosmogenic studies developed from the ANAIS experiment NaI(Tl) detectors are presented. Installed inside a convenient shielding at the Canfranc Underground Laboratory just after finishing surface exposure to cosmic rays and thanks to the prompt data taking developed, identification and quantification of isotopes with half-lives of the order of tens of days were allowed, and thanks to the long-term operation of the detectors long-lived isotopes have been also identified and quantified. Main results for the activation yields of iodine and tellurium isotopes, 22Na, 113Sn, 109Cd, and tritium are presented in this work, together with the estimate of the production rates for their activation by cosmic nucleons while on Earth’s surface based on a selection of excitation functions over the entire energy range of cosmic nucleons.

Collection of Ni-bearing material from electroless plating waste by magnetic separation with HTS bulk magnet

NASA Astrophysics Data System (ADS)

Oka, T.; Fukazawa, H.; Fukui, S.; Ogawa, J.; Sato, T.; Ooizumi, M.; Tsujimura, M.; Yokoyama, K.

2014-01-01

The magnetic separation experiment to collect the Ni compounds from the waste liquid of electroless plating processes was conducted in the open-gradient magnetic separation process with the high temperature superconducting bulk magnet system. The magnetic pole containing Gd-based bulk superconductors was activated to 3.45 T at 35 K in the static magnetic field of 5 T with use of a superconducting solenoid magnet. The coarse Ni-sulfate crystals were formed by adding the concentrated sulfuric acid to the Ni-phosphite precipitates which yielded from the plating waste liquid by controlling the temperature and the pH value. The open-gradient magnetic separation technique was employed to separate the Ni-sulfate crystals from the mixture of the Ni-sulfate and Ni-phosphite compounds by the difference between their magnetic properties. And we succeeded in collecting Ni-sulfate crystals preferentially to the Ni-phosphite by attracting them to the magnetic pole soon after the Ni-sulfate crystals began to grow.

Large fraction of crystal directions leads to ion channeling

NASA Astrophysics Data System (ADS)

Nordlund, K.; Djurabekova, F.; Hobler, G.

2016-12-01

It is well established that when energetic ions are moving in crystals, they may penetrate much deeper if they happen to be directed in some specific crystal directions. This `channeling' effect is utilized for instance in certain ion beam analysis methods and has been described by analytical theories and atomistic computer simulations. However, there have been very few systematic studies of channeling in directions other than the principal low-index ones. We present here a molecular dynamics-based approach to calculate ion channeling systematically over all crystal directions, providing ion `channeling maps' that easily show in which directions channeling is expected. The results show that channeling effects can be quite significant even at energies below 1 keV, and that in many cases, significant planar channeling occurs also in a wide range of crystal directions between the low-index principal ones. In all of the cases studied, a large fraction (˜20 -60 % ) of all crystal directions show channeling. A practical implication of this is that modern experiments on randomly oriented nanostructures will have a large probability of channeling. It also means that when ion irradiations are carried out on polycrystalline samples, channeling effects on the results cannot a priori be assumed to be negligible. The maps allow for easy selection of good `nonchanneling' directions in experiments or alternatively finding wide channels for beneficial uses of channeling. We implement channeling theory to also give the fraction of channeling directions in a manner directly comparable to the simulations. The comparison shows good qualitative agreement. In particular, channeling theory is very good at predicting which channels are active at a given energy. This is true down to sub-keV energies, provided the penetration depth is not too small.

Didanosine polymorphism in a supercritical antisolvent process.

PubMed

Bettini, R; Menabeni, R; Tozzi, R; Pranzo, M B; Pasquali, I; Chierotti, M R; Gobetto, R; Pellegrino, L

2010-04-01

Solid-state properties of active ingredients are crucial in pharmaceutical development owing to their significant clinical and economical implications. In the present work we investigated the solid-state properties and the solubility in water of didanosine, DDI, re-crystallized from a dimethylsulfoxide solution using supercritical CO(2) as an antisolvent (SAS process) for comparison with the commercially available drug product. We also applied modern solid-state NMR (SS NMR) techniques, namely 2D (1)H DQ CRAMPS (Combined Rotation And Multiple Pulse Spectroscopy) and (1)H-(13)C on- and off-resonance CP (cross polarization) FSLG-HETCOR experiments, known for providing reliable information about (1)H-(1)H and (1)H-(13)C intra- and intermolecular proximities, in order to address polymorphism issues arising from the crystallization of a new form in the supercritical process. A new polymorph of didanosine was obtained from the supercritical antisolvent process and characterized by means of 1D and 2D multinuclear ((1)H, (13)C, (15)N) SS NMR. The particle size of the new crystal phase was reduced by varying the antisolvent density through a pressure increase. The structural differences between the commercial product and the SAS re-crystallized DDI are highlighted by X-ray diffractometry and well described by solid-state NMR. The carbon C6 (13)C chemical shift suggests that both commercial and re-crystallized didanosine samples are in the enol form. The analysis of homo- and heteronuclear proximities obtained by means of 2D NMR experiments shows that commercial and SAS re-crystallized DDI possess very similar molecular conformation and hydrogen bond network, but different packing. The new polymorph proved to be a metastable form at ambient conditions, showing higher solubility in water and lower stability to mechanical stress. 2009 Wiley-Liss, Inc. and the American Pharmacists Association

Single-drop optimization of protein crystallization.

PubMed

Meyer, Arne; Dierks, Karsten; Hilterhaus, Dierk; Klupsch, Thomas; Mühlig, Peter; Kleesiek, Jens; Schöpflin, Robert; Einspahr, Howard; Hilgenfeld, Rolf; Betzel, Christian

2012-08-01

A completely new crystal-growth device has been developed that permits charting a course across the phase diagram to produce crystalline samples optimized for diffraction experiments. The utility of the device is demonstrated for the production of crystals for the traditional X-ray diffraction data-collection experiment, of microcrystals optimal for data-collection experiments at a modern microbeam insertion-device synchrotron beamline and of nanocrystals required for data collection on an X-ray laser beamline.

Scientist prepare Lysozyme Protein Crystal

NASA Technical Reports Server (NTRS)

1996-01-01

Dan Carter and Charles Sisk center a Lysozyme Protein crystal grown aboard the USML-2 shuttle mission. Protein isolated from hen egg-white and functions as a bacteriostatic enzyme by degrading bacterial cell walls. First enzyme ever characterized by protein crystallography. It is used as an excellent model system for better understanding parameters involved in microgravity crystal growth experiments. The goal is to compare kinetic data from microgravity experiments with data from laboratory experiments to study the equilibrium.

Skylab experiment performance evaluation manual. Appendix J: Experiment M555 gallium arsenide single crystal growth (MSFC)

NASA Technical Reports Server (NTRS)

Byers, M. S.

1973-01-01

Analyses for Experiment M555, Gallium Arsenide Single Crystal Growth (MSFC), to be used for evaluating the performance of the Skylab corollary experiments under preflight, inflight, and post-flight conditions are presented. Experiment contingency plan workaround procedure and malfunction analyses are presented in order to assist in making the experiment operationally successful.

Inexpensive Electrooptic Experiments on Liquid Crystal Displays.

ERIC Educational Resources Information Center

Ciferno, Thomas M.; And Others

1995-01-01

Describes the construction and use of an electrooptic apparatus that can be incorporated into the classroom to test liquid crystal displays (LCDs) and introduce students to experiments of an applied physics nature with very practical implications. Presents experiments that give students hands-on experience with technologies of current interest to…

STS-67 Space Shuttle mission report

NASA Technical Reports Server (NTRS)

Fricke, Robert W., Jr.

1995-01-01

The STS-67 Space Shuttle Program Mission Report provides the results of the orbiter vehicle performance evaluation during this sixty-eighth flight of the Shuttle Program, the forty-third flight since the return to flight, and the eighth flight of the Orbiter vehicle Endeavour (OV-105). In addition, the report summarizes the payload activities and the performance of the External Tank (ET), Solid Rocket Booster (SRB), Reusable Solid Rocket Motor (RSRM), and the Space Shuttle Main Engines (SSME). The serial numbers of the other elements of the flight vehicle were ET-69 for the ET; 2012, 2033, and 2031 for SSME's 1, 2, and 3, respectively; and Bl-071 for the SRB's. The left-hand RSRM was designated 360W043A, and the right-hand RSRM was designated 360L043B. The primary objective of this flight was to successfully perform the operations of the ultraviolet astronomy (ASTRO-2) payload. Secondary objectives of this flight were to complete the operations of the Protein Crystal Growth - Thermal Enclosure System (PCG-TES), the Protein Crystal Growth - Single Locker Thermal Enclosure System (PCG-STES), the Commercial Materials Dispersion Apparatus ITA Experiments (CMIX), the Shuttle Amateur Radio Experiment-2 (SAREX-2), the Middeck Active Control Experiment (MACE), and two Get-Away Special (GAS) payloads.

Protein crystal growth in microgravity: Temperature induced large scale crystallization of insulin

NASA Technical Reports Server (NTRS)

Long, Marianna M.; Delucas, Larry J.; Smith, C.; Carson, M.; Moore, K.; Harrington, Michael D.; Pillion, D. J.; Bishop, S. P.; Rosenblum, W. M.; Naumann, R. J.

1994-01-01

One of the major stumbling blocks that prevents rapid structure determination using x-ray crystallography is macro-molecular crystal growth. There are many examples where crystallization takes longer than structure determination. In some cases, it is impossible to grow useful crystals on earth. Recent experiments conducted in conjuction with NASA on various Space Shuttle missions have demonstrated that protein crystals often grow larger and display better internal molecular order than their earth-grown counterparts. This paper reports results from three Shuttle flights using the Protein Crystallization Facility (PCF). The PCF hardware produced large, high-quality insulin crystals by using a temperature change as the sole means to affect protein solubility and thus, crystallization. The facility consists of cylinders/containers with volumes of 500, 200, 100, and 50 ml. Data from the three Shuttle flights demonstrated that larger, higher resolution crystals (as evidenced by x-ray diffraction data) were obtained from the microgravity experiments when compared to earth-grown crystals.

Growth of triglycine sulfate (TGS) crystals by solution technique

NASA Technical Reports Server (NTRS)

Lal, R. B.; Kroes, R. L.; Wilcox, W. R.

1982-01-01

The growth of crystals from solution is greatly influenced by buoyancy driven convection. In a low-g environment, convection is greatly suppressed and diffusion becomes the predominant mechanism for thermal and mass transport. An experiment to grow TGS crystals by solution technique during the orbital Spacelab III mission has been designed. Crystals are grown by a new and unique technique of extracting heat from the crystal through a sting. The cooling at the sting tip is responsible for the desired supersaturation near the growing crystal. Calculations indicate that the cooled sting technique for solution crystal growth is necessary in low-g to maintain a maximum growth rate of 1 mm/day. Results of groundbased work in support of the flight experiment are discussed.

Analytics of crystal growth in space

NASA Technical Reports Server (NTRS)

Wilcox, W. R.; Chang, C. E.; Shlichta, P. J.; Chen, P. S.; Kim, C. K.

1974-01-01

Two crystal growth processes considered for spacelab experiments were studied to anticipate and understand phenomena not ordinarily encountered on earth. Computer calculations were performed on transport processes in floating zone melting and on growth of a crystal from solution in a spacecraft environment. Experiments intended to simulate solution growth at micro accelerations were performed.

Fabrication and Characterization of Colloidal Crystal Thin Films

ERIC Educational Resources Information Center

Rodriguez, I.; Ramiro-Manzano, F.; Meseguer, F.; Bonet, E.

2011-01-01

We present a laboratory experiment that allows undergraduate or graduate students to get introduced to colloidal crystal research concepts in an interesting way. Moreover, such experiments and studies can also be useful in the field of crystallography or solid-state physics. The work concerns the growth of colloidal crystal thin films obtained…

Inhibitor-based validation of a homology model of the active-site of tripeptidyl peptidase II.

PubMed

De Winter, Hans; Breslin, Henry; Miskowski, Tamara; Kavash, Robert; Somers, Marijke

2005-04-01

A homology model of the active site region of tripeptidyl peptidase II (TPP II) was constructed based on the crystal structures of four subtilisin-like templates. The resulting model was subsequently validated by judging expectations of the model versus observed activities for a broad set of prepared TPP II inhibitors. The structure-activity relationships observed for the prepared TPP II inhibitors correlated nicely with the structural details of the TPP II active site model, supporting the validity of this model and its usefulness for structure-based drug design and pharmacophore searching experiments.

Viscosity measurements of crystallizing andesite from Tungurahua volcano (Ecuador).

PubMed

Chevrel, Magdalena Oryaëlle; Cimarelli, Corrado; deBiasi, Lea; Hanson, Jonathan B; Lavallée, Yan; Arzilli, Fabio; Dingwell, Donald B

2015-03-01

Viscosity has been determined during isothermal crystallization of an andesite from Tungurahua volcano (Ecuador). Viscosity was continuously recorded using the concentric cylinder method and employing a Pt-sheathed alumina spindle at 1 bar and from 1400°C to subliquidus temperatures to track rheological changes during crystallization. The disposable spindle was not extracted from the sample but rather left in the sample during quenching thus preserving an undisturbed textural configuration of the crystals. The inspection of products quenched during the crystallization process reveals evidence for heterogeneous crystal nucleation at the spindle and near the crucible wall, as well as crystal alignment in the flow field. At the end of the crystallization, defined when viscosity is constant, plagioclase is homogeneously distributed throughout the crucible (with the single exception of experiment performed at the lowest temperature). In this experiments, the crystallization kinetics appear to be strongly affected by the stirring conditions of the viscosity determinations. A TTT (Time-Temperature-Transformation) diagram illustrating the crystallization "nose" for this andesite under stirring conditions and at ambient pressure has been constructed. We further note that at a given crystal content and distribution, the high aspect ratio of the acicular plagioclase yields a shear-thinning rheology at crystal contents as low as 13 vol %, and that the relative viscosity is higher than predicted from existing viscosity models. These viscosity experiments hold the potential for delivering insights into the relative influences of the cooling path, undercooling, and deformation on crystallization kinetics and resultant crystal morphologies, as well as their impact on magmatic viscosity.

Viscosity measurements of crystallizing andesite from Tungurahua volcano (Ecuador)

PubMed Central

Cimarelli, Corrado; deBiasi, Lea; Hanson, Jonathan B.; Lavallée, Yan; Arzilli, Fabio; Dingwell, Donald B.

2015-01-01

Abstract Viscosity has been determined during isothermal crystallization of an andesite from Tungurahua volcano (Ecuador). Viscosity was continuously recorded using the concentric cylinder method and employing a Pt‐sheathed alumina spindle at 1 bar and from 1400°C to subliquidus temperatures to track rheological changes during crystallization. The disposable spindle was not extracted from the sample but rather left in the sample during quenching thus preserving an undisturbed textural configuration of the crystals. The inspection of products quenched during the crystallization process reveals evidence for heterogeneous crystal nucleation at the spindle and near the crucible wall, as well as crystal alignment in the flow field. At the end of the crystallization, defined when viscosity is constant, plagioclase is homogeneously distributed throughout the crucible (with the single exception of experiment performed at the lowest temperature). In this experiments, the crystallization kinetics appear to be strongly affected by the stirring conditions of the viscosity determinations. A TTT (Time‐Temperature‐Transformation) diagram illustrating the crystallization “nose” for this andesite under stirring conditions and at ambient pressure has been constructed. We further note that at a given crystal content and distribution, the high aspect ratio of the acicular plagioclase yields a shear‐thinning rheology at crystal contents as low as 13 vol %, and that the relative viscosity is higher than predicted from existing viscosity models. These viscosity experiments hold the potential for delivering insights into the relative influences of the cooling path, undercooling, and deformation on crystallization kinetics and resultant crystal morphologies, as well as their impact on magmatic viscosity. PMID:27656114

Crystal structure of a cytochrome P450 2B6 genetic variant in complex with the inhibitor 4-(4-chlorophenyl)imidazole at 2.0-A resolution.

PubMed

Gay, Sean C; Shah, Manish B; Talakad, Jyothi C; Maekawa, Keiko; Roberts, Arthur G; Wilderman, P Ross; Sun, Ling; Yang, Jane Y; Huelga, Stephanie C; Hong, Wen-Xu; Zhang, Qinghai; Stout, C David; Halpert, James R

2010-04-01

The structure of the K262R genetic variant of human cytochrome P450 2B6 in complex with the inhibitor 4-(4-chlorophenyl)imidazole (4-CPI) has been determined using X-ray crystallography to 2.0-A resolution. Production of diffraction quality crystals was enabled through a combination of protein engineering, chaperone coexpression, modifications to the purification protocol, and the use of unique facial amphiphiles during crystallization. The 2B6-4-CPI complex is virtually identical to the rabbit 2B4 structure bound to the same inhibitor with respect to the arrangement of secondary structural elements and the placement of active site residues. The structure supports prior P450 2B6 homology models based on other mammalian cytochromes P450 and is consistent with the limited site-directed mutagenesis studies on 2B6 and extensive studies on P450 2B4 and 2B1. Although the K262R genetic variant shows unaltered binding of 4-CPI, altered binding affinity, kinetics, and/or product profiles have been previously shown with several other ligands. On the basis of new P450 2B6 crystal structure and previous 2B4 structures, substitutions at residue 262 affect a hydrogen-bonding network connecting the G and H helices, where subtle differences could be transduced to the active site. Docking experiments indicate that the closed protein conformation allows smaller ligands such as ticlopidine to bind to the 2B6 active site in the expected orientation. However, it is unknown whether 2B6 undergoes structural reorganization to accommodate bulkier molecules, as previously inferred from multiple P450 2B4 crystal structures.

Studies on the in vitro and in vivo antiurolithic activity of Holarrhena antidysenterica

PubMed Central

Khan, Aslam; Khan, Saeed R.; Gilani, Anwar H.

2013-01-01

Background Holarrhena antidysenterica has a traditional use in the treatment of urolithiasis, therefore, its crude extract has been investigated for possible antiurolithic effect. Materials and methods The crude aqueous-methanolic extract of Holarrhena antidysenterica (Ha.Cr) was studied using the in vitro and in vivo methods. Results In the in vitro experiments, Ha.Cr demonstrated a concentration-dependent (0.25–4 mg/ml) inhibitory effect on the slope of aggregation. It decreased the size of crystals and transformed the calcium oxalate monohydrate (COM) to calcium oxalate dehydrate (COD) crystals, in calcium oxalate metastable solutions. It also showed concentration-dependent antioxidant effect against 2,2-diphenyl-1-picrylhydrazyl free radical (DPPH) free radicals and lipid peroxidation induced in rat kidney tissue homogenate. Ha.Cr (0.3 mg/ml) reduced (p < 0.05) the cell toxicity and LDH release in renal epithelial cells (MDCK) exposed to oxalate (0.5 mM) and COM (66 μg/cm2) crystals. In male Wistar rats, receiving 0.75% ethylene glycol (EG) for 21 days along with 1% ammonium chloride (AC) in drinking water, Ha.Cr treatment (30–100 mg/kg) prevented the toxic changes caused by lithogenic agents; EG and AC, like loss of body weight, polyurea, oxaluria, raised serum urea and creatinine levels and crystal deposition in kidneys compared to their respective controls. Conclusion These data indicate that Holarrhena antidysenterica possesses antiurolithic activity, possibly mediated through inhibition of CaOx crystal aggregation, antioxidant and renal epithelial cell protective activities and may provide base for designing future studies to establish its efficacy and safety for clinical use. PMID:22622371

Experimental Study of Sr Partitioning into Calcite at Various Linear Growth Rates and Temperatures: Preliminary Results.

NASA Astrophysics Data System (ADS)

Gabitov, R. I.; Watson, B. E.

2004-05-01

The surface of a crystal in equilibrium with surrounding fluid can have a composition that differs from the bulk crystal. If growth rate of the crystal exceeds a minimum value at which partitioning-equilibrium can be maintained, then the crystal surface composition may be "captured" by the newly-formed lattice. The degree of this entrapment increases with increasing crystal growth rate. Non-equlibrium partitioning of Sr into calcite probably occurs by this entrapment mechanism. Sr and calcite are geochemically significant in understanding the thermal history of the ocean because the substitution of Sr for Ca in calcite is temperature dependent. To improve our understanding of the partitioning of Sr into calcite, we conducted two different types of experiment: 1) calcite growth from Sr-bearing solution with analysis of the crystal cross-section by electron microprobe (bulk crystal-liquid runs); and 2) treatment of calcite cleavage surfaces with Sr-bearing solutions and examination of the top few nm surface layer by X-ray photoelectron spectroscopy (surface-liquid runs). In the series of bulk-liquid experiments crystals were grown by three different procedures: 1) precipitation on glass slide (pre-coated with calcite), where a steady flow of CaCl2 - SrCl2 and Na2CO3 solutions were mixed just before passage through a tube and allowed to drip onto a slide ("cave"-type experiments, ionic strength I=0.01); 2) growth from a CaCl2 - NH4Cl - SrCl2 solution by diffusion of CO2 from an ammonium carbonate source ("drift" experiments, I=0.52); 3) coarsening of small calcite crystals in the CaCO3-SrCO3-NaCl-H2O system at 800-950° C and 0.5-1 kb in a cold seal apparatus. The growth rate of individual crystals was determined by periodic monitoring of crystal size with time or roughly by comparison of final size with duration of the experiment. Surface-liquid experiments were performed by treatment of cleavage surfaces of natural calcite fragments in a Sr(ClO4)2 solution for 1 minute. After treatment the remaining solution was blown out by a stream of nitrogen to preclude the precipitation of Sr phase. We observed that the precipitated calcite crystals can be very different in size even if the runs have the same input rate of calcite components. The cave-type and cold-seal runs yielded 15-40 μ m calcites, but in the drift experiments crystal size varied between 60 μ m and 1 mm. Electron microprobe analysis across the large crystals show that the concentration of Sr is higher in the center and decreases toward the edge. This is probably due to the cube-root dependence of radial growth on the volume change of the growing crystals. Like previous workers who measured bulk uptake of Sr as a function of precipitation rate, we observed that increased growth rate (V, nm/s) enhances Sr uptake into the crystal, raising Kdbulk/liquid=(Sr/Ca)bulk/(Sr/Ca)liquid. Kdbulk/liquid = 0.03 to 0.06 when log(V)=-1.1 to -0.6 at 25° C in the cave-type runs (I=0.01). At higher ionic strength (I=0.52) and T=55° C, Kdbulk/liquid=0.11 to 0.15 when log(V)=-0.6 to 0.4 in the drift experiments. XPS analysis of surface-liquid experiments yielded higher Kdsurface/liquid=(Sr/Ca)surface/(Sr/Ca)liquid values compared with Kdbulk/liquid. This combined evidence supports the idea that Sr is enriched at the calcite surface relative to the bulk crystal during crystal growth.

Silica crystals and aluminum salts mediate NALP-3 inflammasome activation via phagosomal destabilization

PubMed Central

Hornung, Veit; Bauernfeind, Franz; Halle, Annett; Samstad, Eivind O.; Kono, Hajime; Rock, Kenneth L.; Fitzgerald, Katherine A.; Latz, Eicke

2010-01-01

Inhalation of silica crystals causes inflammation in the alveolar space. Prolonged silica exposure can lead to the development of silicosis, an irreversible, fibrotic pulmonary disease. The mechanisms by which silica and other crystals activate immune cells are not well understood. Here, we demonstrate that silica and aluminum salt crystals activate the NALP3 inflammasome. NALP3 activation requires crystal phagocytosis and crystal uptake leads to lysosomal damage and rupture. Sterile lysosomal damage is also sufficient to induce NALP3 activation and inhibition of phagosomal acidification or cathepsin B impairs NALP3 activation. These results indicate that the NALP3 inflammasome can sense lysosomal damage induced by various means as an endogenous danger signal. PMID:18604214

Isothermal Analysis of the Crystallization Kinetics in Lithium Disilicate Glass using Trans Temp Furnace

NASA Technical Reports Server (NTRS)

Fuss, T.; Ray, C. S.; Day, D. E.

2006-01-01

Crystallization kinetics for lithium disilicate, Li2O2SiO2, (LS2) glass has been studied extensively by nonisothermal methods, but only a few studies on the isothermal crystallization kinetics of LS2 are available. In the present research, isothermal crystallization experiments or the LS2 glass were conducted in a Trans Temp furnace between 600 and 635 C, and selected properties such as the activation energy for crystallization (E), crystal growth index or Avrami parameter (n), the concentration of quenched-in nuclei in the starting glass (Ni) and the crystal nucleation rate (I) were measured. The crystal nucleation rate (I) was measured at only one selected temperature of 452 C, at this time. This commercial furnace has a 13 cm long isothermal heating zone (+/- 1 C) that allows precise heat treatment of relatively large samples. By placing a thermocouple within approx. 2 mm of the sample, it was possible to detect the heat of crystallization in the form of an isothermal crystallization exotherm during isothermal heat treatment of the sample. The values of E (318 plus or minus 10 kJ/mol), n (3.6 plus or minus 0.l), and N(sub i) (1.6 x 10(exp l2) m(sup -3)) calculated by analyzing these isotherms using the standard Johnson-Mehl-Avrami (JMA) equation were reproducible and in agreement with the literature values. The value of I, 1.9 x 10(exp 10) m(sup -3) s(sup -1) at 452 C, is an order of magnitude higher than the reported value for LS2.

Protein crystal growth results from shuttle flight 51-F

NASA Technical Reports Server (NTRS)

Bugg, C. E.

1985-01-01

The protein crystal growth (PCG) experiments run on 51-F were analyzed. It was found that: (1) sample stability is increased over that observed during the experiments on flight 51-D; (2) the dialysis experiments produced lysozyme crystals that were significantly larger than those obtained in our identical ground-based studies; (3) temperature fluctuations apparently caused problems during the crystallization experiments on 51-F; (4) it is indicated that teflon tape stabilizes droplets on the syringe tips; (5) samples survived during the reentry and landing in glass tips that were not stoppered with plungers; (6) from the ground-based studies, it was expected that equilibration should be complete within 2 to 4 days for all of these vapor-diffusion experiments, thus it appears that the vapor diffusion rates are somewhat slower under microgravity conditions; (7) drop tethering was highly successful, all four of the tethered drops were stable, even though they contained MPD solutions; (8) the PCG experiments on 51-F were done to assess the hardware and experimental procedures that are developed for future flights, when temperature control will be available. Lysozyme crystals obtained by microdialysis are considerably larger than those obtained on the ground, using the identical apparatus and procedures.

Spontaneous pairing and cooperative movements of micro-particles in a two dimensional plasma crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhdanov, S. K.; Couëdel, L., E-mail: lenaic.couedel@univ-amu.fr; Nosenko, V.

2015-05-15

In an argon plasma of 20 W rf discharge at a pressure of 1.38 Pa, a stable highly ordered monolayer of microparticles is suspended. We observe spontaneous particle pairing when suddenly reducing the gas pressure. Special types of dynamical activity, in particular, entanglement and cooperative movements of coupled particles have been registered. In the course of the experiment first appeared single vertical pairs of particles, in further they gradually accumulated causing melting of the entire crystal. To record pairing events, the particle suspension is side-view imaged using a vertically extended laser sheet. The long-lasting pre-melting phase assured the credible recording and identificationmore » of isolated particle pairs. The high monolayer charge density is crucial to explain the spontaneous pairing events observed in our experiments as the mutual repulsion between the particles comprising the monolayer make its vertical extend thicker.« less

Te-and Zn-Doped InSb Crystals Grown in Microgravity

NASA Technical Reports Server (NTRS)

Ostrogorsky, A. G.; Marin, C.; Volz, M.; Bonner, W. A.; Duffar, T.

2004-01-01

In 2002, within the SUBSA (Solidification Using a Baffle in Sealed Ampoules) investigation, seven doped InSb crystals were grown in microgravity at the International Space Station. The key goals of the SUBSA investigation are: (a) to clarify the origin of the melt convection in space laboratories; (b) to reduce melt convection to the level which allows reproducible diffusion-controlled segregation; (e) to explore the submerged baffle process and liquid encapsulation in microgravity. 30 crystal growth experiments were conducted in the ground unit, to optimize the design of flight ampoules and to test the transparent SUBSA furnace developed by TecMasters Inc. The specially designed furnace, allowed observation of the crystal growth process (melting, seeding, motion of the solid-liquid interface, etc.). In the summer of 2002, eight crystal growth experiments were conducted in the Microgravity Science Glovebox (MSG) facility at the ISS. Four Te-doped (k = 0.5) and three Zn-doped (k2.9) crystals were grown on undoped seeds. In one experiment, we were not able to seed and grow. The seven grown crystals were sectioned and analyzed using SIMS. The design of the SUBSA ampoules, the segregation data and the video images obtained during the SUBSA flight experiments will be presented and discussed.

Syncom 4 deploy, LDEF retrieval highlight 10-day Columbia flight

NASA Technical Reports Server (NTRS)

1989-01-01

The objectives of Space Shuttle Mission STS-32 are described along with major flight activities, prelaunch and launch operations, trajectory sequence of events, and landing and post-landing operations. The primary objectives of STS-32 are the deployment of a Navy synchronous communications satellite (Syncom 4) and the retrieval of the Long Duration Exposure Facility (LDEF) launched from the Challenger in April 1984. Secondary STS-32 payloads include a protein crystal growth experiment, the Fluids Experiment Apparatus (FEA) for the investigation of microgravity materials processing, the Mesoscale Lighting Experiment, the Latitude-Longitude Locator Experiment, the Americal Flight Echocardiograph, and an experiment to investigate neurospora circadian rhythms in a microgravity environment.

Topological Defects in a Living Nematic Ensnare Swimming Bacteria

NASA Astrophysics Data System (ADS)

Genkin, Mikhail M.; Sokolov, Andrey; Lavrentovich, Oleg D.; Aranson, Igor S.

2017-01-01

Active matter exemplified by suspensions of motile bacteria or synthetic self-propelled particles exhibits a remarkable propensity to self-organization and collective motion. The local input of energy and simple particle interactions often lead to complex emergent behavior manifested by the formation of macroscopic vortices and coherent structures with long-range order. A realization of an active system has been conceived by combining swimming bacteria and a lyotropic liquid crystal. Here, by coupling the well-established and validated model of nematic liquid crystals with the bacterial dynamics, we develop a computational model describing intricate properties of such a living nematic. In faithful agreement with the experiment, the model reproduces the onset of periodic undulation of the director and consequent proliferation of topological defects with the increase in bacterial concentration. It yields a testable prediction on the accumulation of bacteria in the cores of +1 /2 topological defects and depletion of bacteria in the cores of -1 /2 defects. Our dedicated experiment on motile bacteria suspended in a freestanding liquid crystalline film fully confirms this prediction. Our findings suggest novel approaches for trapping and transport of bacteria and synthetic swimmers in anisotropic liquids and extend a scope of tools to control and manipulate microscopic objects in active matter.

Decades of Data: Extracting Trends from Microgravity Crystallization History

NASA Technical Reports Server (NTRS)

Judge, R. A.; Snell, E. H.; Kephart, R.; vanderWoerd, M.

2004-01-01

The reduced acceleration environment of an orbiting spacecraft has been proposed as an ideal environment for biological crystal growth as the first sounding rocket flight in 1981 many crystallization experiments have flown with some showing improvement and others not. To further explore macromolecule crystal improvement in microgravity we have accumulated data from published reports and reports submitted by 63 missions including the Space Shuttle program, unmanned satellites, the Russian Space Station MIR and sounding rocket experiments. While it is not at this point in time a comprehensive record of all flight crystallization experimental results, there is however sufficient information for emerging trends to be identified. In this study the effects of the acceleration environment, the techniques of crystallization, sample molecular weight and the response of individual macromolecules to microgravity crystallization will be investigated.

Application Of Empirical Phase Diagrams For Multidimensional Data Visualization Of High Throughput Microbatch Crystallization Experiments.

PubMed

Klijn, Marieke E; Hubbuch, Jürgen

2018-04-27

Protein phase diagrams are a tool to investigate cause and consequence of solution conditions on protein phase behavior. The effects are scored according to aggregation morphologies such as crystals or amorphous precipitates. Solution conditions affect morphological features, such as crystal size, as well as kinetic features, such as crystal growth time. Common used data visualization techniques include individual line graphs or symbols-based phase diagrams. These techniques have limitations in terms of handling large datasets, comprehensiveness or completeness. To eliminate these limitations, morphological and kinetic features obtained from crystallization images generated with high throughput microbatch experiments have been visualized with radar charts in combination with the empirical phase diagram (EPD) method. Morphological features (crystal size, shape, and number, as well as precipitate size) and kinetic features (crystal and precipitate onset and growth time) are extracted for 768 solutions with varying chicken egg white lysozyme concentration, salt type, ionic strength and pH. Image-based aggregation morphology and kinetic features were compiled into a single and easily interpretable figure, thereby showing that the EPD method can support high throughput crystallization experiments in its data amount as well as its data complexity. Copyright © 2018. Published by Elsevier Inc.

The mechanisms of fine particle generation and electrification during Mount St. Helens volcanic eruption

NASA Technical Reports Server (NTRS)

Cheng, R. J.

1982-01-01

Microscopical investigation of volcanic ash collected from ground stations during Mount St. Helens eruptions reveal a distinctive bimodel size distribution with high concentrations of particle ranges at (1) 200-100 microns and (2) 20-0.1 microns. Close examination of individual particles shows that most larger ones are solidified magma particles of porous pumice with numerous gas bubbles in the interior and the smaller ones are all glassy fragments without any detectable gas bubbles. Elemental analysis demonstrates that the fine fragments all have a composition similar to that of the larger pumice particles. Laboratory experiments suggest that the formation of the fine fragments is by bursting of glassy bubbles from a partially solidified surface of a crystallizing molten magma particle. The production of gas bubbles is due to the release of absorbed gases in molten magma particles when solubility decreases during phase transition. Diffusion cloud chamber experiments strongly indicate that sub-micron volcanic fragments are highly hygroscopic and extremely active as cloud condensation nuclei. Ice crystals also are evidently formed on those fragments in a supercooled (-20 C) cloud chamber. It has been reported that charge generation from ocean volcanic eruptions is due to contact of molten lava with sea water. This seems to be insufficient to explain the observed rapid and intense lightning activities over Mount St. Helens eruptions. Therefore, a hypothesis is presented here that highly electrically charged fine solid fragments are ejected by bursting of gas bubbles from the surface of a crystallizing molten magma particles.

Nucleation, crystallization, and melting of atactic polystyrene

NASA Astrophysics Data System (ADS)

Chai, Yu; Forrest, James

Here we present the study of using low molecular weight atactic polystyrene (aPS) as the model system to understand the nucleation, crystallization, and meting behaviors of the stereo-regular polymer chains in aPS. The result is consistent with the theoretical calculation proposed by Semenov. In addition, both the crystallization and melting experiments indicate that all crystals are on or near the surface. Finally, the nucleation experiment below the glass transition temperature provides another piece of evidence of the enhanced surface dynamics in glassy polymers.

Packaging consideration of two-dimensional polymer-based photonic crystals for laser beam steering

NASA Astrophysics Data System (ADS)

Dou, Xinyuan; Chen, Xiaonan; Chen, Maggie Yihong; Wang, Alan Xiaolong; Jiang, Wei; Chen, Ray T.

2009-02-01

In this paper, we report the theoretical study of polymer-based photonic crystals for laser beam steering which is based on the superprism effect as well as the experiment fabrication of the two dimensional photonic crystals for the laser beam steering. Superprism effect, the principle for beam steering, was separately studied in details through EFC (Equifrequency Contour) analysis. Polymer based photonic crystals were fabricated through double exposure holographic interference method using SU8-2007. The experiment results were also reported.

Contortionist bubbles in andesitic enclaves: implications for gas migration and phase segregation in crystal-rich magmas.

NASA Astrophysics Data System (ADS)

Oppenheimer, J. C.; Cashman, K. V.; Rust, A.; Dobson, K. J.; Bacon, C. R.; Dingwell, D. B.

2016-12-01

In order to constrain gas migration behaviors in crystal-rich magmas, we compare results of analogue experiments to frozen structures in andesitic enclaves. In the analogue experiments air was injected into mixtures of syrup and particles sandwiched between glass plates. We observed a significant increase in bubble deformation and coalescence when particle fractions increased beyond a critical value (the random loose packing). At high particle fractions, bubble growth re-organized (compacted) the particles adjacent to the bubble walls. This caused liquid segregation into patches within the particle suspension and into large void spaces near the outer edge of experiments. We compare these experiments to void morphologies in a 58 x 70 x 73 cm andesitic enclave from silicic-andesite lava flows of Mt Mazama, Oregon (Bacon, 1986). This enclave is zoned, with a vesicle-rich center and a glass-rich rim, suggesting gas-driven melt segregation from the center to the rim. We use both 2D (optical microscopy and SEM) and 3D (X-ray tomography) techniques to image crystal textures and bubble shapes. The center of the enclave bears scattered patches of groundmass in the main phenocryst framework. These patches are similar to those observed in experiments, and thus melt segregation in the enclave may have occurred both toward the rim and toward these patches. Bubble morphologies reveal two main types of bubbles. (1) Lobate and finger-like bubbles, similar to the deformed bubbles in experiments, are found exclusively in the groundmass patches. They are also often associated with compacted crystal structures at the bubble walls. (2) Diktytaxitic textures - angular bubbles flattened against phenocrysts - are abundant in the crystal networks. These voids are entirely connected in 3D and formed the gas-rich center of the enclave. They likely represent a gas migration regime where the expanding gas front cannot deform the crystal structure but instead invades the pore-space between crystals, pushing out residual melt (filter pressing). The switch between regimes appears to depend on crystal size and aspect ratio. The similar features between bubbles in the enclave and in experiments are encouraging, and suggest that crystal-induced bubble deformation, and gas-driven melt segregation, may be common in crystal-rich magmas.

On the equivalence between Young's double-slit and crystal double-refraction interference experiments.

PubMed

Ossikovski, Razvigor; Arteaga, Oriol; Vizet, Jérémy; Garcia-Caurel, Enric

2017-08-01

We show, both analytically and experimentally, that under common experimental conditions the interference pattern produced in a classic Young's double-slit experiment is indistinguishable from that generated by means of a doubly refracting uniaxial crystal whose optic axis makes a skew angle with the light propagation direction. The equivalence between diffraction and crystal optics interference experiments, taken for granted by Arago and Fresnel in their pioneering research on the interference of polarized light beams, is thus rigorously proven.

Effect of water on olivine single crystals plasticity, deformed under high pressure and high temperature

NASA Astrophysics Data System (ADS)

Girard, Jennifer

The Earth's upper mantle, mainly composed of olivine, is seismically anisotropic. Seismic anisotropy attenuation has been observed at 220km depth. Karato et al. (1992) attributed this attenuation to a transition between two deformation mechanisms, from dislocation creep above 220km to diffusion creep below 220km, induced by a change in water content. Couvy (2005) and Mainprice et al. (2005) predicted a change in Lattice Preferred Orientation induced by pressure, which comes from a change of slip system, from [100] slip to [001] slip, and is responsible for the seismic anisotropy attenuation. Raterron et al. (2007) ran single crystal deformation experiments under anhydrous conditions and observed that the slip system transition occurs around 8GPa, which corresponds to a depth of 260Km. Experiments were done to quantify the effects of water on olivine single crystals deformed using D-DIA press and synchrotron beam. Deformations were carried out in uniaxial compression along [110]c, [011]c, and [101]c, crystallographic directions, at pressure ranging from 4 to 8GPa and temperature between 1373 and 1473K. Talc sleeves about the annulus of the single crystals were used as source of water in the assembly. Stress and specimen strain rates were calculated by in-situ X-ray diffraction and time resolved imaging, respectively. By direct comparison of single crystals strain rates, we observed that [110]c deforms faster than [011]c below 5GPa. However above 6GPa [011]c deforms faster than [110]c. This revealed that [100](010) is the dominant slip system below 5GPa, and above 6GPa [001](010) becomes dominant. According to our results, the slip system transition, which is induced by pressure, occurs at 6GPa. Water influences the pressure where the switch over occurs, by lowering the transition pressure. The pressure effect on the slip systems activity has been quantified and the hydrolytic weakening has also been estimated for both orientations. Data also shows that temperature affects the slip system activity. The regional variation of the depth for the seismic anisotropy attenuation, which would depend on local hydroxyl content and temperature variations and explains the seismic anisotropy attenuation occurring at about 220Km depth in the mantle, where the pressure is about 6GPa. Deformation of MgO single crystal oriented [100], [110] and [111] were also performed. The results predict a change in the slip system activity at 23GPa, again induced by pressure. This explains the seismic anisotropy observed in the lower mantle.

Purification, crystallization and preliminary X-ray analysis of Enterococcus faecium aminoglycoside-2′′-phosphotransferase-Ib [APH(2′′)-Ib

DOE Office of Scientific and Technical Information (OSTI.GOV)

Walanj, Rupa; Young, Paul; Baker, Heather M.

2005-04-01

APH(2′′)-Ib is an enzyme responsible for high-level gentamicin resistance in E. faecium isolates. Native crystals of this enzyme have been prepared and preliminary X-ray diffraction experiments have been undertaken. Bacterial resistance to the aminoglycoside antibiotics is primarily the result of deactivation of the drugs. Three families of enzymes are responsible for this activity, with one such family being the aminoglycoside phosphotransferases (APHs). The gene encoding one of these enzymes, APH(2′′)-Ib, has been cloned and the protein (comprising 299 amino-acid residues) expressed in Escherichia coli, purified and crystallized in the presence of 16%(w/v) PEG 3350 and gentamicin. The crystals belong tomore » the monoclinic space group P2{sub 1}, with approximate unit-cell parameters a = 79.7, b = 58.8, c = 81.4 Å, β = 98.4°, and preliminary X-ray diffraction analysis is consistent with the presence of two molecules in the asymmetric unit. Synchrotron diffraction data to approximately 2.65 Å resolution were collected from a native APH(2′′)-Ib crystal at beamline BL9-2 at SSRL (Stanford, CA, USA). Selenium-substituted crystals have also been produced and structure determination is proceeding.« less

Rheological flow laws for multiphase magmas: An empirical approach

NASA Astrophysics Data System (ADS)

Pistone, Mattia; Cordonnier, Benoît; Ulmer, Peter; Caricchi, Luca

2016-07-01

The physical properties of magmas play a fundamental role in controlling the eruptive dynamics of volcanoes. Magmas are multiphase mixtures of crystals and gas bubbles suspended in a silicate melt and, to date, no flow laws describe their rheological behaviour. In this study we present a set of equations quantifying the flow of high-viscosity (> 105 Pa·s) silica-rich multiphase magmas, containing both crystals (24-65 vol.%) and gas bubbles (9-12 vol.%). Flow laws were obtained using deformation experiments performed at high temperature (673-1023 K) and pressure (200-250 MPa) over a range of strain-rates (5 · 10- 6 s- 1 to 4 · 10- 3 s- 1), conditions that are relevant for volcanic conduit processes of silica-rich systems ranging from crystal-rich lava domes to crystal-poor obsidian flows. We propose flow laws in which stress exponent, activation energy, and pre-exponential factor depend on a parameter that includes the volume fraction of weak phases (i.e. melt and gas bubbles) present in the magma. The bubble volume fraction has opposing effects depending on the relative crystal volume fraction: at low crystallinity bubble deformation generates gas connectivity and permeability pathways, whereas at high crystallinity bubbles do not connect and act as ;lubricant; objects during strain localisation within shear bands. We show that such difference in the evolution of texture is mainly controlled by the strain-rate (i.e. the local stress within shear bands) at which the experiments are performed, and affect the empirical parameters used for the flow laws. At low crystallinity (< 44 vol.%) we observe an increase of viscosity with increasing strain-rate, while at high crystallinity (> 44 vol.%) the viscosity decreases with increasing strain-rate. Because these behaviours are also associated with modifications of sample textures during the experiment and, thus, are not purely the result of different deformation rates, we refer to ;apparent shear-thickening; and ;apparent shear-thinning; for the behaviours observed at low and high crystallinity, respectively. At low crystallinity, increasing deformation rate favours the transfer of gas bubbles in regions of high strain localisation, which, in turn, leads to outgassing and the observed increase of viscosity with increasing strain-rate. At high crystallinity gas bubbles remain trapped within crystals and no outgassing occurs, leading to strain localisation in melt-rich shear bands and to a decrease of viscosity with increasing strain-rate, behaviour observed also in crystal-bearing suspensions. Increasing the volume fraction of weak phases induces limited variation of the stress exponent and pre-exponential factor in both apparent shear-thickening and apparent shear-thinning regimes; conversely, the activation energy is strongly dependent on gas bubble and melt volume fractions. A transient rheology from apparent shear-thickening to apparent shear-thinning behaviour is observed for a crystallinity of 44 vol.%. The proposed equations can be implemented in numerical models dealing with the flow of crystal- and bubble-bearing magmas. We present results of analytical simulations showing the effect of the rheology of three-phase magmas on conduit flow dynamics, and show that limited bubble volumes (< 10 vol.%) lead to strain localisation at the conduit margins during the ascent of crystal-rich lava domes and crystal-poor obsidian flows.

Comparing olivine single crystal and polycrystal rheology: evidence for supplementary accommodation mechanisms at grain boundaries

NASA Astrophysics Data System (ADS)

Bollinger, C.; Merkel, S.; Raterron, P.; Castelnau, O.; Detrez, F.

2013-12-01

Rheology in the Earth's upper-mantle is mostly constrained by the plastic properties of olivine. Over recent years, several groups have been carrying out deformation experiments on single crystals and polycrystals of olivine at upper mantle pressure (P) and temperature (T). Yet, the rheology of olivine at mantle conditions is still not well constrained. We carried out deformation experiments on San Carlos olivine polycrystals, at P and T ranging from 3 to 8 GPa and 1373 to 1673 K, respectively, and at strain rates ranging from 10-6 to 10-4 s-1, using the D-DIA apparatus installed at the NSLS X17B2 beamline (NY, USA). The deformation rates of the polycrystals are compared to those of single crystals oriented along the soft orientations [110]c, [011]c, [101]c which activate the easiest slip systems (Raterron et al., 2012). This comparison suggests that, in olivine polycrystals deforming in the dislocation creep regime, other relaxation mechanisms need to be considered to account for the observed polycrystal strain rates. This highlights the importance of supplementary mechanisms, such as those occurring at grain boundaries, to properly model olivine aggregates plasticity.

ANAIS: Status and prospects

NASA Astrophysics Data System (ADS)

Amaré, J.; Cebrián, S.; Cuesta, C.; García, E.; Ginestra, C.; Martínez, M.; Oliván, M. A.; Ortigoza, Y.; Ortiz de Solórzano, A.; Pobes, C.; Puimedón, J.; Sarsa, M. L.; Villar, J. A.; Villar, P.

2016-04-01

ANAIS (Annual modulation with NAI Scintillators) experiment aims to look for dark matter annual modulation with 250 kg of ultra-pure NaI(Tl) scintillators at the Canfranc Underground Laboratory (LSC), in order to confirm the DAMA/LIBRA positive signal in a model-independent way. The detector will consists in an array of close-packed single modules, each of them coupled to two high efficiency Hamamatsu photomultipliers. Two 12.5 kg each NaI(Tl) crystals provided by Alpha Spectra are currently taking data at the LSC. These modules have shown an outstanding light collection efficiency (12-16 phe/keV), about the double of that from DAMA/LIBRA phase 1 detectors, which could enable reducing the energy threshold down to 1 keVee. ANAIS crystal radiopurity goals are fulfilled for 232Th and 238U chains, assuming equilibrium, and in the case of 40K, present crystals activity (although not at the required 20 ppb level) could be acceptable. However, a 210Pb contamination out-of-equilibrium has been identified and its origin traced back, so we expect it will be avoided in next prototypes. Finally, current status and prospects of the experiment considering several exposure and background scenarios are presented.

IR Sensor Synchronizing Active Shutter Glasses for 3D HDTV with Flexible Liquid Crystal Lenses

PubMed Central

Han, Jeong In

2013-01-01

IR sensor synchronizing active shutter glasses for three-dimensional high definition television (3D HDTV) were developed using a flexible liquid crystal (FLC) lens. The FLC lens was made on a polycarbonate (PC) substrate using conventional liquid crystal display (LCD) processes. The flexible liquid crystal lens displayed a maximum transmission of 32% and total response time of 2.56 ms. The transmittance, the contrast ratio and the response time of the flexible liquid crystal lens were superior to those of glass liquid crystal lenses. Microcontroller unit and drivers were developed as part of a reception module with power supply for the IR sensor synchronizing active shutter glasses with the flexible liquid crystal lens prototypes. IR sensor synchronizing active shutter glasses for 3D HDTV with flexible liquid crystal lenses produced excellent 3D images viewing characteristics.

Crystal methamphetamine smoking among regular ecstasy users in Australia: increases in use and associations with harm.

PubMed

Kinner, Stuart A; Degenhardt, Louisa

2008-05-01

This study examined (a) changes in crystal methamphetamine use among regular ecstasy users (REU) in Australia and (b) associations of crystal use and smoking with demographics, drug use and harm. Cross-sectional surveys (2000-06) of REU in three Australian capital cities, and in 2006, 750 REU in all Australian capital cities. The interview included: demographics, drug use, risk behaviour, recent criminal activity and methamphetamine dependence using Severity of Dependence Scale. There was little change in overall methamphetamine use, but a marked increase in crystal methamphetamine smoking. Among recent methamphetamine users in 2006 (n = 606), crystal methamphetamine users (n = 364) reported more frequent methamphetamine use and higher levels of dependence. Compared with those who had used only other forms of methamphetamine, recent crystal methamphetamine users were more likely to 'binge' on drugs for > or = 48 hours, engage in crime and experience financial and legal problems related to drug use. Non-smoking crystal methamphetamine users (n = 78) more often reported recent injecting and heroin use. Recent smokers were more likely to have: greater polydrug use, recently overdosed on a 'party drug', and accessed medical services for their drug use. Many of these associations were accounted for by their injecting and heavier methamphetamine use, rather than smoking per se. Crystal methamphetamine smoking among REU has increased markedly and is associated with significant harm. This appears related to smokers' heavier levels of methamphetamine use. Effective harm reduction strategies should be tailored to these specific risks.

Paths to light trapping in thin film GaAs solar cells.

PubMed

Xiao, Jianling; Fang, Hanlin; Su, Rongbin; Li, Kezheng; Song, Jindong; Krauss, Thomas F; Li, Juntao; Martins, Emiliano R

2018-03-19

It is now well established that light trapping is an essential element of thin film solar cell design. Numerous light trapping geometries have already been applied to thin film cells, especially to silicon-based devices. Less attention has been paid to light trapping in GaAs thin film cells, mainly because light trapping is considered less attractive due to the material's direct bandgap and the fact that GaAs suffers from strong surface recombination, which particularly affects etched nanostructures. Here, we study light trapping structures that are implemented in a high-bandgap material on the back of the GaAs active layer, thereby not perturbing the integrity of the GaAs active layer. We study photonic crystal and quasi-random nanostructures both by simulation and by experiment and find that the photonic crystal structures are superior because they exhibit fewer but stronger resonances that are better matched to the narrow wavelength range where GaAs benefits from light trapping. In fact, we show that a 1500 nm thick cell with photonic crystals achieves the same short circuit current as an unpatterned 4000 nm thick cell. These findings are significant because they afford a sizeable reduction in active layer thickness, and therefore a reduction in expensive epitaxial growth time and cost, yet without compromising performance.

The study of electromagnetic wave propagation in photonic crystals via planewave based transfer (scattering) matrix method with active gain material applications

NASA Astrophysics Data System (ADS)

Li, Ming

In this dissertation, a set of numerical simulation tools are developed under previous work to efficiently and accurately study one-dimensional (1D), two-dimensional (2D), 2D slab and three-dimensional (3D) photonic crystal structures and their defects effects by means of spectrum (transmission, reflection, absorption), band structure (dispersion relation), and electric and/or magnetic fields distribution (mode profiles). Further more, the lasing property and spontaneous emission behaviors are studied when active gain materials are presented in the photonic crystal structures. First, the planewave based transfer (scattering) matrix method (TMM) is described in every detail along with a brief review of photonic crystal history (Chapter 1 and 2). As a frequency domain method, TMM has the following major advantages over other numerical methods: (1) the planewave basis makes Maxwell's Equations a linear algebra problem and there are mature numerical package to solve linear algebra problem such as Lapack and Scalapack (for parallel computation). (2) Transfer (scattering) matrix method make 3D problem into 2D slices and link all slices together via the scattering matrix (S matrix) which reduces computation time and memory usage dramatically and makes 3D real photonic crystal devices design possible; and this also makes the simulated domain no length limitation along the propagation direction (ideal for waveguide simulation). (3) It is a frequency domain method and calculation results are all for steady state, without the influences of finite time span convolution effects and/or transient effects. (4) TMM can treat dispersive material (such as metal at visible light) naturally without introducing any additional computation; and meanwhile TMM can also deal with anisotropic material and magnetic material (such as perfectly matched layer) naturally from its algorithms. (5) Extension of TMM to deal with active gain material can be done through an iteration procedure with gain material expressed by electric field dependent dielectric constant. Next, the concepts of spectrum interpolation (Chapter 3), higher-order incident (Chapter 4) and perfectly matched layer (Chapter 5) are introduced and applied to TMM, with detailed simulation for 1D, 2D, and 3D photonic crystal examples. Curvilinear coordinate transform is applied to the Maxwell's Equations to study waveguide bend (Chapter 6). By finding the phase difference along propagation direction at various XY plane locations, the behaviors of electromagnetic wave propagation (such as light bending, focusing etc) can be studied (Chapter 7), which can be applied to diffractive optics for new devices design. Numerical simulation tools for lasing devices are usually based on rate equations which are not accurate above the threshold and for small scale lasing cavities (such as nano-scale cavities). Recently, we extend the TMM package function to include the capacity of dealing active gain materials. Both lasing (above threshold) and spontaneous emission (below threshold) can be studied in the frame work of our Gain-TMM algorithm. Chapter 8 will illustrate the algorithm in detail and show the simulation results for 3D photonic crystal lasing devices. Then, microwave experiments (mainly resonant cavity embedded at layer-by-layer woodpile structures) are performed at Chapter 9 as an efficient practical way to study photonic crystal devices. The size of photonic crystal under microwave region is at the order of centimeter which makes the fabrication easier to realize. At the same time due to the scaling property, the result of microwave experiments can be applied directly to optical or infrared frequency regions. The systematic TMM simulations for various resonant cavities are performed and consistent results are obtained when compared with microwave experiments. Besides scaling the experimental results to much smaller wavelength, designing potential photonic crystal devices for application at microwave is also an interesting and important topic. Finally, we describe the future development of TMM algorithm such as using localized functions as basis to more efficiently simulate disorder problems (Chapter 10). Future applications of photonic crystal concepts are also discussed at Chapter 10. Along with this dissertation, TMM Photonic Crystal Package User Manual and Gain TMM Photonic Crystal Package User Manual written by me, Dr. Jiangrong Cao (Canon USA) and Dr. Xinhua Hu (Ames Lab) focus more on the programming detail, software user interface, trouble shooting, and step-by-step instructions. This dissertation and the two user manuals are essential documents for TMM software package beginners and advanced users. Future software developments, new version releases and FAQs can be tracked through my web page: http://www.public.iastate.edu/~mli/ In summary, this dissertation has extended the planewave based transfer (scattering) matrix method in many aspects which make the TMM and Gain-TMM software package a powerful simulation tool in photonic crystal study. Comparisons of TMM and GTMM results with other published numerical results and experimental results indicate that TMM and GTMM is accurate and highly efficient in photonic crystal device simulation and design. (Abstract shortened by UMI.)

Survey Analysis of Materials Processing Experiments Aboard STS-47: Spacelab J

NASA Technical Reports Server (NTRS)

Sharpe, R. J.; Wright, M. D.

2009-01-01

This Technical Memorandum (TM) is a survey outline of materials processing experiments aboard Space Shuttle Mission STS-47: Spacelab J, a joint venture between NASA and the National Space Development Agency of Japan. The mission explored materials processing experiments including electronics and crystal growth materials, metals and alloys, glasses and ceramics, and fluids. Experiments covered include Growth of Silicone Spherical Crystals and Surface Oxidation, Growth Experiment of Narrow Band-Gap Semiconductor Lead-Tin-Tellurium Crystals in Space, Study on Solidification of Immiscible Alloys, Fabrication of Very-Low-Density, High-Stiffness Carbon Fiber/Aluminum Hybridized Composites, High Temperature Behavior of Glass, and Study of Bubble Behavior. The TM underscores the historical significance of these experiments in the context of materials processing in space.

Experiments with Cholesteric Liquid Crystals

ERIC Educational Resources Information Center

Fergason, James L.

1970-01-01

Describes laboratory experiments designed to demonstrate (1) the properties of cholesteric liquid crystals, (2) thermal mapping, (3) thermal diffusivity, (4) adiabatic expansion of rubber, and (5) measurement of radiated energy by a point source. Contains all of the information on materials and apparatus needed to perform the experiments.…

Crystal growth of artificial snow

NASA Technical Reports Server (NTRS)

Kimura, S.; Oka, A.; Taki, M.; Kuwano, R.; Ono, H.; Nagura, R.; Narimatsu, Y.; Tanii, J.; Kamimiytat, Y.

1984-01-01

Snow crystals were grown onboard the space shuttle during STS-7 and STS-8 to facilitate the investigation of crystal growth under conditions of weightlessness. The experimental design and hardware are described. Space-grown snow crystals were polyhedrons looking like spheres, which were unlike snow crystals produced in experiments on Earth.

An Apparatus for Growth of Small Crystals From Solutions.

ERIC Educational Resources Information Center

Mitrovic, Mico M.

1995-01-01

Describes an apparatus for crystal growth that was designed to study growth kinetics of small crystals from solutions and to obtain crystals of various substances. Describes the use of the apparatus in laboratory practical experiments in the field of crystal growth physics within the course "Solid State Physics". (JRH)

Experiment 3: Zeolite Crystal Growth in Microgravity- The USML-2 Mission

NASA Technical Reports Server (NTRS)

Bac, Nurcan; Warzywoda, Juliusz; Sacco, Albert, Jr.

1998-01-01

The extensive use of zeolites and their impact on the world's economy leads to many efforts to characterize their structure, and to improve the knowledge base for nucleation and growth of these crystals. The Zeolite Crystal Growth (ZCG) experiment on USML-2 aims to enhance the understanding of nucleation and growth of zeolite crystals while attempting to provide a means of controlling the defect concentration in microgravity. Zeolites A, X, Beta, and Silicalite were grown during the 16-day USML-2 mission. The solutions where the nucleation event was controlled yielded larger and more uniform crystals of better morphology and purity than their terrestrial/control counterparts. Space-grown Beta crystals were free of line defects while terrestrial/controls had substantial defects.

Physical Vapor Transport of Mercurous Chloride Crystals: Design of a Microgravity Experiment

NASA Technical Reports Server (NTRS)

Duval, W, M. B.; Singh, N. B.; Glicksman, M. E.

1997-01-01

Flow field characteristics predicted from a computational model show that the dynamical state of the flow, for practical crystal growth conditions of mercurous chloride, can range from steady to unsteady. Evidence that the flow field can be strongly dominated by convection for ground-based conditions is provided by the prediction of asymmetric velocity profiles bv the model which show reasonable agreement with laser Doppler velocimetry experiments in both magnitude and planform. Unsteady flow is shown to be correlated with a degradation of crystal quality as quantified by light scattering pattern measurements, A microgravity experiment is designed to show that an experiment performed with parameters which yield an unsteady flow becomes steady (diffusive-advective) in a microgravity environment of 10(exp -3) g(sub 0) as predicted by the model, and hence yields crystals with optimal quality.

Crystal structures of native and xylosaccharide-bound alkali thermostable xylanase from an alkalophilic Bacillus sp. NG-27: Structural insights into alkalophilicity and implications for adaptation to polyextreme conditions

PubMed Central

Manikandan, Karuppasamy; Bhardwaj, Amit; Gupta, Naveen; Lokanath, Neratur K.; Ghosh, Amit; Reddy, Vanga Siva; Ramakumar, Suryanarayanarao

2006-01-01

Crystal structures are known for several glycosyl hydrolase family 10 (GH10) xylanases. However, none of them is from an alkalophilic organism that can grow in alkaline conditions. We have determined the crystal structures at 2.2 Å of a GH10 extracellular endoxylanase (BSX) from an alkalophilic Bacillus sp. NG-27, for the native and the complex enzyme with xylosaccharides. The industrially important enzyme is optimally active and stable at 343 K and at a pH of 8.4. Comparison of the structure of BSX with those of other thermostable GH10 xylanases optimally active at acidic or close to neutral pH showed that the solvent-exposed acidic amino acids, Asp and Glu, are markedly enhanced in BSX, while solvent-exposed Asn was noticeably depleted. The BSX crystal structure when compared with putative three-dimensional homology models of other extracellular alkalophilic GH10 xylanases from alkalophilic organisms suggests that a protein surface rich in acidic residues may be an important feature common to these alkali thermostable enzymes. A comparison of the surface features of BSX and of halophilic proteins allowed us to predict the activity of BSX at high salt concentrations, which we verified through experiments. This offered us important lessons in the polyextremophilicity of proteins, where understanding the structural features of a protein stable in one set of extreme conditions provided clues about the activity of the protein in other extreme conditions. The work brings to the fore the role of the nature and composition of solvent-exposed residues in the adaptation of enzymes to polyextreme conditions, as in BSX. PMID:16823036

Spontaneous topological charging of tactoids in a living nematic

NASA Astrophysics Data System (ADS)

Genkin, Mikhail M.; Sokolov, Andrey; Aranson, Igor S.

2018-04-01

Living nematic is a realization of an active matter combining a nematic liquid crystal with swimming bacteria. The material exhibits a remarkable tendency towards spatio-temporal self-organization manifested in formation of dynamic textures of self-propelled half-integer topological defects (disclinations). Here we report on the study of such living nematic near normal inclusions, or tactoids, naturally realized in liquid crystals close to the isotropic-nematic (I–N) phase transition. On the basis of the computational analysis, we have established that tactoid’s I–N interface spontaneously acquire negative topological charge which is proportional to the tactoid’s size and depends on the concentration of bacteria. The observed negative charging is attributed to the drastic difference in the mobilities of +1/2 and ‑1/2 topological defects in active systems. The effect is described in the framework of a kinetic theory for point-like weakly-interacting defects with different mobilities. Our dedicated experiment fully confirmed the theoretical prediction. The results hint into new strategies for control of active matter.

Spontaneous topological charging of tactoids in a living nematic

DOE Office of Scientific and Technical Information (OSTI.GOV)

Genkin, Mikhail M.; Sokolov, Andrey; Aranson, Igor S.

Living nematic is a realization of an active matter combining a nematic liquid crystal with swimming bacteria. The material exhibits a remarkable tendency towards spatio-temporal self-organization manifested in formation of dynamic textures of self-propelled half-integer topological defects (disclinations). Here we report on the study of such living nematic near normal inclusions, or tactoids, naturally realized in liquid crystals close to the isotropic-nematic (I-N) phase transition. On the basis of the computational analysis, we have established that tactoid's I-Ninterface spontaneously acquire negative topological charge which is proportional to the tactoid's size and depends on the concentration of bacteria. The observed negativemore » charging is attributed to the drastic difference in the mobilities of +1/2 and -1/2 topological defects in active systems. The effect is described in the framework of a kinetic theory for point-like weakly-interacting defects with different mobilities. Our dedicated experiment fully confirmed the theoretical prediction. Here, the results hint into new strategies for control of active matter.« less

Spontaneous topological charging of tactoids in a living nematic

DOE PAGES

Genkin, Mikhail M.; Sokolov, Andrey; Aranson, Igor S.

2018-04-13

Living nematic is a realization of an active matter combining a nematic liquid crystal with swimming bacteria. The material exhibits a remarkable tendency towards spatio-temporal self-organization manifested in formation of dynamic textures of self-propelled half-integer topological defects (disclinations). Here we report on the study of such living nematic near normal inclusions, or tactoids, naturally realized in liquid crystals close to the isotropic-nematic (I-N) phase transition. On the basis of the computational analysis, we have established that tactoid's I-Ninterface spontaneously acquire negative topological charge which is proportional to the tactoid's size and depends on the concentration of bacteria. The observed negativemore » charging is attributed to the drastic difference in the mobilities of +1/2 and -1/2 topological defects in active systems. The effect is described in the framework of a kinetic theory for point-like weakly-interacting defects with different mobilities. Our dedicated experiment fully confirmed the theoretical prediction. Here, the results hint into new strategies for control of active matter.« less

STS-107 Flight Day 8 Highlights

NASA Technical Reports Server (NTRS)

2003-01-01

This video shows the activities of the STS-107 crew (Rick Husband, Commander; William McCool, Pilot; Kalpana Chawla, David Brown, Michael Anderson, Laurel Clark, Mission Specialists, Ilan Ramon, Payload Specialist) during flight day 8 of the Columbia orbiter's final flight. The primary activities of flight day 8 are spaceborne experiments. Some background information is given on the SOFBALL (Structure of Flame Balls at Low Lewis-Number) microgravity experiment as footage of the flame balls is shown. The video also shows the MEIDEX (Mediterranean Israeli Dust Experiment) calibrating on the Moon. The six STARS (Space Technology and Research Students) international student experiments are profiled, including experiments on carpenter bees (Liechtenstein), spiders (Australia), silkworms (China), ants (United States), crystal growth (Israel), and fish embryos (Japan). A commercial experiment on roses is also profiled. Astronaut Clark gives a tour of the SpaceHab RDM (Research Double Module), in the space shuttle's payload bay. Astronauts McCool and Ramon take turns on an exercise machine. The video includes a partly cloudy view of the Pacific Ocean.

Hematite-Ilmenite with Magnetite from the Ecstall Pluton, British Columbia: Single Crystal Magnetic Experiments

NASA Astrophysics Data System (ADS)

Scott, G. R.; Brownlee, S. J.; Feinberg, J. M.; Renne, P. R.

2008-12-01

Rocks provide a compound paleomagnetic signal from mixtures of various iron minerals with different grain sizes and magnetic stabilities. To unravel this complex signal, specific mineral phases with stable remanence can be individually examined as single crystals. In the case of the Ecstall Pluton (~91 Ma), intra-pluton discordance of paleomagnetic directions may be the result of post-crystallization deformation, or mineralogical changes caused by re-heating from the adjacent Quottoon Pluton (~52 Ma). In order to distinguish between these two hypotheses we conducted rock magnetic experiments on single crystals of finely-exsolved hematite-ilmenite along a transect approaching the Quottoon Pluton. Reflected light, and SEM observations show grains of hematite and ilmenite as the dominant Fe-oxide throughout the Ecstall. Nearest the Quottoon Pluton, the hematite-ilmenite grains exhibit the classic rutile blitz texture. The lamellar microstructure observed in the hematite-ilmenite grains, as well as the rutile blitz texture are linked to the thermal history of the Ecstall Pluton, and have important effects on the magnetic properties of these grains (i.e. lamellar magnetism). Our results include the magnetic unmixing of isothermal remanence magnetization (IRM) acquisition, First Order Reversal Curve (FORC) diagrams, temperature vs. remanence experiments (MPMS), and TEM studies. These data provide a spatially resolved record of rock magnetic variations across the Ecstall Pluton, showing evidence of thermally activated reduction of hematite to magnetite in samples within 13 km of the Quottoon Pluton. TEM analysis shows the magnetite is present as 20-50 nm-sized particles within hematite. This mineralogic change may be responsible for the variations in paleomagnetic directions across the Ecstall Pluton, and clear evidence for this reaction cannot be found by traditional rock characterization techniques, illustrating the need to couple detailed rock magnetic, paleomagnetic, and mineralogic analyses.

Growth of single crystals of mercuric iodide (HgI/sub 2/) in spacelab III

DOE Office of Scientific and Technical Information (OSTI.GOV)

Van Den Berg, L.; Schnepple, W.F.

1981-01-01

Continued development of a system designed to grow crystals by physical vapor transport in the environment of Spacelab III will be described, with special emphasis on simulation of expected space conditions, adjustment of crystal growth parameters, and on board observation and control of the experiment by crew members and ground personnel. A critical factor in the use of mercuric iodide for semiconductor detectors of x-rays and gamma-rays is the crystalline quality of the material. The twofold purpose of the Spacelab III experiment is therefore to grow single crystals with superior electronic properties as an indirect result of the greatly reducedmore » gravity field during the growth, and to obtain data which will lead to improved understanding of the vapor transport mechanism. The experiments planned to evaluate the space crystals, including gamma-ray diffractometry and measurements of stoichiometry, lattice dimensions, mechanical strength, luminescense, and detector performance are discussed.« less

A Differential Scanning Calorimetry Method for Construction of Continuous Cooling Transformation Diagram of Blast Furnace Slag

NASA Astrophysics Data System (ADS)

Gan, Lei; Zhang, Chunxia; Shangguan, Fangqin; Li, Xiuping

2012-06-01

The continuous cooling crystallization of a blast furnace slag was studied by the application of the differential scanning calorimetry (DSC) method. A kinetic model describing the correlation between the evolution of the degree of crystallization with time was obtained. Bulk cooling experiments of the molten slag coupled with numerical simulation of heat transfer were conducted to validate the results of the DSC methods. The degrees of crystallization of the samples from the bulk cooling experiments were estimated by means of the X-ray diffraction (XRD) and the DSC method. It was found that the results from the DSC cooling and bulk cooling experiments are in good agreement. The continuous cooling transformation (CCT) diagram of the blast furnace slag was constructed according to crystallization kinetic model and experimental data. The obtained CCT diagram characterizes with two crystallization noses at different temperature ranges.

Characterization of PbWO4 crystals for high-energy physics experiments

NASA Astrophysics Data System (ADS)

Kim, M. J.; Park, H.; Kim, H. J.

2016-09-01

High-energy physics (HEP) experiments have employed many new types of scintillators. Specifically, bismuth germanate, thallium-doped cesium iodide, and lead tungstate (PbWO4, PWO) have been used for the L3 experiment; CLEO II, Belle and BES-III; and CMS, respectively. PWO has particularly beneficial properties, such as high density, fast decay time, short radiation length and radiation hardness. In this study, we tested the PWO crystals at low temperatures to determine their applicability in future calorimeters. Various crystals from the Proton Antiproton Annihilations at Darmstadt (PANDA) experiment in Giessen, the Bogoroditsk Techno-Chemical Plant (BTCP) in Russia and by Shanghai Institute of Ceramics, Chinese Academy of Sciences (SICCAS) in China were investigated. We studied the scintillation properties of PWO crystals, such as their X-ray luminescence, relative light yields, absolute light yields, energy resolutions, decay times and longitudinal uniformities of their light yields. In addition, we measured the temperature dependences of the light yields and decay times by using a 137Cs γ-ray source. The emission spectra of the PWO crystals consisted of a broad band from 350 nm to 700 nm, and the peak emission wavelength in each spectrum was 420 nm. The emission spectra of the PWO crystals from SICCAS were slightly shifted to longer wavelengths compared with those of the crystals from the other institutions.

Crystallization and preliminary crystallographic analysis of latent, active and recombinantly expressed aurone synthase, a polyphenol oxidase, from Coreopsis grandiflora

DOE Office of Scientific and Technical Information (OSTI.GOV)

Molitor, Christian; Mauracher, Stephan Gerhard; Rompel, Annette, E-mail: annette.rompel@univie.ac.at

2015-05-22

Latent and active aurone synthase purified from petals of C. grandiflora (cgAUS1) were crystallized. The crystal quality of recombinantly expressed latent cgAUS1 was significantly improved by co-crystallization with the polyoxotungstate Na{sub 6}[TeW{sub 6}O{sub 24}] within the liquid–liquid phase-separation zone. Aurone synthase (AUS), a member of a novel group of plant polyphenol oxidases (PPOs), catalyzes the oxidative conversion of chalcones to aurones. Two active cgAUS1 (41.6 kDa) forms that differed in the level of phosphorylation or sulfation as well as the latent precursor form (58.9 kDa) were purified from the petals of Coreopsis grandiflora. The differing active cgAUS1 forms and themore » latent cgAUS1 as well as recombinantly expressed latent cgAUS1 were crystallized, resulting in six different crystal forms. The active forms crystallized in space groups P2{sub 1}2{sub 1}2{sub 1} and P12{sub 1}1 and diffracted to ∼1.65 Å resolution. Co-crystallization of active cgAUS1 with 1,4-resorcinol led to crystals belonging to space group P3{sub 1}21. The crystals of latent cgAUS1 belonged to space group P12{sub 1}1 and diffracted to 2.50 Å resolution. Co-crystallization of recombinantly expressed pro-AUS with the hexatungstotellurate(VI) salt Na{sub 6}[TeW{sub 6}O{sub 24}] within the liquid–liquid phase separation zone significantly improved the quality of the crystals compared with crystals obtained without hexatungstotellurate(VI)« less

Characterization and activity of visible-light-driven TiO 2 photocatalyst codoped with lanthanum and iodine

NASA Astrophysics Data System (ADS)

Li, Ling; Zhuang, Huisheng; Bu, Dan

2011-08-01

The novel visible-light-activated La/I/TiO 2 nanocomposition photocatalyst was successfully synthesized using precipitation-dipping method, and characterized by X-ray powder diffraction (XRD), the Brunauer-Emmett-Teller (BET) method, transmission electron microscopy (TEM), thermogravimetry-differential scanning calorimetry (TG-DSC) and UV-vis diffuse reflectance spectroscopy (UV-vis DRS). The photocatalytic activity of La/I/TiO 2 was evaluated by studying photodegradation of reactive blue 19 as a probe reaction under simulated sunlight irradiation. Photocatalytic experiment results showed that the maximum specific photocatalytic activity of the La/I/TiO 2 photocatalyst appeared when the molar ratio of La/Ti was 2.0 at%, calcined at 350 °C for 2 h, due to the sample with good crystallization, high BET surface area and small crystal size. Under simulated sunlight irradiation, the degradation of reactive blue 19 aqueous solution reached 98.6% in 80 min, which showed La/I/TiO 2 photocatalyst to be much higher photocatalytic activity compared to standard Degussa P25 photocatalyst. The higher visible light activity is due to the codoping of lanthanum and iodine.

Post-flight analyses of the crystals from the M0003-14 quartz crystal microbalance experiment

NASA Technical Reports Server (NTRS)

Stuckey, W. K.; Radhakrishnan, G.; Wallace, D.

1993-01-01

Quartz Crystal Microbalances constructed by QCM Research were flown on the leading and trailing edges of LDEF as one of the sub-experiments of M0003. Response of the crystals coated with 150 A of In2O3 was recorded during the first 424 days of the mission. A second QCM with crystals coated with 150 A of ZnS was also flown but not monitored. After the flight, the QCM's were disassembled and analyzed in The Aerospace Corporation laboratories. The samples included the crystals from the leading and trailing edge samples of both types of coatings along with the reference crystals, which were inside the QCM housing. Analyses were performed by scanning electron microscopy, energy dispersive x-ray analyses, x-ray photoelectron spectroscopy, ion microprobe mass analysis, and reflectance spectroscopy in the infrared and UV/visible regions. The crystals are contaminated predominantly with silicone compounds. The contamination is higher on the leading edge than on the trailing edge and higher on the exposed crystals than on the reference crystals.

Evolution of the Shape of Detached GeSi Crystals in Microgravity

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.

2013-01-01

A series of GeSi crystal growth experiments are planned to be conducted in the Low Gradient Furnace (LGF) onboard the International Space Station. An objective of these experiments is to understand the mechanisms of detached Bridgman growth, a process in which a gap exists between the growing semiconductor crystal and the crucible wall. Crystals grown without wall contact have superior quality to otherwise similar crystals grown in direct contact with a container, especially with respect to impurity incorporation, formation of dislocations, and residual stress in crystals. Numerical calculations are used to determine the conditions in which a gap can exist. According to crystal shape stability theory, only some of these gap widths will be dynamically stable. Beginning with a crystal diameter that differs from stable conditions, the transient crystal growth process is analyzed. In microgravity, dynamic stability depends only on capillary effects and is decoupled from heat transfer. Depending on the initial conditions and growth parameters, the crystal shape will evolve towards the crucible wall, towards a stable gap width, or towards the center of the crucible, collapsing the meniscus.

Highly Non-Linear Optical (NLO) organic crystals

NASA Technical Reports Server (NTRS)

Harris, J. Milton

1987-01-01

This research project involves the synthesis and characterization of organic materials having powerful nonlinear optical (NLO) properties and the growth of highly ordered crystals and monomolecular films of these materials. Research in four areas is discussed: theoretical design of new materials, characterization of NLO materials, synthesis of new materials and development of coupling procedures for forming layered films, and improvement of the techniques for vapor phase and solution phase growth of high quality organic crystals. Knowledge gained from these experiments will form the basis for experiments in the growth of these crystals.

Ultra-compact laser beam steering device using holographically formed two dimensional photonic crystal.

PubMed

Dou, Xinyuan; Chen, Xiaonan; Chen, Maggie Yihong; Wang, Alan Xiaolong; Jiang, Wei; Chen, Ray T

2010-03-01

In this paper, we report the theoretical study of polymer-based photonic crystals for laser beam steering which is based on the superprism effect as well as the experiment fabrication of the two dimensional photonic crystals for the laser beam steering. Superprism effect, the principle for beam steering, was separately studied in details through EFC (Equifrequency Contour) analysis. Polymer based photonic crystals were fabricated through double exposure holographic interference method using SU8-2007. The experiment results showed a beam steering angle of 10 degree for 30 nm wavelength variation.

PromISS 4 hardware set up in the MSG during Expedition 12

NASA Image and Video Library

2006-01-18

ISS012-E-16162 (18 Jan. 2006) --- Astronaut William S. (Bill) McArthur, Expedition 12 commander and NASA space station science officer, configures the Microgravity Science Glovebox (MSG) facility to prepare for the installation and activation of the Protein Crystal Growth Monitoring by Digital Holographic Microscope (PromISS) experiment in the Destiny laboratory on the International Space Station.

PromISS 4 hardware set up in the MSG during Expedition 12

NASA Image and Video Library

2006-01-19

ISS012-E-16237 (19 Jan. 2006) --- Astronaut William S. (Bill) McArthur, Expedition 12 commander and NASA space station science officer, configures the Microgravity Science Glovebox (MSG) facility to prepare for the installation and activation of the Protein Crystal Growth Monitoring by Digital Holographic Microscope (PromISS) experiment in the Destiny laboratory on the International Space Station.

PromISS 4 hardware set up in the MSG during Expedition 12

NASA Image and Video Library

2006-01-19

ISS012-E-16245 (19 Jan. 2006) --- Astronaut William S. (Bill) McArthur, Expedition 12 commander and NASA space station science officer, configures the Microgravity Science Glovebox (MSG) facility to prepare for the installation and activation of the Protein Crystal Growth Monitoring by Digital Holographic Microscope (PromISS) experiment in the Destiny laboratory on the International Space Station.

A Comprehensive Study of Formic Acid Oxidation on Palladium Nanocrystals with Different Types of Facets and Twin Defects

DOE PAGES

Choi, Sang-Il; Herron, Jeffrey A.; Scaranto, Jessica; ...

2015-04-13

Palladium has been recognized as the best anodic, monometallic electrocatalyst for the formic acid oxidation (FAO) reaction in a direct formic acid fuel cell. Here we report a systematic study of FAO on a variety of Pd nanocrystals, including cubes, right bipyramids, octahedra, tetrahedra, decahedra, and icosahedra. These nanocrystals were synthesized with approximately the same size, but different types of facets and twin defects on their surfaces. Our measurements indicate that the Pd nanocrystals enclosed by {100} facets have higher specific activities than those enclosed by {111} facets, in agreement with prior observations for Pd single-crystal substrates. If comparing nanocrystalsmore » predominantly enclosed by a specific type of facet, {100} or {111}, those with twin defects displayed greatly enhanced FAO activities compared to their single-crystal counterparts. To rationalize these experimental results, we performed periodic, self-consistent DFT calculations on model single-crystal substrates of Pd, representing the active sites present in the nanocrystals used in the experiments. The calculation results suggest that the enhancement of FAO activity on defect regions, represented by Pd(211) sites, compared to the activity of both Pd(100) and Pd(111) surfaces, could be attributed to an increased flux through the HCOO-mediated pathway rather than the COOH-mediated pathway on Pd(211). Since COOH has been identified as a precursor to CO, a site-poisoning species, a lower coverage of CO at the defect regions will lead to a higher activity for the corresponding nanocrystal catalysts, containing those defect regions.« less

Synthesis and crystal structure determination of copper(II)-complex: In vitro DNA and HSA binding, pBR322 plasmid cleavage, cell imaging and cytotoxic studies.

PubMed

Tabassum, Sartaj; Zaki, Mehvash; Ahmad, Musheer; Afzal, Mohd; Srivastav, Saurabh; Srikrishna, Saripella; Arjmand, Farukh

2014-08-18

New Cu(II) complex 1 of indole-3-propionic acid and 1,10-phenanthroline was synthesized and characterized by analytical, spectroscopic and single crystal X-ray diffraction. In vitro DNA binding studies of 1 was performed by employing UV-vis and fluorescence spectroscopic techniques. The binding affinity towards human serum albumin (HSA) was also investigated to understand the carrier role in body system, as the time dependent HPLC experiment of 1 revealed that bonded drug with protein releases slowly in presence of DNA. Complex 1 exhibited good anti-tumor activity (GI50 values <10 μg/ml), and to elucidate the mechanism of tumor inhibition, topoisomerase I enzymatic activity was carried out and further validated by cell imaging studies which clearly showed its nuclear localization. Copyright © 2014 Elsevier Masson SAS. All rights reserved.

Flight Experiments of Physical Vapor Transport of ZnSe: Growth of Crystals in Various Convective Conditions

NASA Technical Reports Server (NTRS)

Su, Ching-Hua

2015-01-01

A low gravity material experiment will be performed in the Material Science Research Rack (MSRR) on International Space Station (ISS). The flight experiment will conduct crystal growths of ZnSe and related ternary compounds, such as ZnSeS and ZnSeTe, by physical vapor transport (PVT). The main objective of the project is to determine the relative contributions of gravity-driven fluid flows to the compositional distribution, incorporation of impurities and defects, and deviation from stoichiometry observed in the grown crystals as results of buoyancy-driven convection and growth interface fluctuations caused by irregular fluid-flows on Earth. The investigation consists of extensive ground-based experimental and theoretical research efforts and concurrent flight experimentation. The objectives of the ground-based studies are (1) obtain the experimental data and conduct the analyses required to define the optimum growth parameters for the flight experiments, (2) perfect various characterization techniques to establish the standard procedure for material characterization, (3) quantitatively establish the characteristics of the crystals grown on Earth as a basis for subsequent comparative evaluations of the crystals grown in a low-gravity environment and (4) develop theoretical and analytical methods required for such evaluations. ZnSe and related ternary compounds have been grown by vapor transport technique with real time in-situ non-invasive monitoring techniques. The grown crystals have been characterized extensively by various techniques to correlate the grown crystal properties with the growth conditions. This talk will focus on the ground-based studies on the PVT crystal growth of ZnSe and related ternary compounds, especially the effects of different growth orientations related to gravity direction on the grown crystals.

A study of crystal growth by solution technique

NASA Technical Reports Server (NTRS)

Lal, R. B.

1981-01-01

The mechanism of crystal growth by solution technique was studied. A low temperature solution crystal growth setup was developed. Crystals of triglycine sulfate (TGS) were grown using this arrangement. Some additional tasks were performed toward fabrication of experiments for future space flight.

The 1989 Solar Maximum Mission event list

NASA Technical Reports Server (NTRS)

Dennis, B. R.; Licata, J. P.; Tolbert, A. K.

1992-01-01

This document contains information on solar burst and transient activity observed by the Solar Maximum Mission (SMM) during 1989 pointed observations. Data from the following SMM experiments are included: (1) Gamma Ray Spectrometer, (2) Hard X-Ray Burst Spectrometer, (3) Flat Crystal Spectrometer, (4) Bent Crystal Spectrometer, (5) Ultraviolet Spectrometer Polarimeter, and (6) Coronagraph/Polarimeter. Correlative optical, radio, and Geostationary Operational Satellite (GOES) X-ray data are also presented. Where possible, bursts or transients observed in the various wavelengths were grouped into discrete flare events identified by unique event numbers. Each event carries a qualifier denoting the quality or completeness of the observations. Spacecraft pointing coordinates and flare site angular displacement values from sun center are also included.

The 1988 Solar Maximum Mission event list

NASA Technical Reports Server (NTRS)

Dennis, B. R.; Licata, J. P.; Tolbert, A. K.

1992-01-01

Information on solar burst and transient activity observed by the Solar Maximum Mission (SMM) during 1988 pointed observations is presented. Data from the following SMM experiments are included: (1) gamma ray spectrometer; (2) hard x ray burst spectrometer; (3) flat crystal spectrometers; (4) bent crystal spectrometer; (5) ultraviolet spectrometer polarimeter; and (6) coronagraph/polarimeter. Correlative optical, radio, and Geostationary Operational Environmental Satellite (GOES) x ray data are also presented. Where possible, bursts, or transients observed in the various wavelengths were grouped into discrete flare events identified by unique event numbers. Each event carries a qualifier denoting the quality or completeness of the observation. Spacecraft pointing coordinates and flare site angular displacement values from sun center are also included.

The 1984 - 1987 Solar Maximum Mission event list

NASA Technical Reports Server (NTRS)

Dennis, B. R.; Licata, J. P.; Nelson, J. J.; Tolbert, A. K.

1992-01-01

Information on solar burst and transient activity observed by the Solar Maximum Mission (SMM) during 1984-1987 pointed observations is presented. Data from the following SMM experiments are included: (1) gamma ray spectrometer; (2) hard x-ray burst spectrometer; (3) flat crystal spectrometer; (4) bent crystal spectrometer; (5) ultraviolet spectrometer polarimeter; and (6) coronograph/polarimeter. Correlative optical, radio, and Geostationary Operational Environmental Satellite (GOES) x ray data are also presented. Where possible, bursts or transients observed in the various wavelengths were grouped into discrete flare events identified by unique event numbers. Each event carries a qualifier denoting the quality or completeness of the observations. Spacecraft pointing coordinates and flare site angular displacement values from sun center are also included.

Spectroscopic investigations using density functional theory on 2-methoxy- 4(phenyliminomethyl)phenol: A non linear optical material

NASA Astrophysics Data System (ADS)

Hijas, K. M.; Madan Kumar, S.; Byrappa, K.; Geethakrishnan, T.; Jeyaram, S.; Nagalakshmi, R.

2018-03-01

Single crystals of 2-methoxy-4(phenyliminomethyl)phenol were grown from ethanol by slow evaporation solution growth technique. Single crystal X-ray diffraction experiment reveals the crystallization in orthorhombic system having non-centrosymmetric space group C2221. Geometrical optimization by density functional theory method was carried out using Gaussian program and compared with experimental results. Detailed experimental and theoretical vibrational analyses were carried out and the results were correlated to find close agreement. Thermal analyses show the material is thermally stable with a melting point of 159 °C. Natural bond orbital analysis was carried out to explain charge transfer interactions through hydrogen bonding. Relatively smaller HOMO-LUMO band gap favors the non linear optical activity of the molecule. Natural population analysis and molecular electrostatic potential calculations visualize the charge distribution in an isolated molecule. Calculated first-order molecular hyperpolarizability and preliminary second harmonic generation test carried out using Kurtz-Perry technique establish 2-methoxy-4(phenyliminomethyl)phenol crystal as a good non linear optical material. Z-scan proposes the material for reverse saturable absorption.

Conductivity equations of protons transporting through 2D crystals obtained with the rate process theory and free volume concept

NASA Astrophysics Data System (ADS)

Hao, Tian; Xu, Yuanze; Hao, Ting

2018-04-01

The Eyring's rate process theory and free volume concept are employed to treat protons (or other particles) transporting through a 2D (two dimensional) crystal like graphene and hexagonal boron nitride. The protons are assumed to be activated first in order to participate conduction and the conduction rate is dependent on how much free volume available in the system. The obtained proton conductivity equations show that only the number of conduction protons, proton size and packing structure, and the energy barrier associated with 2D crystals are critical; the quantization conductance is unexpectedly predicted with a simple Arrhenius type temperature dependence. The predictions agree well with experimental observations and clear out many puzzles like much smaller energy barrier determined from experiments than from the density function calculations and isotope separation rate independent of the energy barrier of 2D crystals, etc. Our work may deepen our understandings on how protons transport through a membrane and has direct implications on hydrogen related technology and proton involved bioprocesses.

Absorbing a Little Water: The Structural, Thermodynamic, and Kinetic Relationship between Pyrogallol and Its Tetarto-Hydrate

PubMed Central

2013-01-01

The anhydrate and the stoichiometric tetarto-hydrate of pyrogallol (0.25 mol water per mol pyrogallol) are both storage stable at ambient conditions, provided that they are phase pure, with the system being at equilibrium at aw (water activity) = 0.15 at 25 °C. Structures have been derived from single crystal and powder X-ray diffraction data for the anhydrate and hydrate, respectively. It is notable that the tetarto-hydrate forms a tetragonal structure with water in channels, a framework that although stabilized by water, is found as a higher energy structure on a computationally generated crystal energy landscape, which has the anhydrate crystal structure as the most stable form. Thus, a combination of slurry experiments, X-ray diffraction, spectroscopy, moisture (de)sorption, and thermo-analytical methods with the computationally generated crystal energy landscape and lattice energy calculations provides a consistent picture of the finely balanced hydration behavior of pyrogallol. In addition, two monotropically related dimethyl sulfoxide monosolvates were found in the accompanying solid form screen. PMID:24027438

Absorbing a Little Water: The Structural, Thermodynamic, and Kinetic Relationship between Pyrogallol and Its Tetarto-Hydrate.

PubMed

Braun, Doris E; Bhardwaj, Rajni M; Arlin, Jean-Baptiste; Florence, Alastair J; Kahlenberg, Volker; Griesser, Ulrich J; Tocher, Derek A; Price, Sarah L

2013-09-04

The anhydrate and the stoichiometric tetarto-hydrate of pyrogallol (0.25 mol water per mol pyrogallol) are both storage stable at ambient conditions, provided that they are phase pure, with the system being at equilibrium at a w (water activity) = 0.15 at 25 °C. Structures have been derived from single crystal and powder X-ray diffraction data for the anhydrate and hydrate, respectively. It is notable that the tetarto-hydrate forms a tetragonal structure with water in channels, a framework that although stabilized by water, is found as a higher energy structure on a computationally generated crystal energy landscape, which has the anhydrate crystal structure as the most stable form. Thus, a combination of slurry experiments, X-ray diffraction, spectroscopy, moisture (de)sorption, and thermo-analytical methods with the computationally generated crystal energy landscape and lattice energy calculations provides a consistent picture of the finely balanced hydration behavior of pyrogallol. In addition, two monotropically related dimethyl sulfoxide monosolvates were found in the accompanying solid form screen.

Solid Xenon Project

NASA Astrophysics Data System (ADS)

Balakishiyeva, Durdana N.; Mahapatra, Rupak; Saab, Tarek; Yoo, Jonghee

2010-08-01

Crystals like Germanium and Silicon need to be grown in specialized facilities which is time and money costly. It takes many runs to test the detector once it's manufactured and mishaps are very probable. It is of a great challenge to grow big germanium crystals and that's why stacking them up in a tower is the only way at the moment to increase testing mass. Liquid Noble gas experiments experiencing contamination problems, their predicted energy resolution at 10 keV and lower energy range is not as good as predicted. Every experiment is targeting one specific purpose, looking for one thing. Why not to design an experiment that is diverse and build a detector that can search for Dark Matter, Solar Axions, Neutrinoless Double Beta decay, etc. Solid Xenon detector is such detector. We designed a simple Xenon crystal growing chamber that was put together at Fermi National Accelerator Laboratory. The first phase of this experiment was to demonstrate that a good, crack free Xenon crystal can be grown (regardless of many failed attempts by various groups) and our first goal, 1 kg crystal, was successful.

Kotov works with Plasma Crystal-3+ Experiment in the SM during Expedition 22

NASA Image and Video Library

2010-01-25

ISS022-E-035436 (25 Jan. 2010) --- Russian cosmonaut Oleg Kotov, Expedition 22 flight engineer, works with the Plasma Crystal-3 experiment in the Zvezda Service Module of the International Space Station.

Kotov works with Plasma Crystal-3+ Experiment in the SM during Expedition 22

NASA Image and Video Library

2010-01-25

ISS022-E-035434 (25 Jan. 2010) --- Russian cosmonaut Oleg Kotov, Expedition 22 flight engineer, works with the Plasma Crystal-3 experiment in the Zvezda Service Module of the International Space Station.

Structural Biology of Proteins of the Multi-enzyme Assembly Human Pyruvate Dehydrogenase Complex

NASA Technical Reports Server (NTRS)

2003-01-01

Objectives and research challenges of this effort include: 1. Need to establish Human Pyruvate Dehydrogenase Complex protein crystals; 2. Need to test value of microgravity for improving crystal quality of Human Pyruvate Dehydrogenase Complex protein crystals; 3. Need to improve flight hardware in order to control and understand the effects of microgravity on crystallization of Human Pyruvate Dehydrogenase Complex proteins; 4. Need to integrate sets of national collaborations with the restricted and specific requirements of flight experiments; 5. Need to establish a highly controlled experiment in microgravity with a rigor not yet obtained; 6. Need to communicate both the rigor of microgravity experiments and the scientific value of results obtained from microgravity experiments to the national community; and 7. Need to advance the understanding of Human Pyruvate Dehydrogenase Complex structures so that scientific and commercial advance is identified for these proteins.

Using Magnetic Field Gradients to Simulate Variable Gravity in Fluids and Materials Experiments

NASA Technical Reports Server (NTRS)

Ramachandran, Narayanan

2006-01-01

Fluid flow due to a gravitational field is caused by sedimentation, thermal buoyancy, or solutal buoyancy induced convection. During crystal growth, for example, these flows are undesirable and can lead to crystal imperfections. While crystallization in microgravity can approach diffusion limited growth conditions (no convection), terrestrially strong magnetic fields can be used to control fluid flow and sedimentation effects. In this work, a theory is presented on the stability of solutal convection of a magnetized fluid(weak1y paramagnetic) in the presence of a magnetic field. The requirements for stability are developed and compared to experiments performed within the bore of a superconducting magnet. The theoretical predictions are in good agreement with the experiments. Extension of the technique can also be applied to study artificial gravity requirements for long duration exploration missions. Discussion of this application with preliminary experiments and application of the technique to crystal growth will be provided.

Nucleation and crystallization kinetics of hydrated amorphous lactose above the glass transition temperature.

PubMed

Schmitt, E A; Law, D; Zhang, G G

1999-03-01

The crystallization kinetics of amorphous lactose in the presence and absence of seed crystals were investigated at 57.5% relative humidity. Isothermal crystallization studies were conducted gravimetrically in an automated vacuum moisture balance at several temperatures between 18 and 32 degrees C. The crystallization rate constants were then determined from Johnson-Mehl-Avrami (JMA) treatment and isothermal activation energies were obtained from Arrhenius plots. Based on microscopic observations, a reaction order of 3 was used for JMA analysis. The nonisothermal activation energies were determined by differential scanning calorimetry using Kissinger's analysis. Isothermal activation energies for amorphous lactose with and without seed crystals were 89.5 (+/-5.6) kJ/mol and 186.5 (+/-17.6) kJ/mol, respectively. Nonisothermal activation energies with and without seed crystals were 71 (+/-7.5) kJ/mol and 80.9 (+/-8.9) kJ/mol, respectively. The similarity of the isothermal and nonisothermal activation energies for the sample with seeds suggested that crystallization was occurring by growth from a fixed number of preexisting nuclei. Markedly different isothermal and nonisothermal activation energies in the absence of seeds suggested a site-saturated nucleation mechanism, and therefore allowed calculation of an activation energy for nucleation of 317 kJ/mol.

Adaptation of in-situ microscopy for crystallization processes

NASA Astrophysics Data System (ADS)

Bluma, A.; Höpfner, T.; Rudolph, G.; Lindner, P.; Beutel, S.; Hitzmann, B.; Scheper, T.

2009-08-01

In biotechnological and pharmaceutical engineering, the study of crystallization processes gains importance. An efficient analytical inline sensor could help to improve the knowledge about these processes in order to increase efficiency and yields. The in-situ microscope (ISM) is an optical sensor developed for the monitoring of bioprocesses. A new application for this sensor is the monitoring in downstream processes, e.g. the crystallization of proteins and other organic compounds. This contribution shows new aspects of using in-situ microscopy to monitor crystallization processes. Crystals of different chemical compounds were precipitated from supersaturated solutions and the crystal growth was monitored. Exemplified morphological properties and different forms of crystals could be distinguished on the basis of offline experiments. For inline monitoring of crystallization processes, a special 0.5 L stirred tank reactor was developed and equipped with the in-situ microscope. This reactor was utilized to carry out batch experiments for crystallizations of O-acetylsalicyclic acid (ASS) and hen egg white lysozyme (HEWL). During the whole crystallization process, the in-situ microscope system acquired images directly from the crystallization broth. For the data evaluation, an image analysis algorithm was developed and implemented in the microscope analysis software.

Curved crystals for high-resolution focusing of X and gamma rays through a Laue lens

NASA Astrophysics Data System (ADS)

Guidi, Vincenzo; Bellucci, Valerio; Camattari, Riccardo; Neri, Ilaria

2013-08-01

Crystals with curved diffracting planes have been investigated as high-efficiency optical components for the realization of a Laue lens for satellite-borne experiments in astrophysics. At Sensor and Semiconductor Laboratory (Ferrara, Italy) a research and development plan to implement Si and Ge curved crystals by surface grooving technique has been undertaken. The method of surface grooving allows obtaining Si and Ge curved crystals with self-standing curvature, i.e., with no need for external bending device, which is a mandatory issue in satellite-borne experiments. Si and Ge grooved crystals have been characterized by X-ray diffraction at ESRF and ILL to prove their functionality for a high-reflectivity Laue lens.

Antiurolithic activity of Origanum vulgare is mediated through multiple pathways

PubMed Central

2011-01-01

Background Origanum vulgare Linn has traditionally been used in the treatment of urolithiasis. Therefore, we investigated the crude extract of Origanum vulgare for possible antiurolithic effect, to rationalize its medicinal use. Methods The crude aqueous-methanolic extract of Origanum vulgare (Ov.Cr) was studied using the in vitro and in vivo methods. In the in vitro experiments, supersaturated solution of calcium and oxalate, kidney epithelial cell lines (MDCK) and urinary bladder of rabbits were used, whereas, in the in vivo studies, rat model of urolithiasis was used for the study of preventive and curative effect. Results In the in vitro experiments, Ov.Cr exhibited a concentration-dependent (0.25-4 mg/ml) inhibitory effect on the slope of nucleation and aggregation and also decreased the number of calcium oxalate monohydrate crystals (COM) produced in calcium oxalate metastable solutions. It also showed concentration-dependent antioxidant effect against DPPH free radical and lipid peroxidation induced in rat kidney tissue homogenate. Ov.Cr reduced the cell toxicity using MTT assay and LDH release in renal epithelial cells (MDCK) exposed to oxalate (0.5 mM) and COM (66 μg/cm2) crystals. Ov.Cr relaxed high K+ (80 mM) induced contraction in rabbit urinary bladder strips, and shifted the calcium concentration-response curves (CRCs) towards right with suppression of the maximum response similar to that of verapamil, a standard calcium channel blocker. In male Wistar rats receiving lithogenic treatment comprising of 0.75% ethylene glycol in drinking water given for 3 weeks along with ammonium chloride (NH4Cl) for the first 5 days, Ov.Cr treatment (10-30 mg/kg) prevented as well as reversed toxic changes including loss of body weight, polyurea, crystalluria, oxaluria, raised serum urea and creatinine levels and crystal deposition in kidneys compared to their respective controls. Conclusion These data indicating the antiurolithic activity in Ov.Cr, possibly mediated through inhibition of CaOx crystallization, antioxidant, renal epithelial cell protective and antispasmodic activities, rationalizes its medicinal use in urolithiasis. PMID:22004514

Controlled In Meso Phase Crystallization – A Method for the Structural Investigation of Membrane Proteins

PubMed Central

Kubicek, Jan; Schlesinger, Ramona; Baeken, Christian; Büldt, Georg; Schäfer, Frank; Labahn, Jörg

2012-01-01

We investigated in meso crystallization of membrane proteins to develop a fast screening technology which combines features of the well established classical vapor diffusion experiment with the batch meso phase crystallization, but without premixing of protein and monoolein. It inherits the advantages of both methods, namely (i) the stabilization of membrane proteins in the meso phase, (ii) the control of hydration level and additive concentration by vapor diffusion. The new technology (iii) significantly simplifies in meso crystallization experiments and allows the use of standard liquid handling robots suitable for 96 well formats. CIMP crystallization furthermore allows (iv) direct monitoring of phase transformation and crystallization events. Bacteriorhodopsin (BR) crystals of high quality and diffraction up to 1.3 Å resolution have been obtained in this approach. CIMP and the developed consumables and protocols have been successfully applied to obtain crystals of sensory rhodopsin II (SRII) from Halobacterium salinarum for the first time. PMID:22536388

Development of Active Control Method for Supercooling Releasing of Water

NASA Astrophysics Data System (ADS)

Mito, Daisuke; Kozawa, Yoshiyuki; Tanino, Masayuki; Inada, Takaaki

We have tested the prototype ice-slurry generator that enables both production of supercooled water (-2°C) and releasing of its supercooling simultaneously and continuously in a closed piping system. In the experiment, we adopted the irradiation of ultrasonic wave as an active control method of triggering for supercooling releasing, and evaluated the reliability for a practical use compared with the seed ice-crystal trigger. As the results, it has been confirmed that the ultrasonic wave trigger acts assuredly at the same level of degree of supercooling as that by using the seed ice-crystal Trigger. Moreover, it can be found that the ultrasonic wave trigger has the advantage of removing the growing ice-crystals on the pipe wall at the same time. Finally, we have specified the bombardment condition of ultrasonic wave enough to make continuously the ice-slurry in a closed system as the output surface power density > 31.4kW/m2 and the superficial bombardment time > 4.1sec. We have also demonstrated the continuous ice-slurry making for more than 6hours by using the refrigerator system with the practical scale of 88kW.

Crystallization of Calcium Carbonate in a Large Scale Field Study

NASA Astrophysics Data System (ADS)

Ueckert, Martina; Wismeth, Carina; Baumann, Thomas

2017-04-01

The long term efficiency of geothermal facilities and aquifer thermal energy storage in the carbonaceous Malm aquifer in the Bavarian Molasse Basin is seriously affected by precipitations of carbonates. This is mainly caused by pressure and temperature changes leading to oversaturation during production. Crystallization starts with polymorphic nuclei of calcium carbonate and is often described as diffusion-reaction controlled. Here, calcite crystallization is favoured by high concentration gradients while aragonite crystallization is occurring at high reaction rates. The factors affecting the crystallization processes have been described for simplified, well controlled laboratory experiments, the knowledge about the behaviour in more complex natural systems is still limited. The crystallization process of the polymorphic forms of calcium carbonate were investigated during a heat storage test at our test site in the eastern part of the Bavarian Molasse Basin. Complementary laboratory experiments in an autoclave were run. Both, field and laboratory experiments were conducted with carbonaceous tap water. Within the laboratory experiments additionally ultra pure water was used. To avoid precipitations of the tap water, a calculated amount of {CO_2} was added prior to heating the water from 45 - 110°C (laboratory) resp. 65 - 110°C (field). A total water volume of 0.5 L (laboratory) resp. 1 L (field) was immediately sampled and filtrated through 10 - 0.1

Synthesis, Characterization, and Crystallization of Syndiotactic Alternating Ethylene-Propylene Crystalline Copolymer and its Blends.

NASA Astrophysics Data System (ADS)

Chien, Haoyang

A syndiotactic alternating ethylene-propylene (SYN-ALT-EP) crystalline copolymer was synthesized by complete hydrogenation, using a diimide reduction, of syndiotactic cis-1,4-poly(pentadiene-1,3) (CIS-PPD). The microstructure was studied by both high resolution nuclear magnetic resonance (NMR) spectroscopy and also fourier transform infra-red (FTIR) spectroscopy. The number average length of syndiotactic sequences is about 69 which indicates a high degree of syndiotacticity (97%) in the microstructure of this copolymer. The single FTIR absorbance at 733 cm^{ -1} without any splitting suggests an alternating arrangement of ethylene and propylene units. The solution state characterization of SYN-ALT -EP was studied by gel permeation chromatography using on -line measurements of multi-angle laser light scattering (MALLS), single capillary viscosities (VISC), and concentrations by differential refractive index (DRI) detectors. The Mark-Houwink-Sakurada parameters of "K" and "a" in THF at 30^circC are determined to be 8.99 times 10^ {-5} and 0.8, respectively. The universal GPC calibration curve can be applied to this copolymer in THF at 30^circC. Two different molecular relaxation processes ( alpha and beta relaxations) were found via dynamic mechanical (DM) analysis below room temperature: an alpha relaxation (around -60^ circC) and a beta relaxation (around -125^circ C). The apparent activation energy of the alpha relaxation is 285 kJ/mol, and the activation energy of the beta relaxation is 43 kJ/mol based on the Arrhenius equation. Molecular motion in SYN-ALT-EP copolymer was probed by solid state ^{13}C NMR experiments. At temperatures above T_{rm g} there are two major molecular motions in this copolymer: a backbone motion (the rotational motion about single bonds) and a methyl side group rotation. The backbone motion is frozen below T_{rm g}, but the methyl rotation still occurs. As the temperature is further decreased to about -175 ^circC, well below the beta -transition observed in DM analysis, the methyl side group rotation slows down, suggesting that the methyl rotation may be associated with the observed beta relaxation process. The equilibrium melting temperature is 55 +/- 1^circC; the equilibrium heat of fusion is 8.8 +/- 0.3 kJ/mol. The overall crystallization kinetics show an Avrami exponent (n) that qualitatively increases with crystallization temperature during primary crystallization. The transition from Regime II to Regime III is observed near T_{rm c} = 26 ^circC based on linear crystal growth rate experiments. The fold surface free energy ( sigma_{rm e}) is determined to be 33 erg/cm^2. A monoclinic crystal unit cell was determined (a = 11.19A b = 11.82A c = 9.00A gamma = 67.03^circ) from the fiber pattern via wide angle x-ray diffraction experiments (WAXD). A banded spherulitic morphology was observed by polarized light microscopy (PLM) and transmission electron microscopy (TEM). Such texture is characteristic of the co-twisting of growing lamellae. The morphology changes from regularly banded spherulites to non-regularly banded spherulites and may be correlated with the Regime III to Regime II transition. A plate-like single crystal morphology was also observed by polarized light microscopy after a melt crystallization at small supercooling conditions. Blends of SYN-ALT-EP/IPP, SYN-ALT-EP/HDPE, and SYN-ALT-EP/LDPE were made and examined. Neither T _{rm g} shifting nor co-crystallization using different blending compositions were observed. Therefore, only limited, if any, miscibility exists in these blends.

Vibration Control of Deployable Astromast Boom: Preliminary Experiments

NASA Technical Reports Server (NTRS)

Swaminadham, M.; Hamilton, David A.

1994-01-01

This paper deals with the dynamic characterization of a flexible aerospace solar boom. The modeling issues and sine dwell vibration testing to determine natural frequencies and mode shapes of a continuous-longer on deployable ASTROMAST lattice boom are discussed. The details of the proof-of-concept piezoelectric active vibration experiments on a simple cantilever beam to control its vibrations are presented. The control parameters like voltage to the controller crystal and its location are investigated, to determine the effectiveness of control element to suppress selected resonant vibrations of the test specimen. Details of this experiment and plans for its future adaptation to the prototype structure are also discussed.

The role of superheating in the formation of Glass Mountain obsidians (Long Valley, CA) inferred through crystallization of sanidine

NASA Astrophysics Data System (ADS)

Waters, Laura E.; Andrews, Benjamin J.

2016-10-01

The Glass Mountain obsidians (Long Valley, CA) are crystal poor (<8 vol%) and highly evolved (high SiO2, low Sr), and therefore, their formation required extremely efficient separation of melts from a crystal-rich source. A petrologic and experimental investigation of the mineral phases in Glass Mountain lavas identifies conditions under which phenocrysts grew and the driving mechanism for crystallization, which places constraints on the possible processes that generated the obsidians. The obsidian in this study (GM-11) is saturated in nine phases (sanidine + quartz + plagioclase + titanomagnetite + ilmenite + zircon + apatite + allanite + biotite), and results of high-resolution SEM compositional mapping and electron microprobe analysis reveal that individual sanidine crystals are normally zoned and span a range of compositions (Or40-78). Sanidines have a "granophyric" texture, characterized by intergrowths of quartz and sanidine. Mineral phases in the natural sample are compared to H2O-saturated phase equilibrium experiments conducted in cold-seal pressure vessels, over a range of conditions (700-850 °C; 75-225 MPa), and all are found to be plausible phenocrysts. Comparison of sanidine compositions from the natural sample with those grown in phase equilibrium experiments demonstrates that sanidine in the natural sample occurs in a reduced abundance. Further comparison with phase equilibrium experiments suggests that sanidine compositions track progressive loss of dissolved melt water (±cooling), suggesting that crystallization in the natural obsidian was driven predominantly by degassing resulting from decompression. It is paradoxical that an effusively (slowly) erupted lava should contain multiple phenocryst phases, including sanidine crystals that span a range of compositions with granophyric textures, and yet remain so crystal poor. To resolve this paradox, it is necessary that the solidification mechanism (degassing or cooling) that produced the sanidine crystals (and other mineral phases) must have an associated kinetic effect(s) that efficiently hinders crystal nucleation and growth. Decompression experiments conducted in this study and from the literature collectively demonstrate that the simplest way to inhibit nucleation during degassing-induced crystallization is to initiate degassing ± cooling from superliquidus conditions, and therefore, the Glass Mountain obsidians were superheated prior to crystallization.

Peculiarities of Crystallization of the Restriction Endonuclease EcoRII

NASA Technical Reports Server (NTRS)

Karpove, Elizaveta; Pusey, M.arc L.

1998-01-01

Nucleases interfere with most standard molecular biology procedures. We have purified and crystallized the restriction endonuclease EcoRII, which belongs to the type II of restriction- modification enzyme, to study the protein crystallization process using a "non standard" macromolecule. A procedure for the purification of EcoRII was developed and 99% pure protein as determined by SDS PAGE electrophoresis obtained. Light scattering experiments were performed to assist in screening protein suitable crystallization conditions. The second virial coefficient was determined as a function of precipitating salt concentration, using sodium chloride, ammonium sulfate, and sodium sulfate. Small (maximum size approximately 0.2 mm) well shaped crystals have been obtained. Larger poorly formed crystals (ca 0.5 mm) have also been obtained, but we have been unable to mount them for diff-raction analysis due to their extreme fragility. Crystallization experiments with PEG have shown that using this precipitant, the best crystals are obtained from slightly over-saturated solutions. Use of higher precipitant concentration leads to dendritic crystal formation. EcoRII is difficult to solubilize and meticulous attention must be paid to the presence of reducing agents.

(PCG) Protein Crystal Growth Horse Serum Albumin

NASA Technical Reports Server (NTRS)

1995-01-01

Horse Serum Albumin crystals grown during the USML-1 (STS-50) mission's Protein Crystal Growth Glovebox Experiment. These crystals were grown using a vapor diffusion technique at 22 degrees C. The crystals were allowed to grow for nine days while in orbit. Crystals of 1.0 mm in length were produced. The most abundant blood serum protein, regulates blood pressure and transports ions, metabolites, and therapeutic drugs. Principal Investigator was Edward Meehan.

A novel microseeding method for the crystallization of membrane proteins in lipidic cubic phase.

PubMed

Kolek, Stefan Andrew; Bräuning, Bastian; Stewart, Patrick Douglas Shaw

2016-04-01

Random microseed matrix screening (rMMS), in which seed crystals are added to random crystallization screens, is an important breakthrough in soluble protein crystallization that increases the number of crystallization hits that are available for optimization. This greatly increases the number of soluble protein structures generated every year by typical structural biology laboratories. Inspired by this success, rMMS has been adapted to the crystallization of membrane proteins, making LCP seed stock by scaling up LCP crystallization conditions without changing the physical and chemical parameters that are critical for crystallization. Seed crystals are grown directly in LCP and, as with conventional rMMS, a seeding experiment is combined with an additive experiment. The new method was used with the bacterial integral membrane protein OmpF, and it was found that it increased the number of crystallization hits by almost an order of magnitude: without microseeding one new hit was found, whereas with LCP-rMMS eight new hits were found. It is anticipated that this new method will lead to better diffracting crystals of membrane proteins. A method of generating seed gradients, which allows the LCP seed stock to be diluted and the number of crystals in each LCP bolus to be reduced, if required for optimization, is also demonstrated.

Modeling of Macroscopic/Microscopic Transport and Growth Phenomena in Zeolite Crystal Solutions Under Microgravity Conditions

NASA Technical Reports Server (NTRS)

Gatsonis, Nikos A.; Alexandrou, Andreas; Shi, Hui; Ongewe, Bernard; Sacco, Albert, Jr.

1999-01-01

Crystals grown from liquid solutions have important industrial applications. Zeolites, for instance, a class of crystalline aluminosilicate materials, form the backbone of the chemical process industry worldwide, as they are used as adsorbents and catalysts. Many of the phenomena associated with crystal growth processes are not well understood due to complex microscopic and macroscopic interactions. Microgravity could help elucidate these phenomena and allow the control of defect locations, concentration, as well as size of crystals. Microgravity in an orbiting spacecraft could help isolate the possible effects of natural convection (which affects defect formation) and minimize sedimentation. In addition, crystals will stay essentially suspended in the nutrient pool under a diffusion-limited growth condition. This is expected to promote larger crystals by allowing a longer residence time in a high-concentration nutrient field. Among other factors, the crystal size distribution depends on the nucleation rate and crystallization. These two are also related to the "gel" polymerization/depolymerization rate. Macroscopic bulk mass and flow transport and especially gravity, force the crystals down to the bottom of the reactor, thus forming a sedimentation layer. In this layer, the growth rate of the crystals slows down as crystals compete for a limited amount of nutrients. The macroscopic transport phenomena under certain conditions can, however, enhance the nutrient supply and therefore, accelerate crystal growth. Several zeolite experiments have been performed in space with mixed results. The results from our laboratory have indicated an enhancement in size of 30 to 70 percent compared to the best ground based controls, and a reduction of lattice defects in many of the space grown crystals. Such experiments are difficult to interpret, and cannot be easily used to derive empirical or other laws since many physical parameters are simultaneously involved in the process. At the same time, however, there is increased urgency to develop such an understanding in order to more accurately quantify the process. In order to better understand the results obtained from our prior space experiments, and design future experiments, a detailed fluid dynamic model simulating the crystal growth mechanism is required. This will not only add to the fundamental knowledge on the crystallization of zeolites, but also be useful in predicting the limits of size and growth of these important industrial materials. Our objective is to develop macro/microscopic theoretical and computational models to study the effect of transport phenomena in the growth of crystals grown in solutions. Our effort has concentrated so far in the development of separate macroscopic and microscopic models. The major highlights of our accomplishments are described.

Fast ultrasonic wavelength tuning in X-ray experiment

DOE Office of Scientific and Technical Information (OSTI.GOV)

Blagov, A. E., E-mail: blagov-ae@mail.ru; Pisarevskii, Yu. V.; Koval’chuk, M. V.

2016-03-15

A method of tuning (scanning) X-ray beam wavelength based on modulation of the lattice parameter of X-ray optical crystal by an ultrasonic standing wave excited in it has been proposed and experimentally implemented. The double-crystal antiparallel scheme of X-ray diffraction, in which an ultrasonic wave is excited in the second crystal, is used in the experiment. The profile of characteristic line k{sub α1} of an X-ray tube with a molybdenum anode is recorded using both the proposed tuning scheme and conventional mechanical rotation of crystal. The results obtained by both techniques are in good agreement.

Timing and tracking for the Crystal Barrel detector

NASA Astrophysics Data System (ADS)

Beck, Reinhard; Brinkmann, Kai; Novotny, Rainer

2017-01-01

The aim of the project D.3 is the upgrade of several detector components used in the CBELSA/TAPS experiment at ELSA. The readout of the Crystal Barrel Calorimeter will be extended by a timing branch in order to gain trigger capability for the detector, which will allow to measure completely neutral final states in photoproduction reactions (see projects A.1 and C.5). Additionally, the readout of the inner crystals of the TAPS detector, which covers the forward opening of the Crystal Barrel Calorimeter, will be modified to be capable of high event rates due to the intensity upgrade of ELSA. Furthermore, a full-scale prototype Time Projection Chamber (TPC) has been built to be used as a new central tracker for the CBELSA/TAPS experiment at ELSA and the FOPI experiment at GSI.

High-Temperature Controlled Redox Crystallization Studies

NASA Technical Reports Server (NTRS)

Williams, R. J.

1985-01-01

The crystallization of silicates containing redox sensitive ions (e.g., Fe, Ti, Ce) must be performed under controlled and known redox conditions in order to obtain the maximum scientific benefit from experimental study. Furthermore, many compositions crystallize dense phases which settle during ground-based experiments. This settling influences the texture and chemical evolution of the crystallizing system. The purpose of this investigation is to develop a test system in which controlled redox experiments can be performed in the microgravity environment. The system will use solid ceramic oxygen electrolyte cells for control, measurements, and production of the required redox conditions. A preliminary design for a prototype is developed, the electrolyte and furnace tested, and a tentative protocol for experiment developed. The control parameter is to be established and a laboratory prototype built.

Astronaut Scott Parazynski works with PCG experiment on middeck

NASA Image and Video Library

1994-11-14

STS066-13-029 (3-14 Nov 1994) --- On the Space Shuttle Atlantis' mid-deck, astronaut Scott E. Parazynski, mission specialist, works at one of two areas onboard the Shuttle which support the Protein Crystal Growth (PCG) experiment. This particular section is called the Vapor Diffusion Apparatus (VDA), housed in a Single Locker Thermal Enclosure (STES). Together with the Crystal Observation System, housed in the Thermal Enclosure System (COS/TES) the VDA represents the continuing research into the structures of proteins and other macromolecules such as viruses. In addition to using the microgravity of space to grow high-quality protein crystals for structural analyses, the experiments are expected to help develop technologies and methods to improve the protein crystallization process on Earth as well as in space.

Topological defects in a living nematic ensnare swimming bacteria [Linking bacterial motility and liquid crystallinity in a model of living nematic

DOE Office of Scientific and Technical Information (OSTI.GOV)

Genkin, Mikhail Mikhailovich; Sokolov, Andrey; Lavrentovich, Oleg D.

Active matter exemplified by suspensions of motile bacteria or synthetic self-propelled particles exhibits a remarkable propensity to self-organization and collective motion. The local input of energy and simple particle interactions often lead to complex emergent behavior manifested by the formation of macroscopic vortices and coherent structures with long-range order. A realization of an active system has been conceived by combining swimming bacteria and a lyotropic liquid crystal. Here, by coupling the well-established and validated model of nematic liquid crystals with the bacterial dynamics, we develop a computational model describing intricate properties of such a living nematic. In faithful agreement withmore » the experiment, the model reproduces the onset of periodic undulation of the director and consequent proliferation of topological defects with the increase in bacterial concentration. It yields a testable prediction on the accumulation of bacteria in the cores of +1/2 topological defects and depletion of bacteria in the cores of -1/2 defects. Our dedicated experiment on motile bacteria suspended in a freestanding liquid crystalline film fully confirms this prediction. Lastly, our findings suggest novel approaches for trapping and transport of bacteria and synthetic swimmers in anisotropic liquids and extend a scope of tools to control and manipulate microscopic objects in active matter.« less

Topological defects in a living nematic ensnare swimming bacteria [Linking bacterial motility and liquid crystallinity in a model of living nematic

DOE PAGES

Genkin, Mikhail Mikhailovich; Sokolov, Andrey; Lavrentovich, Oleg D.; ...

2017-03-08

Active matter exemplified by suspensions of motile bacteria or synthetic self-propelled particles exhibits a remarkable propensity to self-organization and collective motion. The local input of energy and simple particle interactions often lead to complex emergent behavior manifested by the formation of macroscopic vortices and coherent structures with long-range order. A realization of an active system has been conceived by combining swimming bacteria and a lyotropic liquid crystal. Here, by coupling the well-established and validated model of nematic liquid crystals with the bacterial dynamics, we develop a computational model describing intricate properties of such a living nematic. In faithful agreement withmore » the experiment, the model reproduces the onset of periodic undulation of the director and consequent proliferation of topological defects with the increase in bacterial concentration. It yields a testable prediction on the accumulation of bacteria in the cores of +1/2 topological defects and depletion of bacteria in the cores of -1/2 defects. Our dedicated experiment on motile bacteria suspended in a freestanding liquid crystalline film fully confirms this prediction. Lastly, our findings suggest novel approaches for trapping and transport of bacteria and synthetic swimmers in anisotropic liquids and extend a scope of tools to control and manipulate microscopic objects in active matter.« less

Changes in copper sulfate crystal habit during cooling crystallization

NASA Astrophysics Data System (ADS)

Giulietti, M.; Seckler, M. M.; Derenzo, S.; Valarelli, J. V.

1996-09-01

The morphology of technical grade copper(II) sulfate pentahydrate crystals produced from batch cooling experiments in the temperature range of 70 to 30°C is described and correlated with the process conditions. A slow linear cooling rate (batch time of 90 min) predominantly caused the appearance of well-formed crystals. Exponential cooling (120 min) resulted in the additional formation of agglomerates and twins. The presence of seeds for both cooling modes led to round crystals, agglomerates and twins. Fast linear cooling (15 min) gave rise to a mixture of the former types. Broken crystals and adhering fragments were often found. Growth zoning was pronounced in seeded and linear cooling experiments. Fluid inclusions were always found and were more pronounced for larger particles. The occurrence of twinning, zoning and fluid inclusions was qualitatively explained in terms of fundamental principles.

CRYSTAL: The Cirrus Regional Study of Tropical Anvils and Layers

NASA Technical Reports Server (NTRS)

Delnore, Victor E.; Cox, Stephen K.; Curran, Robert J.

1999-01-01

CRYSTAL the Cirrus Regional Study of Tropical Anvils and Layers is part of the ongoing series of field experiments to study clouds and their impact on world weather and climate, and will attempt to improve the application of cloud effects in global climate models. CRYSTAL is being planned as two parts: a limited CRYSTAL field campaign in 2001 to examine towering clouds and anvil genesis over the Everglades of Florida, and the main CRYSTAL field campaign in the summer of 2003 in the Tropical Western Pacific. The latter is timed to take advantage of several cloud measurement satellites that will be operational at that time. This paper discusses some of the issues to be addressed in CRYSTAL, gives a brief description of the research plan, and describes its relationship to other important field experiments.

Ice forming experiment

NASA Technical Reports Server (NTRS)

Vali, G.

1982-01-01

A low gravity experiment to assess the effect of the presence of supercooled cloud droplets on the diffusional growth rate of ice crystals is described. The theoretical work and the feasibility studies are summarized. The nucleation of ice crystals in supercooled clouds is also discussed.

Plasma Crystal-3 Plus experiment Chamber Leak Check

NASA Image and Video Library

2010-07-01

ISS024-E-007144 (1 July 2010) --- Russian cosmonaut Alexander Skvortsov, Expedition 24 commander, performs chamber leak checks on the new Plasma Crystal-3 Plus experiment in the Poisk Mini-Research Module 2 (MRM2) of the International Space Station.

Kotov works with Plasma Crystal-3+ Experiment in the SM during Expedition 22

NASA Image and Video Library

2010-01-28

ISS022-E-040614 (28 Jan. 2010) --- Russian cosmonaut Oleg Kotov, Expedition 22 flight engineer, is pictured while working with the Plasma Crystal-3 experiment in the Zvezda Service Module of the International Space Station.

Kotov works with Plasma Crystal-3 Experiment in the SM during Expedition 22

NASA Image and Video Library

2010-01-25

ISS022-E-035439 (25 Jan. 2010) --- Russian cosmonaut Oleg Kotov, Expedition 22 flight engineer, is pictured while working with the Plasma Crystal-3 experiment in the Zvezda Service Module of the International Space Station.

Kotov works with Plasma Crystal-3 Experiment in the SM during Expedition 22

NASA Image and Video Library

2010-01-25

ISS022-E-035438 (25 Jan. 2010) --- Russian cosmonaut Oleg Kotov, Expedition 22 flight engineer, uses a computer while servicing the Plasma Crystal-3 experiment in the Zvezda Service Module of the International Space Station.

Kotov works with Plasma Crystal-3+ Experiment in the SM during Expedition 22

NASA Image and Video Library

2010-01-28

ISS022-E-040617 (28 Jan. 2010) --- Russian cosmonaut Oleg Kotov, Expedition 22 flight engineer, is pictured while working with the Plasma Crystal-3 experiment in the Zvezda Service Module of the International Space Station.

Kotov works with Plasma Crystal-3+ Experiment in the SM during Expedition 22

NASA Image and Video Library

2010-01-28

ISS022-E-040615 (28 Jan. 2010) --- Russian cosmonaut Oleg Kotov, Expedition 22 flight engineer, uses a computer while servicing the Plasma Crystal-3 experiment in the Zvezda Service Module of the International Space Station.

Skylab M518 multipurpose furnace convection analysis

NASA Technical Reports Server (NTRS)

Bourgeois, S. V.; Spradley, L. W.

1975-01-01

An analysis was performed of the convection which existed on ground tests and during skylab processing of two experiments: vapor growth of IV-VI compounds growth of spherical crystals. A parallel analysis was also performed on Skylab experiment indium antimonide crystals because indium antimonide (InSb) was used and a free surface existed in the tellurium-doped Skylab III sample. In addition, brief analyses were also performed of the microsegregation in germanium experiment because the Skylab crystals indicated turbulent convection effects. Simple dimensional analysis calculations and a more accurate, but complex, convection computer model, were used in the analysis.

KSC-97PC1382

NASA Image and Video Library

1997-09-08

United States Microgravity Payload-4 (USMP-4) experiments are prepared to be flown on Space Shuttle mission STS-87 in the Space Station Processing Facility at Kennedy Space Center (KSC). This horizontal tube is known as MEPHISTO, the French acronym for a cooperative American-French investigation of the fundamentals of crystal growth. This experiment, designed for the study of solidification (or freezing) during the growth cycle of liquid materials used for semiconductor crystals, aims to aid in the development of techniques for growing higher quality crystals on Earth. All STS-87 experiments are scheduled for launch on Nov. 19 from KSC

ACTIVE MEDIA: BaY2F8 single crystals doped with rare-earth ions as promising up-conversion media for UV and VUV lasers

NASA Astrophysics Data System (ADS)

Pushkar', A. A.; Uvarova, T. V.; Molchanov, V. N.

2008-04-01

BaY2F8 crystals are studied as promising active media for UV and VUV lasers. The up-conversion pumping of rare-earth activators is proposed to solve problems related to the solarisation of the medium and the selection of pump sources. The technology of growing oriented BaY2F8 single crystals is developed and the influence of the crystal orientation on the growth rate and quality of single crystals is determined.

Structure and crystallization of SiO2 and B2O3 doped lithium disilicate glasses from theory and experiment.

PubMed

Erlebach, Andreas; Thieme, Katrin; Sierka, Marek; Rüssel, Christian

2017-09-27

Solid solutions of SiO 2 and B 2 O 3 in Li 2 O·2SiO 2 are synthesized and characterized for the first time. Their structure and crystallization mechanisms are investigated employing a combination of simulations at the density functional theory level and experiments on the crystallization of SiO 2 and B 2 O 3 doped lithium disilicate glasses. The remarkable agreement of calculated and experimentally determined cell parameters reveals the preferential, kinetically controlled incorporation of [SiO 4 ] and [BO 4 ] at the Li + lattice sites of the Li 2 O·2SiO 2 crystal structure. While the addition of SiO 2 increases the glass viscosity resulting in lower crystal growth velocities, glasses containing B 2 O 3 show a reduction of both viscosities and crystal growth velocities. These observations could be rationalized by a change of the chemical composition of the glass matrix surrounding the precipitated crystal phase during the course of crystallization, which leads to a deceleration of the attachment of building units required for further crystal growth at the liquid-crystal interface.

STS-34: Mission Overview Briefing

NASA Technical Reports Server (NTRS)

1989-01-01

Live footage shows Milt Heflin, the Lead Flight Director participating in the STS-34 Mission Briefing. He addresses the primary objective, and answered questions from the audience and other NASA Centers. Heflin also mentions the Shuttle Solar Backscatter Ultraviolet secondary payload, and several experiments. These experiments include Growth Hormone Crystal Distribution (Plants), Polymer Morphology, Sensor Technology Experiment, Mesoscale Lightning Experiment, Shuttle Student Involvement Program "Ice Crystals", and the Air Force Maui Optical Site.

Liquid Crystals: The Phase of the Future.

ERIC Educational Resources Information Center

Ondris-Crawford, Renate; And Others

1992-01-01

Liquid crystal displays are currently utilized to convey information via graphic displays. Presents experiments and explanations that employ the concept of liquid crystals to learn concepts related to the various states of matter, electric and magnetic forces, refraction of light, and optics. Discusses applications of liquid crystal technology.…

Support of research in X-ray astronomy

NASA Technical Reports Server (NTRS)

Garmire, G.

1983-01-01

Activities described include: (1) the evaluation of CCD detectors for X-ray astronomy applications; (2) contributions to the development of an imaging gas scintillation proportional counter; (3) the evaluation of certain metal oxide crystals as potential radiation detectors; (4) optical observations and searches for X-ray sources discovered by the HEAO-1 A2 experiment; and (5) theoretical modeling of nonequilibrium ionization structure of supernova remnants.

Activator anion binding site in pyridoxal phosphorylase b: the binding of phosphite, phosphate, and fluorophosphate in the crystal.

PubMed Central

Oikonomakos, N. G.; Zographos, S. E.; Tsitsanou, K. E.; Johnson, L. N.; Acharya, K. R.

1996-01-01

It has been established that phosphate analogues can activate glycogen phosphorylase reconstituted with pyridoxal in place of the natural cofactor pyridoxal 5'-phosphate (Change YC. McCalmont T, Graves DJ. 1983. Biochemistry 22:4987-4993). Pyridoxal phosphorylase b has been studied by kinetic, ultracentrifugation, and X-ray crystallographic experiments. In solution, the catalytically active species of pyridoxal phosphorylase b adopts a conformation that is more R-state-like than that of native phosphorylase b, but an inactive dimeric species of the enzyme can be stabilized by activator phosphite in combination with the T-state inhibitor glucose. Co-crystals of pyridoxal phosphorylase b complexed with either phosphite, phosphate, or fluorophosphate, the inhibitor glucose, and the weak activator IMP were grown in space group P4(3)2(1)2, with native-like unit cell dimensions, and the structures of the complexes have been refined to give crystallographic R factors of 18.5-19.2%, for data between 8 and 2.4 A resolution. The anions bind tightly at the catalytic site in a similar but not identical position to that occupied by the cofactor 5'-phosphate group in the native enzyme (phosphorus to phosphorus atoms distance = 1.2 A). The structural results show that the structures of the pyridoxal phosphorylase b-anion-glucose-IMP complexes are overall similar to the glucose complex of native T-state phosphorylase b. Structural comparisons suggest that the bound anions, in the position observed in the crystal, might have a structural role for effective catalysis. PMID:8976550

Probing antioxidant activity of 2'-hydroxychalcones: crystal and molecular structures, in vitro antiproliferative studies and in vivo effects on glucose regulation.

PubMed

Rossi, Miriam; Caruso, Francesco; Crespi, Erica J; Pedersen, Jens Z; Nakano, Gail; Duong, Michelle; McKee, Celia; Lee, Sharon; Jiwrajka, Manasi; Caldwell, Charles; Baffour, Francis; Karlin, Dylan Alex; Lidoff, Genevieve; Leone, Stefano; Balducci, Valentina; Miler, Jaroslav; Incerpi, Sandra

2013-10-01

In order to better understand the antioxidant behavior of a series of polyphenolic 2'-hydroxychalcones, we describe the results of several chemical and biological studies, in vitro and in vivo. Single crystal X-ray methods elucidated their molecular structures and important intermolecular interactions such as H-bonding and molecular stacking in the crystal structures that contribute to our knowledge in explaining antioxidant activity. The results of experiments using the 1,1-diphenyl-2-dipicrylhydrazyl (DPPH) UV-vis spectroscopic method indicate that a hydroxyl group in position 5' induces the highest antioxidant activity. Consequently, 2,2',5'-trihydroxychalcone was selected for further study in vitro towards ROS scavenging in L-6 myoblasts and THP-1 human monocytes, where it shows an excellent antioxidant activity in a concentration range lower than that reported by most studies of related molecules. In addition, this chalcone shows a very selective activity: it inhibits the proliferation of leukemic cells, but it does not affect the normal L-6 myoblasts and human fibroblasts. In studying 2,2',5'-trihydroxychalcone's effect on weight gain and serum glucose and insulin levels in Zucker fatty (fa(-)/fa(-)) rats we found that supplementing the diet with a 10 mg/kg dose of this chalcone (3 times weekly) blunted the increase in glucose that co-occurs with weight gain over the 6-week treatment period. It is concluded that 2,2',5'-trihydroxychalcone has the potential to serve as a protective agent for some debilitating diseases. Copyright © 2013 Elsevier Masson SAS. All rights reserved.

A novel fabrication of Cu{sub 2}O@Cu{sub 7}S{sub 4} core-shell micro/nanocrystals from Cu{sub 2}O temples and enhanced photocatalytic activities

DOE Office of Scientific and Technical Information (OSTI.GOV)

Li, Junqi, E-mail: sfmlab@163.com; Sun, Long; Yan, Ying

2016-08-15

Highlights: • The Cu{sub 2}O@Cu{sub 7}S{sub 4} core-shell crystals maintained the same morphology with template. • The crystals exhibit enhanced photocatalytic activity than the pure Cu{sub 2}O crystals. • The photocatalytic activity of different R crystals is diverse from each other. • A possible formation mechanism has been proposed. - Abstract: Uniform and monodispersed Cu{sub 2}O@Cu{sub 7}S{sub 4} core-shell micro/nanocrystals have been synthesized successfully at room temperature via a simple chemical etching reaction, using Cu{sub 2}O as sacrificial template. The structure and properties of the crystals were characterized by X-ray diffraction (XRD), scanning electron microscope (SEM), transmission electron microscopy (TEM),more » X-ray photoelectron spectra (XPS). The photocatalytic activity of the Cu{sub 2}O@Cu{sub 7}S{sub 4} crystals was evaluated by photocatalytic decolorization of MeO (methyl orange) aqueous solution at ambient temperature under visible-light irradiation. The results show that the as-prepared Cu{sub 2}O@Cu{sub 7}S{sub 4} crystals revealed core-shell structure, which maintained the same morphology with corresponding template and were composed of cuboctahedron Cu{sub 7}S{sub 4} shell and active Cu{sub 2}O core. Due to the unique Cu{sub 2}O@Cu{sub 7}S{sub 4} core-shell structure, the crystals exhibit enhanced photocatalytic activity than that of the pure Cu{sub 2}O crystals, and the photocatalytic activity of different R crystals is diverse from each other. A possible formation mechanism has been proposed.« less

Assessment of microcrystal quality by transmission electron microscopy for efficient serial femtosecond crystallography.

PubMed

Barnes, Christopher O; Kovaleva, Elena G; Fu, Xiaofeng; Stevenson, Hilary P; Brewster, Aaron S; DePonte, Daniel P; Baxter, Elizabeth L; Cohen, Aina E; Calero, Guillermo

2016-07-15

Serial femtosecond crystallography (SFX) employing high-intensity X-ray free-electron laser (XFEL) sources has enabled structural studies on microcrystalline protein samples at non-cryogenic temperatures. However, the identification and optimization of conditions that produce well diffracting microcrystals remains an experimental challenge. Here, we report parallel SFX and transmission electron microscopy (TEM) experiments using fragmented microcrystals of wild type (WT) homoprotocatechuate 2,3-dioxygenase (HPCD) and an active site variant (H200Q). Despite identical crystallization conditions and morphology, as well as similar crystal size and density, the indexing efficiency of the diffraction data collected using the H200Q variant sample was over 7-fold higher compared to the diffraction results obtained using the WT sample. TEM analysis revealed an abundance of protein aggregates, crystal conglomerates and a smaller population of highly ordered lattices in the WT sample as compared to the H200Q variant sample. While not reported herein, the 1.75 Å resolution structure of the H200Q variant was determined from ∼16 min of beam time, demonstrating the utility of TEM analysis in evaluating sample monodispersity and lattice quality, parameters critical to the efficiency of SFX experiments. Copyright © 2016 Elsevier Inc. All rights reserved.

Impurity effect of iron(III) on the growth of potassium sulfate crystal in aqueous solution

NASA Astrophysics Data System (ADS)

Kubota, Noriaki; Katagiri, Ken-ichi; Yokota, Masaaki; Sato, Akira; Yashiro, Hitoshi; Itai, Kazuyoshi

1999-01-01

Growth rates of the {1 1 0} faces of a potassium sulfate crystal were measured in a flow cell in the presence of traces of impurity Fe(III) (up to 2 ppm) over the range of pH=2.5-6.0. The growth rate was significantly suppressed by the impurity. The effect became stronger as the impurity concentration was increased and at pH<5. It became weaker with increasing supersaturation. It also became weaker as the pH was increased and at pH>5 it finally disappeared completely. The concentration and supersaturation effects on the impurity action were reasonably explained with a model proposed by Kubota and Mullin [J. Crystal Growth, 152 (1995) 203]. The surface coverage of the active sites by Fe(III) is estimated to increase linearly on increasing its concentration in solution in the range examined by growth experiments. The impurity effectiveness factor is confirmed to increase inversely proportional to the supersaturation as predicted by the model. Apart from the discussion based on the model, the pH effect on the impurity action is qualitatively explained by assuming that the first hydrolysis product of aqua Fe(III) complex compound, [Fe(H 2O) 5(OH)] 2+, is both growth suppression and adsorption active, but the second hydrolysis product, [Fe(H 2O) 4(OH) 2] +, is only adsorption active.

Cohesive finite element modeling of the delamination of HTPB binder and HMX crystals under tensile loading

DOE Office of Scientific and Technical Information (OSTI.GOV)

Walters, David J.; Luscher, Darby J.; Yeager, John D.

Accurately modeling the mechanical behavior of the polymer binders and the degradation of interfaces between binder and crystal is important to science-based understanding of the macro-scale response of polymer bonded explosives. The paper presents a description of relatively a simple bi-crystal HMX-HTPB specimen and associated tensile loading experiment including computed tomography imaging, the pertinent constitutive theory, and details of numerical simulations used to infer the behavior of the material during the delamination process. Within this work, mechanical testing and direct numerical simulation of this relatively simple bi-crystal system enabled reasonable isolation of binder-crystal interface delamination, in which the effects ofmore » the complicated thermomechanical response of explosive crystals were minimized. Cohesive finite element modeling of the degradation and delamination of the interface between a modified HTPB binder and HMX crystals was used to reproduce observed results from tensile loading experiments on bi-crystal specimens. Several comparisons are made with experimental measurements in order to identify appropriate constitutive behavior of the binder and appropriate parameters for the cohesive traction-separation behavior of the crystal-binder interface. This research demonstrates the utility of directly modeling the delamination between binder and crystal within crystal-binder-crystal tensile specimen towards characterizing the behavior of these interfaces in a manner amenable to larger scale simulation of polycrystalline PBX materials. One critical aspect of this approach is micro computed tomography imaging conducted during the experiments, which enabled comparison of delamination patterns between the direct numerical simulation and actual specimen. In addition to optimizing the cohesive interface parameters, one important finding from this investigation is that understanding and representing the strain-hardening plasticity of HTPB binder is important within the context of using a cohesive traction-separation model for the delamination of a crystal-binder system.« less

Cohesive finite element modeling of the delamination of HTPB binder and HMX crystals under tensile loading

DOE PAGES

Walters, David J.; Luscher, Darby J.; Yeager, John D.; ...

2018-02-27

Accurately modeling the mechanical behavior of the polymer binders and the degradation of interfaces between binder and crystal is important to science-based understanding of the macro-scale response of polymer bonded explosives. The paper presents a description of relatively a simple bi-crystal HMX-HTPB specimen and associated tensile loading experiment including computed tomography imaging, the pertinent constitutive theory, and details of numerical simulations used to infer the behavior of the material during the delamination process. Within this work, mechanical testing and direct numerical simulation of this relatively simple bi-crystal system enabled reasonable isolation of binder-crystal interface delamination, in which the effects ofmore » the complicated thermomechanical response of explosive crystals were minimized. Cohesive finite element modeling of the degradation and delamination of the interface between a modified HTPB binder and HMX crystals was used to reproduce observed results from tensile loading experiments on bi-crystal specimens. Several comparisons are made with experimental measurements in order to identify appropriate constitutive behavior of the binder and appropriate parameters for the cohesive traction-separation behavior of the crystal-binder interface. This research demonstrates the utility of directly modeling the delamination between binder and crystal within crystal-binder-crystal tensile specimen towards characterizing the behavior of these interfaces in a manner amenable to larger scale simulation of polycrystalline PBX materials. One critical aspect of this approach is micro computed tomography imaging conducted during the experiments, which enabled comparison of delamination patterns between the direct numerical simulation and actual specimen. In addition to optimizing the cohesive interface parameters, one important finding from this investigation is that understanding and representing the strain-hardening plasticity of HTPB binder is important within the context of using a cohesive traction-separation model for the delamination of a crystal-binder system.« less

Monitoring and modeling of ultrasonic wave propagation in crystallizing mixtures

NASA Astrophysics Data System (ADS)

Marshall, T.; Challis, R. E.; Tebbutt, J. S.

2002-05-01

The utility of ultrasonic compression wave techniques for monitoring crystallization processes is investigated in a study of the seeded crystallization of copper II sulfate pentahydrate from aqueous solution. Simple models are applied to predict crystal yield, crystal size distribution and the changing nature of the continuous phase. A scattering model is used to predict the ultrasonic attenuation as crystallization proceeds. Experiments confirm that modeled attenuation is in agreement with measured results.

Fragment-based screen against HIV protease.

PubMed

Perryman, Alexander L; Zhang, Qing; Soutter, Holly H; Rosenfeld, Robin; McRee, Duncan E; Olson, Arthur J; Elder, John E; Stout, C David

2010-03-01

We have employed a fragment-based screen against wild-type (NL4-3) HIV protease (PR) using the Active Sight fragment library and X-ray crystallography. The experiments reveal two new binding sites for small molecules. PR was co-crystallized with fragments, or crystals were soaked in fragment solutions, using five crystal forms, and 378 data sets were collected to 2.3-1.3 A resolution. Fragment binding induces a distinct conformation and specific crystal form of TL-3 inhibited PR during co-crystallization. One fragment, 2-methylcyclohexanol, binds in the 'exo site' adjacent to the Gly(16)Gly(17)Gln(18)loop where the amide of Gly(17)is a specific hydrogen bond donor, and hydrophobic contacts occur with the side chains of Lys(14)and Leu(63). Another fragment, indole-6-carboxylic acid, binds on the 'outside/top of the flap' via hydrophobic contacts with Trp(42), Pro(44), Met(46), and Lys(55), a hydrogen bond with Val(56), and a salt-bridge with Arg(57). 2-acetyl-benzothiophene also binds at this site. This study is the first fragment-based crystallographic screen against HIV PR, and the first time that fragments were screened against an inhibitor-bound drug target to search for compounds that both bind to novel sites and stabilize the inhibited conformation of the target.

Fragment-Based Screen against HIV Protease

PubMed Central

Perryman, A. L.; Zhang, Q.; Soutter, H. H.; Rosenfeld, R.; McRee, D. E.; Olson, A. J.; Elder, J. E.; Stout, C. D.

2009-01-01

We have employed a fragment-based screen against wild-type (NL4-3) HIV protease (PR) using the Active Sight fragment library and X-ray crystallography. The experiments reveal two new binding sites for small molecules. PR was co-crystallized with fragments, or crystals were soaked in fragment solutions, using five crystal forms, and 378 data sets were collected to 2.3-1.3 Å resolution. Fragment binding induces a distinct conformation and specific crystal form of TL-3 inhibited PR during co-crystallization. One fragment, 2-methylcyclohexanol, binds in the ‘exo site’ adjacent to the Gly16Gly17Gln18 loop where the amide of Gly17 is a specific hydrogen bond donor, and hydrophobic contacts occur with the side chains of Lys14 and Leu63. Another fragment, indole-6-carboxylic acid, binds on the ‘outside/top of the flap’ via hydrophobic contacts with Trp42, Pro44, Met46, and Lys55, a hydrogen bond with Val56, and a salt-bridge with Arg57. 2-acetyl-benzothiophene also binds at this site. This study is the first fragment-based crystallographic screen against HIV PR, and the first time that fragments were screened against an inhibitor-bound drug target to search for compounds that both bind to novel sites and stabilize the inhibited conformation of the target. PMID:20659109

Containerless processing of single crystals in low-G environment

NASA Technical Reports Server (NTRS)

Walter, H. U.

1974-01-01

Experiments on containerless crystal growth from the melt were conducted during Skylab missions SL3 and SL4 (Skylab Experiment M-560). Six samples of InSb were processed, one of them heavily doped with selenium. The concept of the experiment is discussed and related to general crystal growth methods and their merits as techniques for containerless processing in space. The morphology of the crystals obtained is explained in terms of volume changes associated with solidification and wetting conditions during solidification. All samples exhibit extremely well developed growth facets. Analysis by X-ray topographical methods and chemical etching shows that the crystals are of high structural perfection. Average dislocation density as revealed by etching is of the order of 100 per sq cm; no dislocation clusters could be observed in the space-grown samples. A sequence of striations that is observed in the first half of the selenium-doped sample is explained as being caused by periodic surface breakdown.

Preliminary Work in Obtaining Site-Directed Mutants of Hen Egg White Lysozyme

NASA Technical Reports Server (NTRS)

Holmes, Leonard D.

1996-01-01

Protein crystal growth studies are recognized as a critical endeavor in the field of molecular biotechnology. The scientific applications of this field include the understanding of how enzymes function and the accumulation of accurate information of atomic structures, a key factor in the process of rational drug design. NASA has committed substantial investment and resources to the field of protein crystal growth and has conducted many microgravity protein crystal growth experiments aboard shuttle flights. Crystals grown in space tend to be larger, denser and have a more perfect habit and geometry. These improved properties gained in the microgravity environment of space result largely from the reduction of solutal convection, and the elimination of sedimentation at the growing crystal surface. Shuttle experiments have yielded many large, high quality crystals that are suitable for high resolution X-ray diffraction analysis. Examples of biologically important macromolecules which have been successfully crystallized during shuttle missions include: lysozyme, isocitrate lyase, gamma-interferon, insulin, human serum albumin and canavalin. Numerous other examples are also available. In addition to obtaining high quality crystals, investigators are also interested in learning the mechanisms by which the growth events take place. Crystallization experiments indicate that for the enzyme HEWL, measured growth rates do not follow mathematical models for 2D nucleation and dislocation-led growth of tetragonal protein crystals. As has been suggested by the laboratory of Marc L. Pusey, a possible explanation for the disagreement between observation and data is that HEWL tetraconal crystals form by aggregated units of lysozyme in supersaturated solutions. Surface measurement data was shown to fit very well with a model using an octamer unit cell as the growth unit. According to this model, the aggregation pathway and subsequent crystal growth is described by: monomer < ------ > dimer < ------- > tetramer < ------ > octamer < ------ > higher order. It is believed that multimer aggregation of lysozyme occurs by interaction at specific binding sites on the surface of the protein crystals. If the presence of discrete binding sites and the aggregation hypothesis is true, then it follows that the alteration of the binding site(s) should have significant effect on the measurements obtained during growth experiments. Site-directed mutagenesis allows the specific alteration of proteins by replacement, deletion or addition of specific amino acid residues. This report outlines the approach for this strategy and the progress made thus far toward that end.

Study of Fluid Flow Control in Protein Crystallization using Strong Magnetic Fields

NASA Astrophysics Data System (ADS)

Ramachandran, Narayanan; Leslie, Fred; Ciszak, Ewa

2002-11-01

An important component in biotechnology, particularly in the area of protein engineering and rational drug design is the knowledge of the precise three-dimensional molecular structure of proteins. The quality of structural information obtained from X-ray diffraction methods is directly dependent on the degree of perfection of the protein crystals. As a consequence, the growth of high quality macromolecular crystals for diffraction analyses has been the central focus for biochemists, biologists, and bioengineers. Macromolecular crystals are obtained from solutions that contain the crystallizing species in equilibrium with higher aggregates, ions, precipitants, other possible phases of the protein, foreign particles, the walls of the container, and a likely host of other impurities. By changing transport modes in general, i.e., reduction of convection and sedimentation, as is achieved in "microgravity", researchers have been able to dramatically affect the movement and distribution of macromolecules in the fluid, and thus their transport, formation of crystal nuclei, and adsorption to the crystal surface. While a limited number of high quality crystals from space flights have been obtained, as the recent National Research Council (NRC) review of the NASA microgravity crystallization program pointed out, the scientific approach and research in crystallization of proteins has been mainly empirical yielding inconclusive results. We postulate that we can reduce convection in ground-based experiments and we can understand the different aspects of convection control through the use of strong magnetic fields and field gradients. Whether this limited convection in a magnetic field will provide the environment for the growth of high quality crystals is still a matter of conjecture that our research will address. The approach exploits the variation of fluid magnetic susceptibility with concentration for this purpose and the convective damping is realized by appropriately positioning the crystal growth cell so that the magnetic susceptibility force counteracts terrestrial gravity. The general objective is to test the hypothesis of convective control using a strong magnetic field and magnetic field gradient and to understand the nature of the various forces that come into play. Specifically we aim to delineate causative factors and to quantify them through experiments, analysis and numerical modeling. Once the basic understanding is obtained, the study will focus on testing the hypothesis on proteins of pyruvate dehydrogenase complex (PDC), proteins E1 and E3. Obtaining high crystal quality of these proteins is of great importance to structural biologists since their structures need to be determined. Specific goals for the investigation are: 1. To develop an understanding of convection control in diamagnetic fluids with concentration gradients through experimentation and numerical modeling. Specifically solutal buoyancy driven convection due to crystal growth will be considered. 2. To develop predictive measures for successful crystallization in a magnetic field using analyses and numerical modeling for use in future protein crystal growth experiments. This will establish criteria that can be used to estimate the efficacy of magnetic field flow damping on crystallization of candidate proteins. 3. To demonstrate the understanding of convection damping by high magnetic fields to a class of proteins that is of interest and whose structure is as yet not determined. 4. To compare quantitatively, the quality of the grown crystals with and without a magnetic field. X-ray diffraction techniques will be used for the comparative studies. In a preliminary set of experiments, we studied crystal dissolution effects in a 5 Tesla magnet available at NASA Marshall Space Flight Center (MSFC). Using a Schlieren setup, a 1mm crystal of Alum (Aluminum-Potassium Sulfate) was introduced in a 75% saturated solution and the resulting dissolution plume was observed. The experiment was conducted both in the presence and absence of a magnetic field gradient. The magnet produces a gradient field of approx. 1 Tesla2/cm. Image analysis of the recorded images indicated an enhanced plume velocity that was of the order of the measurement limit. For this experiment, both the gradient and gravity fields are in the same direction resulting in an enhanced effective gravity that tends to accelerate the observed plume velocity. While the results are not conclusive, pending further tests, it clearly points out the inadequacy of the MSFC magnet for conducting protein crystallization experiments and the need for a stronger magnet. In spacebased experiments, however, where the gravitational effects are small, only a weak magnetic field will be required to control or mitigate the effects of convective contamination.

Study of Fluid Flow Control in Protein Crystallization using Strong Magnetic Fields

NASA Technical Reports Server (NTRS)

Ramachandran, Narayanan; Leslie, Fred; Ciszak, Ewa

2002-01-01

An important component in biotechnology, particularly in the area of protein engineering and rational drug design is the knowledge of the precise three-dimensional molecular structure of proteins. The quality of structural information obtained from X-ray diffraction methods is directly dependent on the degree of perfection of the protein crystals. As a consequence, the growth of high quality macromolecular crystals for diffraction analyses has been the central focus for biochemists, biologists, and bioengineers. Macromolecular crystals are obtained from solutions that contain the crystallizing species in equilibrium with higher aggregates, ions, precipitants, other possible phases of the protein, foreign particles, the walls of the container, and a likely host of other impurities. By changing transport modes in general, i.e., reduction of convection and sedimentation, as is achieved in "microgravity", researchers have been able to dramatically affect the movement and distribution of macromolecules in the fluid, and thus their transport, formation of crystal nuclei, and adsorption to the crystal surface. While a limited number of high quality crystals from space flights have been obtained, as the recent National Research Council (NRC) review of the NASA microgravity crystallization program pointed out, the scientific approach and research in crystallization of proteins has been mainly empirical yielding inconclusive results. We postulate that we can reduce convection in ground-based experiments and we can understand the different aspects of convection control through the use of strong magnetic fields and field gradients. Whether this limited convection in a magnetic field will provide the environment for the growth of high quality crystals is still a matter of conjecture that our research will address. The approach exploits the variation of fluid magnetic susceptibility with concentration for this purpose and the convective damping is realized by appropriately positioning the crystal growth cell so that the magnetic susceptibility force counteracts terrestrial gravity. The general objective is to test the hypothesis of convective control using a strong magnetic field and magnetic field gradient and to understand the nature of the various forces that come into play. Specifically we aim to delineate causative factors and to quantify them through experiments, analysis and numerical modeling. Once the basic understanding is obtained, the study will focus on testing the hypothesis on proteins of pyruvate dehydrogenase complex (PDC), proteins E1 and E3. Obtaining high crystal quality of these proteins is of great importance to structural biologists since their structures need to be determined. Specific goals for the investigation are: 1. To develop an understanding of convection control in diamagnetic fluids with concentration gradients through experimentation and numerical modeling. Specifically solutal buoyancy driven convection due to crystal growth will be considered. 2. To develop predictive measures for successful crystallization in a magnetic field using analyses and numerical modeling for use in future protein crystal growth experiments. This will establish criteria that can be used to estimate the efficacy of magnetic field flow damping on crystallization of candidate proteins. 3. To demonstrate the understanding of convection damping by high magnetic fields to a class of proteins that is of interest and whose structure is as yet not determined. 4. To compare quantitatively, the quality of the grown crystals with and without a magnetic field. X-ray diffraction techniques will be used for the comparative studies. In a preliminary set of experiments, we studied crystal dissolution effects in a 5 Tesla magnet available at NASA Marshall Space Flight Center (MSFC). Using a Schlieren setup, a 1mm crystal of Alum (Aluminum-Potassium Sulfate) was introduced in a 75% saturated solution and the resulting dissolution plume was observed. The experiment was conducted both in the presence and absence of a magnetic field gradient. The magnet produces a gradient field of approx. 1 Tesla2/cm. Image analysis of the recorded images indicated an enhanced plume velocity that was of the order of the measurement limit. For this experiment, both the gradient and gravity fields are in the same direction resulting in an enhanced effective gravity that tends to accelerate the observed plume velocity. While the results are not conclusive, pending further tests, it clearly points out the inadequacy of the MSFC magnet for conducting protein crystallization experiments and the need for a stronger magnet. In spacebased experiments, however, where the gravitational effects are small, only a weak magnetic field will be required to control or mitigate the effects of convective contamination.

Sodium intercalation in the phosphosulfate cathode NaFe2(PO4)(SO4)2

NASA Astrophysics Data System (ADS)

Ben Yahia, Hamdi; Essehli, Rachid; Amin, Ruhul; Boulahya, Khalid; Okumura, Toyoki; Belharouak, Ilias

2018-04-01

The compound NaFe2(PO4)(SO4)2 is successfully synthesized via a solid state reaction route and its crystal structure is determined using powder X-ray diffraction data. NaFe2(PO4)(SO4)2 phase is also characterized by cyclic voltammetry, galvanostatic cycling and electrochemical impedance spectroscopy. NaFe2(PO4)(SO4)2 crystallizes with the well-known NASICON-type structure. SAED and HRTEM experiments confirm the structural model, and no ordering between the PO4-3 and SO4-2 polyanions is detected. The electrochemical tests indicate that NaFe2(PO4)(SO4)2 is a 3 V sodium intercalating cathode. The electrical conductivity is relatively low (2.2 × 10-6 Scm-1 at 200 °C) and the obtained activation energy is ∼0.60eV. The GITT experiments indicate that the diffusivity values are in the range of 10-11-10-12 cm2/s within the measured sodium concentrations.

Comparative study on ATR-FTIR calibration models for monitoring solution concentration in cooling crystallization

NASA Astrophysics Data System (ADS)

Zhang, Fangkun; Liu, Tao; Wang, Xue Z.; Liu, Jingxiang; Jiang, Xiaobin

2017-02-01

In this paper calibration model building based on using an ATR-FTIR spectroscopy is investigated for in-situ measurement of the solution concentration during a cooling crystallization process. The cooling crystallization of L-glutamic Acid (LGA) as a case is studied here. It was found that using the metastable zone (MSZ) data for model calibration can guarantee the prediction accuracy for monitoring the operating window of cooling crystallization, compared to the usage of undersaturated zone (USZ) spectra for model building as traditionally practiced. Calibration experiments were made for LGA solution under different concentrations. Four candidate calibration models were established using different zone data for comparison, by using a multivariate partial least-squares (PLS) regression algorithm for the collected spectra together with the corresponding temperature values. Experiments under different process conditions including the changes of solution concentration and operating temperature were conducted. The results indicate that using the MSZ spectra for model calibration can give more accurate prediction of the solution concentration during the crystallization process, while maintaining accuracy in changing the operating temperature. The primary reason of prediction error was clarified as spectral nonlinearity for in-situ measurement between USZ and MSZ. In addition, an LGA cooling crystallization experiment was performed to verify the sensitivity of these calibration models for monitoring the crystal growth process.

Spacelab 3 vapor crystal growth experiment

NASA Technical Reports Server (NTRS)

Schnepple, W.; Vandenberg, L.; Skinner, N.; Ortale, C.

1987-01-01

The Space Shuttle Challenger, with Spacelab 3 as its payload, was launched into orbit April 29, 1985. The mission, number 51-B, emphasized materials processing in space, although a wide variety of experiments in other disciplines were also carried onboard. One of the materials processing experiments on this flight is described, specifically the growth of single crystals of mercuric iodide by physical vapor transport.

KSC-03PD-1471

NASA Technical Reports Server (NTRS)

2003-01-01

KENNEDY SPACE CENTER, FLA. - The crystals visible in this laboratory dish were part of an experiment carried on mission STS-107. Several experiments were found during the search for Columbia debris. Included in the Commercial ITA Biomedical Experiments payload on mission STS-107 are urokinase cancer research, microencapsulation of drugs, the Growth of Bacterial Biofilm on Surfaces during Spaceflight (GOBBSS), and tin crystal formation.

Microgravity

NASA Image and Video Library

1995-09-17

Horse Serum Albumin crystals grown during the USML-1 (STS-50) mission's Protein Crystal Growth Glovebox Experiment. These crystals were grown using a vapor diffusion technique at 22 degrees C. The crystals were allowed to grow for nine days while in orbit. Crystals of 1.0 mm in length were produced. The most abundant blood serum protein, regulates blood pressure and transports ions, metabolites, and therapeutic drugs. Principal Investigator was Edward Meehan.

Angular selectivity asymmetry of holograms recorded in near infrared sensitive liquid crystal photopolymerizable materials

NASA Astrophysics Data System (ADS)

Harbour, Steven; Galstian, Tigran; Akopyan, Rafik; Galstyan, Artur

2004-08-01

We have experimentally observed and theoretically explained the angular selectivity asymmetry in polymer dispersed liquid crystal holograms. Experiments are conducted in compounds with near infrared sensitivity. The coupled-wave theory is used to describe the diffraction properties of obtained anisotropic holographic gratings. Furthermore, the comparison of theory and experiments provides information about the optical axis direction that is defined by the average molecular orientation of the liquid crystal in the polymer matrix.

Comparison of OARE Accelerometer Data with Dopant Distribution in Se-Doped GaAs Crystals Grown During USML-1

NASA Technical Reports Server (NTRS)

Moskowitz, Milton E.; Bly, Jennifer M.; Matthiesen, David H.

1997-01-01

Experiments were conducted in the crystal growth furnace (CGF) during the first United States Microgravity Laboratory (USML-1), the STS-50 flight of the Space Shuttle Columbia, to determine the segregation behavior of selenium in bulk GaAs in a microgravity environment. After the flight, the selenium-doped GaAs crystals were sectioned, polished, and analyzed to determine the free carrier concentration as a function of position, One of the two crystals initially exhibited an axial concentration profile indicative of diffusion controlled growth, but this profile then changed to that predicted for a complete mixing type growth. An analytical model, proposed by Naumann [R.J. Naumann, J. Crystal Growth 142 (1994) 253], was utilized to predict the maximum allowable microgravity disturbances transverse to the growth direction during the two different translation rates used for each of the experiments. The predicted allowable acceleration levels were 4.86 microgram for the 2.5 micrometers/s furnace translation rate and 38.9 microgram for the 5.0 micrometers/s rate. These predicted values were compared to the Orbital Acceleration Research Experiment (OARE) accelerometer data recorded during the crystal growth periods for these experiments. Based on the analysis of the OARE acceleration data and utilizing the predictions from the analytical model, it is concluded that the change in segregation behavior was not caused by any acceleration events in the microgravity environment.

Towards establishing a combined rate law of nucleation and crystal growth - The case study of gypsum precipitation

NASA Astrophysics Data System (ADS)

Rendel, Pedro M.; Gavrieli, Ittai; Wolff-Boenisch, Domenik; Ganor, Jiwchar

2018-03-01

The main obstacle in the formulation of a quantitative rate-model for mineral precipitation is the absence of a rigorous method for coupling nucleation and growth processes. In order to link both processes, we conducted a series of batch experiments in which gypsum nucleation was followed by crystal growth. Experiments were carried out using various stirring methods in several batch vessels made of different materials. In the experiments, the initial degree of supersaturation of the solution with respect to gypsum (Ωgyp) was set between 1.58 and 1.82. Under these conditions, heterogeneous nucleation is the dominant nucleation mode. Based on changes in SO42- concentration with time, the induction time of gypsum nucleation and the following rate of crystal growth were calculated for each experiment. The induction time (6-104 h) was found to be a function of the vessel material, while the rates of crystal growth, which varied over three orders of magnitude, were strongly affected by the stirring speed and its mode (i.e. rocking, shaking, magnetic stirrer, and magnetic impeller). The SO42- concentration data were then used to formulate a forward model that couples the simple rate laws for nucleation and crystal growth of gypsum into a single kinetic model. Accordingly, the obtained rate law is based on classical nucleation theory and heterogeneous crystal growth.

On the origin of size-dependent and size-independent crystal growth: Influence of advection and diffusion

USGS Publications Warehouse

Kile, D.E.; Eberl, D.D.

2003-01-01

Crystal growth experiments were conducted using potassium alum and calcite crystals in aqueous solution under both non-stirred and stirred conditions to elucidate the mechanism for size-dependent (proportionate) and size-independent (constant) crystal growth. Growth by these two laws can be distinguished from each other because the relative size difference among crystals is maintained during proportionate growth, leading to a constant crystal size variance (??2) for a crystal size distribution (CSD) as the mean size increases. The absolute size difference among crystals is maintained during constant growth, resulting in a decrease in size variance. Results of these experiments show that for centimeter-sized alum crystals, proportionate growth occurs in stirred systems, whereas constant growth occurs in non-stirred systems. Accordingly, the mechanism for proportionate growth is hypothesized to be related to the supply of reactants to the crystal surface by advection, whereas constant growth is related to supply by diffusion. Paradoxically, micrometer-sized calcite crystals showed proportionate growth both in stirred and in non-stirred systems. Such growth presumably results from the effects of convection and Brownian motion, which promote an advective environment and hence proportionate growth for minute crystals in non-stirred systems, thereby indicating the importance of solution velocity relative to crystal size. Calcite crystals grown in gels, where fluid motion was minimized, showed evidence for constant, diffusion-controlled growth. Additional investigations of CSDs of naturally occurring crystals indicate that proportionate growth is by far the most common growth law, thereby suggesting that advection, rather than diffusion, is the dominant process for supplying reactants to crystal surfaces.

Giant magmatic water reservoirs at mid-crustal depth inferred from electrical conductivity and the growth of the continental crust

NASA Astrophysics Data System (ADS)

Laumonier, Mickael; Gaillard, Fabrice; Muir, Duncan; Blundy, Jon; Unsworth, Martyn

2017-01-01

The formation of the continental crust at subduction zones involves the differentiation of hydrous mantle-derived magmas through a combination of crystallization and crustal melting. However, understanding the mechanisms by which differentiation occurs at depth is hampered by the inaccessibility of the deep crust in active continental arcs. Here we report new high-pressure electrical conductivity and petrological experiments on hydrated andesitic melt from Uturuncu volcano on the Bolivian Altiplano. By applying our results to regional magnetotelluric data, we show that giant conductive anomalies at mid-crustal levels in several arcs are characterized by relatively low amounts of intergranular andesitic partial melts with unusually high dissolved water contents (≥8 wt.% H2O). Below Uturuncu, the Altiplano-Puna Magma Body (APMB) displays an electrical conductivity that requires high water content (up to 10 wt.%) dissolved in the melt based on crystal-liquid equilibria and melt H2O solubility experiments. Such a super-hydrous andesitic melt must constitute about 10% of the APMB, the remaining 90% being a combination of magmatic cumulates and older crustal rocks. The crustal ponding level of these andesites at around 6 kbar pressure implies that on ascent through the crust hydrous magmas reach their water saturation pressure in the mid-crust, resulting in decompression-induced crystallization that increases magma viscosity and in turn leads to preferential stalling and differentiation. Similar high conductivity features are observed beneath the Cascades volcanic arc and Taupo Volcanic Zone. This suggests that large amounts of water in super-hydrous andesitic magmas could be a common feature of active continental arcs and may illustrate a key step in the structure and growth of the continental crust. One Sentence Summary: Geophysical, laboratory conductivity and petrological experiments reveal that deep electrical conductivity anomalies beneath the Central Andes, Cascades and Taupo Volcanic Zone image the ponding of super-hydrous andesitic melts which contributes to the growth of continental crust.

Stability of Magnetically-Suppressed Solutal Convection In Protein Crystal Growth

NASA Technical Reports Server (NTRS)

Leslie, F. W.; Ramachandran, N.

2005-01-01

The effect of convection during the crystallization of proteins is not very well understood. In a gravitational field, convection is caused by crystal sedimentation and by solutal buoyancy induced flow and these can lead to crystal imperfections. While crystallization in microgravity can approach diffusion limited growth conditions (no convection), terrestrially strong magnetic fields can be used to control fluid flow and sedimentation effects. In this work, a theory is presented on the stability of solutal convection of a magnetized fluid in the presence of a magnetic field. The requirements for stability are developed and compared to experiments performed within the bore of a superconducting magnet. The theoretical predictions are in good agreement with the experiments and show solutal convection can be stabilized if the surrounding fluid has larger magnetic susceptibility and the magnetic field has a specific structure. Discussion on the application of the technique to protein crystallization is also provided.

Application of X-ray topography to USSR and Russian space materials science

PubMed Central

Shul’pina, I. L.; Prokhorov, I. A.; Serebryakov, Yu. A.; Bezbakh, I. Zh.

2016-01-01

The authors’ experience of the application of X-ray diffraction imaging in carrying out space technological experiments on semiconductor crystal growth for the former USSR and for Russia is reported, from the Apollo–Soyuz programme (1975) up to the present day. X-ray topography was applied to examine defects in crystals in order to obtain information on the crystallization conditions and also on their changes under the influence of factors of orbital flight in space vehicles. The data obtained have promoted a deeper understanding of the conditions and mechanisms of crystallization under both microgravity and terrestrial conditions, and have enabled the elaboration of terrestrial methods of highly perfect crystal growth. The use of X-ray topography in space materials science has enriched its methods in the field of digital image processing of growth striations and expanded its possibilities in investigating the inhomogeneity of crystals. PMID:27158506

Observation of divergent-beam X-ray diffraction from a crystal of diamond using synchrotron radiation.

PubMed

Glazer, A M; Collins, S P; Zekria, D; Liu, J; Golshan, M

2004-03-01

In 1947 Kathleen Lonsdale conducted a series of experiments on X-ray diffraction using a divergent beam external to a crystal sample. Unlike the Kossel technique, where divergent X-rays are excited by the presence of fluorescing atoms within the crystal, the use of an external divergent source made it possible to study non-fluorescing crystals. The resulting photographs not only illustrated the complexity of X-ray diffraction from crystals in a truly beautiful way, but also demonstrated unprecedented experimental precision. This long-forgotten work is repeated here using a synchrotron radiation source and, once again, considerable merit is found in Lonsdale's technique. The results of this experiment suggest that, through the use of modern 'third-generation' synchrotron sources, divergent-beam diffraction could soon enjoy a renaissance for high-precision lattice-parameter determination and the study of crystal perfection.

Application of X-ray topography to USSR and Russian space materials science.

PubMed

Shul'pina, I L; Prokhorov, I A; Serebryakov, Yu A; Bezbakh, I Zh

2016-05-01

The authors' experience of the application of X-ray diffraction imaging in carrying out space technological experiments on semiconductor crystal growth for the former USSR and for Russia is reported, from the Apollo-Soyuz programme (1975) up to the present day. X-ray topography was applied to examine defects in crystals in order to obtain information on the crystallization conditions and also on their changes under the influence of factors of orbital flight in space vehicles. The data obtained have promoted a deeper understanding of the conditions and mechanisms of crystallization under both microgravity and terrestrial conditions, and have enabled the elaboration of terrestrial methods of highly perfect crystal growth. The use of X-ray topography in space materials science has enriched its methods in the field of digital image processing of growth striations and expanded its possibilities in investigating the inhomogeneity of crystals.

The Quartz-Crystal Microbalance in an Undergraduate Laboratory Experiment: I. Fundamentals and Instrumentation

ERIC Educational Resources Information Center

Tsionsky, Vladimir

2007-01-01

The fundamentals, as well as the instrumentation of the quartz-crystal microbalance (QCM) technique that is used in an undergraduate laboratory experiment are being described. The QCM response can be easily used to change the properties of any system.

Crewmember working on the mid deck Zeolite Crystal Growth experiment.

NASA Technical Reports Server (NTRS)

1992-01-01

View showing Payload Specialist Bonnie Dunbar, in the mid deck, conducting the Zeolite Crystal Growth (ZCG) Experiment in the mid deck stowage locker work area. View shows assembly of zeolite sample in the metal autoclave cylinders prior to insertion into the furnace.

Association of Ions and Fractional Crystallization.

ERIC Educational Resources Information Center

Scaife, Charles W. J.; Dubs, Richard L.

1983-01-01

Presents an experiment in which color is used as an additional characteristic when purifying and identifying crystals of two soluble salts obtained from a metathesis reaction. Indicates that the experiment has been used with both nonmajors and inorganic chemistry students in at least their third term. (JN)

The Quartz-Crystal Microbalance in an Undergraduate Laboratory Experiment II: Measuring Viscosity

ERIC Educational Resources Information Center

Tsionsky, Vladimir

2007-01-01

Various water-alcohol and alcohol-alcohol based experiments are used to demonstrate how the quartz-crystal microbalance (QCM) technique is used for measuring the viscosity of a system. The technique is very advantageous, as it is inexpensive and provides digital output.

Analysis and implementation of a space resolving spherical crystal spectrometer for x-ray Thomson scattering experiments

DOE Office of Scientific and Technical Information (OSTI.GOV)

Harding, E. C.; Ao, T.; Bailey, J. E.

2015-04-15

The application of a space-resolving spectrometer to X-ray Thomson Scattering (XRTS) experiments has the potential to advance the study of warm dense matter. This has motivated the design of a spherical crystal spectrometer, which is a doubly focusing geometry with an overall high sensitivity and the capability of providing high-resolution, space-resolved spectra. A detailed analysis of the image fluence and crystal throughput in this geometry is carried out and analytical estimates of these quantities are presented. This analysis informed the design of a new spectrometer intended for future XRTS experiments on the Z-machine. The new spectrometer collects 6 keV x-raysmore » with a spherically bent Ge (422) crystal and focuses the collected x-rays onto the Rowland circle. The spectrometer was built and then tested with a foam target. The resulting high-quality spectra prove that a spherical spectrometer is a viable diagnostic for XRTS experiments.« less

Analysis and implementation of a space resolving spherical crystal spectrometer for x-ray Thomson scattering experiments.

PubMed

Harding, E C; Ao, T; Bailey, J E; Loisel, G; Sinars, D B; Geissel, M; Rochau, G A; Smith, I C

2015-04-01

The application of a space-resolving spectrometer to X-ray Thomson Scattering (XRTS) experiments has the potential to advance the study of warm dense matter. This has motivated the design of a spherical crystal spectrometer, which is a doubly focusing geometry with an overall high sensitivity and the capability of providing high-resolution, space-resolved spectra. A detailed analysis of the image fluence and crystal throughput in this geometry is carried out and analytical estimates of these quantities are presented. This analysis informed the design of a new spectrometer intended for future XRTS experiments on the Z-machine. The new spectrometer collects 6 keV x-rays with a spherically bent Ge (422) crystal and focuses the collected x-rays onto the Rowland circle. The spectrometer was built and then tested with a foam target. The resulting high-quality spectra prove that a spherical spectrometer is a viable diagnostic for XRTS experiments.

Probing dynamics in colloidal crystals with pump-probe experiments at LCLS: Methodology and analysis

DOE PAGES

Mukharamova, Nastasia; Lazarev, Sergey; Meijer, Janne -Mieke; ...

2017-05-19

We present results of the studies of dynamics in colloidal crystals performed by pump-probe experiments using an X-ray free-electron laser (XFEL). Colloidal crystals were pumped with an infrared laser at a wavelength of 800 nm with varying power and probed by XFEL pulses at an energy of 8 keV with a time delay up to 1000 ps. The positions of the Bragg peaks, and their radial and azimuthal widths were analyzed as a function of the time delay. The spectral analysis of the data did not reveal significant enhancement of frequencies expected in this experiment. As a result, this allowedmore » us to conclude that the amplitude of vibrational modes excited in colloidal crystals was less than the systematic error caused by the noise level.« less

Crystallization of Hard Sphere Colloids in Microgravity: Results of the Colloidal Disorder-Order Transition, CDOT on USML-2. Experiment 33

NASA Technical Reports Server (NTRS)

Zhu, Ji-Xiang; Chaikin, P. M.; Li, Min; Russel, W. B.; Ottewill, R. H.; Rogers, R.; Meyer, W. V.

1998-01-01

Classical hard spheres have long served as a paradigm for our understanding of the structure of liquids, crystals, and glasses and the transitions between these phases. Ground-based experiments have demonstrated that suspensions of uniform polymer colloids are near-ideal physical realizations of hard spheres. However, gravity appears to play a significant and unexpected role in the formation and structure of these colloidal crystals. In the microgravity environment of the Space Shuttle, crystals grow purely via random stacking of hexagonal close-packed planes, lacking any of the face-centered cubic (FCC) component evident in crystals grown in 1 g beyond melting and allowed some time to settle. Gravity also masks 33-539 the natural growth instabilities of the hard sphere crystals which exhibit striking dendritic arms when grown in microgravity. Finally, high volume fraction "glass" samples which fail to crystallize after more than a year in 1 g begin nucleation after several days and fully crystallize in less than 2 weeks on the Space Shuttle.

Student Pave Way for First Microgravity Experiments on International Space Station

NASA Technical Reports Server (NTRS)

1999-01-01

Chemist Arna Holmes, left, from the University of Alabama in Huntsville, teaches NaLonda Moorer, center, and Maricar Bana, right, both from Terry Parker High School in Jacksonville, Fl, procedures for preparing protein crystal growth samples for flight aboard the International Space Station (ISS). NASA/Marshall Space Flight Center in Huntsville, AL, is a sponsor for this educational activity. The proteins are placed in plastic tubing that is heat-sealed at the ends, then flash-frozen and preserved in a liquid nitrogen Dewar. Aborad the ISS, the nitrogen will be allowed to evaporated so the samples thaw and then slowly crystallize. They will be analyzed after return to Earth. Photo credit: NASA/Marshall Space Flight Center (MSFC)

Thermally Assisted Macroscopic Quantum Resonance on a Single-Crystal of Mn12-ac

NASA Astrophysics Data System (ADS)

Lionti, F.; Thomas, L.; Ballou, R.; Wernsdorfer, W.; Barbara, B.; Sulpice, A.; Sessoli, R.; Gatteschi, D.

1997-03-01

Magnetization measurements have been performed on a single mono-crystal of the molecule Mn12-acetate (L. Thomas, F. Lionti, R. Ballou, R. Sessoli, D. Gatteschi and B. Barbara, Nature, 383, 145 (1996).). Steps were observed in the hysteresis loop for values of the applied field at which level crossings of the collective spin states of each manganese clusters take place. The influence of quartic terms is taken into account. At these fields, the magnetization relaxes at short time scales, being otherwise essentially blocked. This novel behavior is interpreted in terms of resonant quantum tunneling of the magnetization from thermally activated energy levels. Hysteresis loop measurements performed for different field orientations and ac-susceptibility experiments, confirm general trends of this picture.

Layer-by-layer polyelectrolyte coating for surface-enhanced Raman scattering on gold nanostars inside hollow core photonic crystal fibers

NASA Astrophysics Data System (ADS)

Burmistrova, Natalia A.; Bondarenko, Sergei D.; Bratashov, Daniil N.; Shuvalov, Andrei A.; Chibrova, Anastasiya A.; Khlebtsov, Boris N.; Skibina, Julia S.; Goryacheva, Irina Y.

2018-04-01

Photonic crystal fibers with hollow core (HC PCFs) are a specific class of optical fibers characterized by microstructure with periodic holes oriented along fiber. The combination of HC PCF with Raman spectroscopy for biosensors creation is attractive in the terms of the low sample volume, the possibility to increase the integration time without sample degradation and maintaining constant focus during experiments. Here we propose layer-by-layer polyelectrolyte coating of HC PCF inner surface in order to obtain charge-selective absorption of analyte, stabilization of Surface-Enhanced Raman scattering (SERS)-active gold nanoparticles. Distance between SERS hotspots and glass reduces nonlinear signals from glass, and increases signal-to-noise ratio of SERS spectra.

The 1980 solar maximum mission event listing

NASA Technical Reports Server (NTRS)

Speich, D. M.; Nelson, J. J.; Licata, J. P.; Tolbert, A. K.

1991-01-01

Information is contained on solar burst and transient activity observed by the Solar Maximum Mission (SMM) during 1980 pointed observations. Data from the following SMM experiments are included: (1) Gamma Ray Spectrometer, (2) Hard X-Ray Burst Spectrometer, (3) Hard X-Ray Imaging Spectrometer, (4) Flat Crystal Spectrometer, (5) Bent Crystal Spectrometer, (6) Ultraviolet Spectrometer and Polarimeter, and (7) Coronagraph/Polarimeter. Correlative optical, radio, and Geostationary Operational Environmental Satellite (GOES) x ray data are also presented. Where possible, bursts or transients observed in the various wavelengths were grouped into discrete flare events identified by unique event numbers. Each event carries a qualifier denoting the quality or completeness of the observations. Spacecraft pointing coordinates and flare site angular displacement values from Sun center are also included.

A study of crystal growth by solution technique. [triglycine sulfate single crystals

NASA Technical Reports Server (NTRS)

Lal, R. B.

1979-01-01

The advantages and mechanisms of crystal growth from solution are discussed as well as the effects of impurity adsorption on the kinetics of crystal growth. Uncertainities regarding crystal growth in a low gravity environment are examined. Single crystals of triglycine sulfate were grown using a low temperature solution technique. Small components were assembled and fabricated for future space flights. A space processing experiment proposal accepted by NASA for the Spacelab-3 mission is included.

Ignition and growth modeling of detonation reaction zone experiments on single crystals of PETN and HMX

NASA Astrophysics Data System (ADS)

White, Bradley W.; Tarver, Craig M.

2017-01-01

It has long been known that detonating single crystals of solid explosives have much larger failure diameters than those of heterogeneous charges of the same explosive pressed or cast to 98 - 99% theoretical maximum density (TMD). In 1957, Holland et al. demonstrated that PETN single crystals have failure diameters of about 8 mm, whereas heterogeneous PETN charges have failure diameters of less than 0.5 mm. Recently, Fedorov et al. quantitatively determined nanosecond time resolved detonation reaction zone profiles of single crystals of PETN and HMX by measuring the interface particle velocity histories of the detonating crystals and LiF windows using a PDV system. The measured reaction zone time durations for PETN and HMX single crystal detonations were approximately 100 and 260 nanoseconds, respectively. These experiments provided the necessary data to develop Ignition and Growth (I&G) reactive flow model parameters for the single crystal detonation reaction zones. Using these parameters, the calculated unconfined failure diameter of a PETN single crystal was 7.5 +/- 0.5 mm, close to the 8 mm experimental value. The calculated failure diameter of an unconfined HMX single crystal was 15 +/- 1 mm. The unconfined failure diameter of an HMX single crystal has not yet been determined precisely, but Fedorov et al. detonated 14 mm diameter crystals confined by detonating a HMX-based plastic bonded explosive (PBX) without initially overdriving the HMX crystals.

Helium Diffusion in Natural Xenotime

NASA Astrophysics Data System (ADS)

Anderson, A. J.; Hodges, K. V.; Van Soest, M. C.; Hanchar, J. M.

2017-12-01

Xenotime (nominally YPO4) occurs as an accessory mineral in felsic igneous rocks, pegmatites, and gneisses, often incorporating weight percent levels of U, Th, and REEs. Although commonly used for precise U-Pb geochronology, xenotime is seldom used for (U-Th)/He thermochronometry despite the fact that its high radionuclide content allows for the rapid accumulation of radiogenic He that could potentially allow for the precise dating of very young cooling events in active geologic settings. Xenotime's likely high concentrations of radiogenic 4He also make it a promising candidate for laser microprobe (U-Th)/He dating. Unfortunately, limited data are currently available for He diffusion in xenotime, and previous experimental studies of natural and synthetic xenotime have led to discrepant results (1). Published estimates of the (U-Th)/He closure temperature for xenotime based on these experiments range from 60˚C to 300˚C. In this contribution, we report new results for incremental step heating `bulk' 4He diffusion experiments on a fragment of a natural xenotime crystal from the Torghar district of the Khyber Agency in the Federally Administered Tribal Areas of Pakistan. Laser ablation 238U/206Pb dating of this crystal yields a crystallization age of 28.82 ± 0.13 Ma. The results of our He diffusion experiments- which display excellent linearity on an Arrhenius plot assuming a spherical geometry - indicate kinetic parameters of E 133 kJ/mol and ln(D0/a2) 10.9 s-1. Our results imply a preliminary (U-Th)/He closure temperature of 80˚C for xenotime crystals with a diffusion dimension of 220 μm. This closure temperature is much lower than that previously estimated for natural xenotime (1), and it is possible, perhaps likely, that He diffusion in natural xenotime crystals display a strong compositional dependency (1). Nevertheless, our experimental data suggest that near-end member (YPO4) xenotime has an intrinsic helium diffusivity consistent with a closure temperature comparable to that of the apatite (U-Th)/He thermochronometer. As a consequence, xenotime He chronometry may serve as a higher-precision alternative to apatite He chronometry for revealing low temperature cooling histories of rocks in which it crystallized. References: 1) Farley, 2007, Geochimica et Cosmochimica Acta, v. 71.

Comprehensive Study of the Model Mercury-Based Cuprate Superconductors

DOE Office of Scientific and Technical Information (OSTI.GOV)

Greven, Martin

This is the Final Report on DE-SC0006858, which opened 15 August 2011 and closed 14 August 2017. The Principal Investigator is Martin Greven, School of Physics and Astronomy, University of Minnesota, Minneapolis, MN 555455 (email: greven@umn.edu). The Administrative Point of Contact is Patricia Jondahl, phone: 612-624-5599, email: awards@umn.edu. The DOE Program is the Office of Basic Energy Sciences, Program manager is Dr. P. Thiyagarajan, Neutron Scattering SC-22.2/ Germantown Bldg. (email: Thiyagarajan@science.doe.gov). The chief activity was the crystal growth, characterization, neutron and X-ray scattering study of the mercury-based cuprates, arguably the most desirable high-Tc superconductors for experimental study due to theirmore » record values of Tc and their relatively simple crystal structures. It is thought that the unusual magnetic and charge degrees of freedom of the copper-oxygen sheets that form the fundamental building block of all cuprate superconductors give rise to the high Tc and to many other unusual properties exhibited by the class of quantum materials. Neutron scattering experiments were performed to reveal the nature of the magnetic degrees of freedom of the copper-oxygen sheets, whereas X-ray scattering experiments and complementary charge-transport experiments were performed to reveal the nature of the charge degrees of freedom. In addition, collaborations were initiated with experts in the use of complementary experimental techniques. The primary products are (i) scientific articles published in peer-reviewed scientific journals, (ii) scientific presentations at national and international conferences, and (iii) education of postdoctoral researchers, PhD graduate students and undergraduate researchers by providing a research experience in crystal growth, characterization and scattering. Twenty scientific papers were published in peer-reviewed journals, thirty-one invited talks were presented at national or international conferences, or as colloquia or seminars, and three postdoctoral researchers, six PhD graduate students and nine undergraduate researchers were supported wholly or in part in the pursuit of the scientific topics of this award. This report summarizes the activity and productivity, lists highlights, publications and conference presentations, postdocs, students and collaborators. A balance of zero remained at the close of the grant.« less

Study of FES/CAST/HGS

NASA Technical Reports Server (NTRS)

Workman, Gary L.; Cummings, Rick; Jones, Brian

1992-01-01

The microgravity materials processing program has been instrumental in providing the crystal growth community with an experimental environment to better understand the phenomena associated with the growing of crystals. In many applications one may pursue the growth of large single crystals which cannot be grown on earth due to convective driven flows. A microgravity environment is characterized by neither convection of buoyancy. Consequently superior crystals are able to be grown in space. On the other hand, since neither convection nor buoyancy dominates the fluid flow in a microgravity environment, then lesser dominating phenomena can affect crystal growth, such as surface driven flows or diffusion limited solidification. In the case of experiments that are to be flown in space using the Fluid Experiments System (FES), diffusion limited growth should be the dominating phenomenon. The use of holographic and Schlieren optical techniques for studying the concentration gradients in solidification processes has been used by several investigators over the years. The Holographic Ground System (HGS) facility at MSFC has been a primary resource in researching this capability. Consequently scientific personnel have been able to utilize these techniques in both ground based research and in space experiments. An important event in the scientific utilization of the HGS facilities was the TGS (triglycine sulfate) Crystal Growth and the Casting and Solidification Technology (CAST) experiments that were flown on the International Microgravity Lab (IML) mission in March of this year. The preparation and processing of these space observations are the primary experiments reported in this work. This project provides some ground-based studies to optimize on the holographic techniques used to acquire information about the crystal growth processes flown on IML. Since the ground-based studies will be compared with the space-based experimental results, it is necessary to conduct sufficient ground based studies to best determine how the experiment in space worked. The current capabilities in computer based systems for image processing and numerical computation have certainly assisted in those efforts. As anticipated, this study has certainly shown that these advanced computing capabilities are helpful in the data analysis of such experiments.

Critical experiments of the self-consistent model for polycrystalline Hastelloy-X

NASA Technical Reports Server (NTRS)

Shi, Shixiang; Walker, Kevin P.; Jordan, Eric H.

1991-01-01

A viscoplastic constitutive model is presented for the estimation of the overall mechanical response of Hastelloy-X polycrystalline metals from a knowledge of single crystal behavior. The behavior of polycrystal is derived from that of single crystals using a self-consistent formulation. The single crystal behavior which has been used was developed by summing postulated slip on crystallographic slip systems. The plasticity and creep are treated coupledly using unified viscoplastic model which includes the interaction effects between rapid and slow deformation at elevated temperature. The validity of the model is directly tested by experiments on Hastelloy-X in both single crystal and polycrystalline versions.

Chemo-mechanics of salt damage in stone.

PubMed

Flatt, Robert J; Caruso, Francesco; Sanchez, Asel Maria Aguilar; Scherer, George W

2014-09-11

Many porous materials are damaged by pressure exerted by salt crystals growing in their pores. This is a serious issue in conservation science, geomorphology, geotechnical engineering and concrete materials science. In all cases, a central question is whether crystallization pressure will cause damage. Here we present an experiment in which the crystallization pressure and the pore saturation are varied in a controlled way. We demonstrate that a strain energy failure criterion can be used to predict when damage will occur. The experiment considered is the most widely used means to study the susceptibility to salt crystallization, so quantification of this test has far-reaching implications.

The Crystallization of Canavalin as a Function of pH and NaCl Concentration

NASA Technical Reports Server (NTRS)

Forsythe, Elizabeth L.; Gorti, Sridhar; Pusey, Marc L.

2004-01-01

We posed the question of what happens to a protein that is known to grow as an n-mer when it is placed in solution conditions where it is monomeric. The trypsin-treated, or cut, form of the protein canavalin (CCAN) has been shown to nucleate and grow crystals as a trimer from neutral to slightly acidic solutions. Under these conditions the solution is composed almost wholly of trimers. The crystalline protein can be readily dissolved by weakly basic solution, which has been proposed to result in a solution that is monomeric. There are three possible outcomes to an attempt at crystallization of the protein under monomeric (high pH) conditions: 1) we will obtain the same crystals as under trimer conditions, but at different protein concentrations governed by the self association equilibria; 2) we will obtain crystals having a different symmetry, based upon a monomeric growth unit; 3) we will not obtain crystals. Obtaining the first result would be indicative that the solution-phase self-association process is critical to the crystal nucleation and growth process. The second result would be less clear, as it may also reflect a pH-dependent shift in the trimer-trimer molecular interactions. The third result, particularly for experiments in the transition pH's between trimeric and monomeric CCAN, would indicate that the monomer does not crystallize, and that solution phase self association is not part of the crystal nucleation and growth path. Results are presented for crystallization experiments of CCAN over the pH 6.4 to 9.6 range. Fluorescence anisotropy, light scattering, and gel filtration experiments show that the solutions are primarily trimers, with association to form larger species occurring as a function of protein concentration.

All-optical image processing with nonlinear liquid crystals

NASA Astrophysics Data System (ADS)

Hong, Kuan-Lun

Liquid crystals are fascinating materials because of several advantages such as large optical birefringence, dielectric anisotropic, and easily compatible to most kinds of materials. Compared to the electro-optical properties of liquid crystals widely applied in displays and switching application, transparency through most parts of wavelengths also makes liquid crystals a better candidate for all-optical processing. The fast response time of liquid crystals resulting from multiple nonlinear effects, such as thermal and density effect can even make real-time processing realized. In addition, blue phase liquid crystals with spontaneously self-assembled three dimensional cubic structures attracted academic attention. In my dissertation, I will divide the whole contents into six parts. In Chapter 1, a brief introduction of liquid crystals is presented, including the current progress and the classification of liquid crystals. Anisotropy and laser induced director axis reorientation is presented in Chapter 2. In Chapter 3, I will solve the electrostrictive coupled equation and analyze the laser induced thermal and density effect in both static and dynamic ways. Furthermore, a dynamic simulation of laser induced density fluctuation is proposed by applying finite element method. In Chapter 4, two image processing setups are presented. One is the intensity inversion experiment in which intensity dependent phase modulation is the mechanism. The other is the wavelength conversion experiment in which I can read the invisible image with a visible probe beam. Both experiments are accompanied with simulations to realize the matching between the theories and practical experiment results. In Chapter 5, optical properties of blue phase liquid crystals will be introduced and discussed. The results of grating diffractions and thermal refractive index gradient are presented in this chapter. In addition, fiber arrays imaging and switching with BPLCs will be included in this chapter. Finally, I will give a brief summary and mention a few future researches in Chapter 6.

Integrated Approach for Understanding Impurity Adsorption on Calcite: Mechanisms for Micro-scale Surface Phenomena

NASA Astrophysics Data System (ADS)

Vinson, M. D.; Arvidson, R. S.; Luttge, A.

2004-12-01

A longstanding goal within the field of environmental geochemistry has been the development of a fundamental understanding of the kinetics that governs the interactions of solution-borne impurities with the calcite mineral surface. Recent dissolution experiments using Mg2+, Mn2+, and Sr2+ have shown distinct differences in the interaction of these three impurity ions with the calcite crystal surface. Because the dissolution of carbonate minerals in soils and sediments influences the uptake and migration of groundwater contaminants, a rigorous understanding of the basic processes that occur at the mineral-fluid interface is necessary. We have used vertical scanning interferometry (VSI) coupled with scanning probe microscopy (SPM) to examine calcite crystal dissolution in the presence of Mg2+, Mn2+, and Sr2+, all known dissolution inhibitors and possible groundwater contaminants. We have studied the kinetics of impurity-crystal interactions at a pH 8.8, and in the presence or absence of dissolved inorganic carbon. Our data show that, when individually introduced into undersaturated solutions, Mg2+ and Mn2+ are shown to activate the calcite crystal surface, resulting in enhanced etch pit nucleation rates and step density. Conversely, Sr2+ is shown to cause passivation of the calcite surface. The effect is intensified when solutions are saturated with respect to atmospheric CO2. Results indicate that aqueous CO32- (or HCO3-) may influence how aqueous metal ionic complexes interact with the crystal surface. Furthermore, the influence is differently exhibited, and passivation or activation ultimately depends on the properties of the diffusing metal ion or metal-hydroxide complex. These properties include for example, differences in hydration enthalpy, the effective ionic radius, and electron shell configuration.

Protein Crystal Movements and Fluid Flows During Microgravity Growth

NASA Technical Reports Server (NTRS)

Boggon, Titus J.; Chayen, Naomi E.; Snell, Edward H.; Dong, Jun; Lautenschlager, Peter; Potthast, Lothar; Siddons, D. Peter; Stojanoff, Vivian; Gordon, Elspeth; Thompson, Andrew W.;

High-density grids for efficient data collection from multiple crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Baxter, Elizabeth L.; Aguila, Laura; Alonso-Mori, Roberto

Higher throughput methods to mount and collect data from multiple small and radiation-sensitive crystals are important to support challenging structural investigations using microfocus synchrotron beamlines. Furthermore, efficient sample-delivery methods are essential to carry out productive femtosecond crystallography experiments at X-ray free-electron laser (XFEL) sources such as the Linac Coherent Light Source (LCLS). To address these needs, a high-density sample grid useful as a scaffold for both crystal growth and diffraction data collection has been developed and utilized for efficient goniometer-based sample delivery at synchrotron and XFEL sources. A single grid contains 75 mounting ports and fits inside an SSRL cassettemore » or uni-puck storage container. The use of grids with an SSRL cassette expands the cassette capacity up to 7200 samples. Grids may also be covered with a polymer film or sleeve for efficient room-temperature data collection from multiple samples. New automated routines have been incorporated into theBlu-Ice/DCSSexperimental control system to support grids, including semi-automated grid alignment, fully automated positioning of grid ports, rastering and automated data collection. Specialized tools have been developed to support crystallization experiments on grids, including a universal adaptor, which allows grids to be filled by commercial liquid-handling robots, as well as incubation chambers, which support vapor-diffusion and lipidic cubic phase crystallization experiments. Experiments in which crystals were loaded into grids or grown on grids using liquid-handling robots and incubation chambers are described. As a result, crystals were screened at LCLS-XPP and SSRL BL12-2 at room temperature and cryogenic temperatures.« less

High-density grids for efficient data collection from multiple crystals

PubMed Central

Baxter, Elizabeth L.; Aguila, Laura; Alonso-Mori, Roberto; Barnes, Christopher O.; Bonagura, Christopher A.; Brehmer, Winnie; Brunger, Axel T.; Calero, Guillermo; Caradoc-Davies, Tom T.; Chatterjee, Ruchira; Degrado, William F.; Fraser, James S.; Ibrahim, Mohamed; Kern, Jan; Kobilka, Brian K.; Kruse, Andrew C.; Larsson, Karl M.; Lemke, Heinrik T.; Lyubimov, Artem Y.; Manglik, Aashish; McPhillips, Scott E.; Norgren, Erik; Pang, Siew S.; Soltis, S. M.; Song, Jinhu; Thomaston, Jessica; Tsai, Yingssu; Weis, William I.; Woldeyes, Rahel A.; Yachandra, Vittal; Yano, Junko; Zouni, Athina; Cohen, Aina E.

2016-01-01

Higher throughput methods to mount and collect data from multiple small and radiation-sensitive crystals are important to support challenging structural investigations using microfocus synchrotron beamlines. Furthermore, efficient sample-delivery methods are essential to carry out productive femtosecond crystallography experiments at X-ray free-electron laser (XFEL) sources such as the Linac Coherent Light Source (LCLS). To address these needs, a high-density sample grid useful as a scaffold for both crystal growth and diffraction data collection has been developed and utilized for efficient goniometer-based sample delivery at synchrotron and XFEL sources. A single grid contains 75 mounting ports and fits inside an SSRL cassette or uni-puck storage container. The use of grids with an SSRL cassette expands the cassette capacity up to 7200 samples. Grids may also be covered with a polymer film or sleeve for efficient room-temperature data collection from multiple samples. New automated routines have been incorporated into the Blu-Ice/DCSS experimental control system to support grids, including semi-automated grid alignment, fully automated positioning of grid ports, rastering and automated data collection. Specialized tools have been developed to support crystallization experiments on grids, including a universal adaptor, which allows grids to be filled by commercial liquid-handling robots, as well as incubation chambers, which support vapor-diffusion and lipidic cubic phase crystallization experiments. Experiments in which crystals were loaded into grids or grown on grids using liquid-handling robots and incubation chambers are described. Crystals were screened at LCLS-XPP and SSRL BL12-2 at room temperature and cryogenic temperatures. PMID:26894529

Plagioclase nucleation and growth kinetics in a hydrous basaltic melt by decompression experiments

NASA Astrophysics Data System (ADS)

Arzilli, Fabio; Agostini, C.; Landi, P.; Fortunati, A.; Mancini, L.; Carroll, M. R.

2015-12-01

Isothermal single-step decompression experiments (at temperature of 1075 °C and pressure between 5 and 50 MPa) were used to study the crystallization kinetics of plagioclase in hydrous high-K basaltic melts as a function of pressure, effective undercooling (Δ T eff) and time. Single-step decompression causes water exsolution and a consequent increase in the plagioclase liquidus, thus imposing an effective undercooling (Δ T eff), accompanied by increased melt viscosity. Here, we show that the decompression process acts directly on viscosity and thermodynamic energy barriers (such as interfacial-free energy), controlling the nucleation process and favoring the formation of homogeneous nuclei also at high pressure (low effective undercoolings). In fact, this study shows that similar crystal number densities ( N a) can be obtained both at low and high pressure (between 5 and 50 MPa), whereas crystal growth processes are favored at low pressures (5-10 MPa). The main evidence of this study is that the crystallization of plagioclase in decompressed high-K basalts is more rapid than that in rhyolitic melts on similar timescales. The onset of the crystallization process during experiments was characterized by an initial nucleation event within the first hour of the experiment, which produced the largest amount of plagioclase. This nucleation event, at short experimental duration, can produce a dramatic change in crystal number density ( N a) and crystal fraction ( ϕ), triggering a significant textural evolution in only 1 h. In natural systems, this may affect the magma rheology and eruptive dynamics on very short time scales.

High-density grids for efficient data collection from multiple crystals

DOE PAGES

Baxter, Elizabeth L.; Aguila, Laura; Alonso-Mori, Roberto; ...

2015-11-03

Higher throughput methods to mount and collect data from multiple small and radiation-sensitive crystals are important to support challenging structural investigations using microfocus synchrotron beamlines. Furthermore, efficient sample-delivery methods are essential to carry out productive femtosecond crystallography experiments at X-ray free-electron laser (XFEL) sources such as the Linac Coherent Light Source (LCLS). To address these needs, a high-density sample grid useful as a scaffold for both crystal growth and diffraction data collection has been developed and utilized for efficient goniometer-based sample delivery at synchrotron and XFEL sources. A single grid contains 75 mounting ports and fits inside an SSRL cassettemore » or uni-puck storage container. The use of grids with an SSRL cassette expands the cassette capacity up to 7200 samples. Grids may also be covered with a polymer film or sleeve for efficient room-temperature data collection from multiple samples. New automated routines have been incorporated into theBlu-Ice/DCSSexperimental control system to support grids, including semi-automated grid alignment, fully automated positioning of grid ports, rastering and automated data collection. Specialized tools have been developed to support crystallization experiments on grids, including a universal adaptor, which allows grids to be filled by commercial liquid-handling robots, as well as incubation chambers, which support vapor-diffusion and lipidic cubic phase crystallization experiments. Experiments in which crystals were loaded into grids or grown on grids using liquid-handling robots and incubation chambers are described. As a result, crystals were screened at LCLS-XPP and SSRL BL12-2 at room temperature and cryogenic temperatures.« less

Dynamic Crystallization Experiments on LEW97008: Experimental Reproduction of Chondroid Textures

NASA Technical Reports Server (NTRS)

Nettles, J. W.; Le, L.; Lofgren, G. E.; McSween, H. Y, Jr.

2003-01-01

Dynamic crystallization experiments were conducted using LEW97008 (L3.4) as starting material. Experiments were melted at temperatures well below its liquidus (1250-1450 C) in order to document the textural and compositional changes that occur in UOC material with modest amounts of partial melting and subsequent crystallization. The textures of the experimental products compare very well to natural chondroids (partially melted nebular particles that would become chondrules if more completely melted). Thus it is possible to use the textures in these experiments as a guide to unraveling the melting and cooling histories of natural chondroids. The Antarctic meteorite LEW97008 was chosen as the starting material for our experiments. As an L3.4 it is slightly more metamorphosed than would ordinarily be preferred, but this meteorite is unusually fresh for an Antarctic meteorite, which made it attractive.

An automated image-collection system for crystallization experiments using SBS standard microplates.

PubMed

Brostromer, Erik; Nan, Jie; Su, Xiao Dong

2007-02-01

As part of a structural genomics platform in a university laboratory, a low-cost in-house-developed automated imaging system for SBS microplate experiments has been designed and constructed. The imaging system can scan a microplate in 2-6 min for a 96-well plate depending on the plate layout and scanning options. A web-based crystallization database system has been developed, enabling users to follow their crystallization experiments from a web browser. As the system has been designed and built by students and crystallographers using commercially available parts, this report is aimed to serve as a do-it-yourself example for laboratory robotics.

SABRE - A test of DAMA with high-purity NaI(Tl) crystals

NASA Astrophysics Data System (ADS)

Xu, Jingke; Calaprice, Frank; Froborg, Francis; Shields, Emily; Suerfu, Burkhant

2015-08-01

The dark matter claim by DAMA is both significant and controversial. Several experiments have claimed to rule out DAMA/LIBRA, but the comparisons are made based on dark matter halo and dark matter-interaction models that are currently unknown. Therefore, an unambiguous test of DAMA/LIBRA is best made using NaI(Tl) crystals with lower residual background than that of DAMA/LIBRA, and the SABRE experiment is designed to achieve this goal. In this paper we will discuss the development of high-purity SABRE NaI(Tl) crystals and detectors, and progress of the SABRE experiment toward testing DAMA/LIBRA.

Stability Enhancement of Polymeric Sensing Films Using Fillers

NASA Technical Reports Server (NTRS)

Lin, Brian; Shevade, Abhijit; Ryan, Margaret Amy; Kisor, Adam; Yen, Shiao-Pin; Manatt, Kenneth; Homer, Margie; Fleurial, Jean-Pierre

2006-01-01

Experiments have shown the stability enhancement of polymeric sensing films on mixing the polymer with colloidal filler particles (submicron-sized) of carbon black, silver, titanium dioxide, and fumed silicon dioxide. The polymer films are candidates for potential use as sensing media in micro/nano chemical sensor devices. The need for stability enhancement of polymer sensing films arises because such films have been found to exhibit unpredictable changes in sensing activity over time, which could result in a possible failure of the sensor device. The changes in the physical properties of a polymer sensing film caused by the sorption of a target molecule can be measured by any of several established transduction techniques: electrochemical, optical, calorimetric, or piezoelectric, for example. The transduction technique used in the current polymer stability experiments is based on piezoelectric principles using a quartz-crystal microbalance (QCM). The surface of the QCM is coated with the polymer, and the mass uptake by the polymer film causes a change in the oscillating frequency of the quartz crystal. The polymer used for the current study is ethyl cellulose. The polymer/ polymer composite solutions were prepared in 1,3 dioxolane solvent. The filler concentration was fixed at 10 weight percent for the composites. The polymer or polymer composite solutions were cast on the quartz crystal having a fundamental frequency of about 6 MHz. The coated crystal was subjected to a multistage drying process to remove all measurable traces of the solvent. In each experiment, the frequency of oscillation was measured while the QCM was exposed to clean, dry, flowing air for about 30 minutes, then to air containing a known concentration of isopropanol for about 30 minutes, then again to clean dry air for about 30 minutes, and so forth. This cycle of measurements for varying isopropanol concentrations was repeated at intervals for several months. The figure depicts some of the sensing film stability results for ethyl cellulose polymer, ethyl cellulose-carbon black, and ethyl cellulose-silicon dioxide composite systems. An ethyl cellulose film exhibited a marked decline in response in the first few months of study and settled to a steady average response after about four months. However, response varied widely around the average response for ethyl cellulose film. In contrast, ethyl cellulose- carbon black and ethyl cellulose-silicon dioxide composites also declined in the early months, but showed more repeatable sensing film activity after the initial decline. Similar trends were observed in experiments for ethyl cellulose-titanium dioxide and ethyl cellulose-silver composites.

Crucible de-wetting during bridgman growth of semiconductors in microgravity

NASA Astrophysics Data System (ADS)

Duffar, T.; Paret-Harter, I.; Dusserre, P.

1990-02-01

After a literature survey and observations made during a space experiment, the phenomenon of crucible de-wetting by the crystal during Bridgman solidification in microgravity is explained by a model involving composite wetting of the crucible by the liquid, crystal angle of growth and interface advance. A ground experiment was run in order to validate this model which also explains why a crystal detaches from the crucible surface when a sand blasted crucible is used in Bridgman solidification on the ground. It is shown that de-wetting leads to enhanced quality of the crystal produced and that capillary-induced convection effects are not to be feared in this case. Consequently, it is highly advisable to use rough-surface crucibles for crystal growth both in microgravity and on the ground.

Solid-Phase and Oscillating Solution Crystallization Behavior of (+)- and (-)-N-Methylephedrine.

PubMed

Tulashie, Samuel Kofi; Polenske, Daniel; Seidel-Morgenstern, Andreas; Lorenz, Heike

2016-11-01

This work involves the study of the solid-phase and solution crystallization behavior of the N-methylephedrine enantiomers. A systematic investigation of the melt phase diagram of the enantiomeric N-methylephedrine system was performed considering polymorphism. Two monotropically related modifications of the enantiomer were found. Solubilities and the ternary solubility phase diagrams of N-methylephedrine enantiomers in 2 solvents [isopropanol:water, 1:3 (Vol) and (2R, 3R)-diethyl tartrate] were determined in the temperature ranges between 15°C and 25°C, and 25°C and 40°C, respectively. Preferential nucleation and crystallization experiments at higher supersaturation leading to an unusual oscillatory crystallization behavior as well as a successful preferential crystallization experiment at lower supersaturation are presented and discussed. Copyright © 2016. Published by Elsevier Inc.

Romanenko works with the Coulomb Crystal Experiment in the MRM-2

NASA Image and Video Library

2013-01-28

ISS034-E-035764 (28 Jan. 2013) --- In the International Space Station?s Poisk Mini-Research Module 2 (MRM2), Russian cosmonaut Roman Romanenko, Expedition 34 flight engineer, works with the Coulomb Crystal experiment, which gathers data about charged particles in a weightless environment.

Rotational Mobility in a Crystal Studied by Dielectric Relaxation Spectroscopy

ERIC Educational Resources Information Center

Dionisio, Madalena S. C.; Diogo, Herminio P.; Farinha, J. P. S.; Ramos, Joaquim J. Moura

2005-01-01

A laboratory experiment for undergraduate physical chemistry courses that uses the experimental technique of dielectric relaxation spectroscopy to study molecular mobility in a crystal is proposed. An experiment provides an excellent opportunity for dealing with a wide diversity of important basic concepts in physical chemistry.

The Quartz-Crystal Microbalance in an Undergraduate Laboratory Experiment: Measuring Mass

ERIC Educational Resources Information Center

Tsionsky, Vladimir

2007-01-01

The study explains the quartz-crystal microbalance (QCM) technique, which is often used as an undergraduate laboratory experiment for measuring the mass of a system. QCM can be used as a mass sensor only when the measured mass is rigidly attached to the surface.

Struvite crystal growth inhibition by trisodium citrate and the formation of chemical complexes in growth solution

NASA Astrophysics Data System (ADS)

Prywer, Jolanta; Mielniczek-Brzóska, Ewa; Olszynski, Marcin

2015-05-01

Effect of trisodium citrate on the crystallization of struvite was studied. To evaluate such an effect an experiment of struvite growth from artificial urine was performed. The investigations are related to infectious urinary stones formation. The crystallization process was induced by the addition of aqueous ammonia solution to mimic the bacterial activity. The spectrophotometric results demonstrate that trisodium citrate increases induction time with respect to struvite formation and decreases the growth efficiency of struvite. The inhibitory effect of trisodium citrate on the nucleation and growth of struvite is explained in base of chemical speciation analysis. Such an analysis demonstrates that the inhibitory effect is related with the fact that trisodium citrate binds NH4 + and Mg2+ ions in the range of pH from 7 to 9.5 characteristic for struvite precipitation. The most important is the MgCit- complex whose concentration strongly depends on an increase in pH rather than on an increase in citrate concentrations.

Crystal Facets Make a Profound Difference in Polyoxometalate-Containing Metal-Organic Frameworks as Catalysts for Biodiesel Production.

PubMed

Liu, Yiwei; Liu, Shumei; He, Danfeng; Li, Ning; Ji, Yujuan; Zheng, Zhiping; Luo, Fang; Liu, Shuxia; Shi, Zhan; Hu, Changwen

2015-10-07

An inherent challenge in using metal-organic frameworks (MOFs) for catalysis is how to access the catalytic sites generally confined inside the porous structure, in particular for substrates larger than the pores. We present here a promising solution to bypass this roadblock by modulating the facets of a crystalline MOF NENU-3a to enhance the facet exposure of the catalytic sites and the adsorption of substrates. Specifically, by transforming it with encapsulated catalysis-responsible polyoxometalate from octahedron characterized entirely by {111} facets to cube with only {100} facets, much enhanced catalytic activities were observed, especially for sterically demanding substrates that are otherwise hard to diffuse into the pores. Crystallographic analysis and adsorption/desorption experiments collectively established the critical effects of morphological control on the enhanced catalysis. The cubic crystals were then applied for biodiesel production, reaching more than 90% conversion of fatty acids (C12-C22) in comparison to <22% using octahedral crystals.

Organic Crystal Growth Facility (OCGF) and Radiation Monitoring Container Device (RMCD) Groups in

NASA Technical Reports Server (NTRS)

1992-01-01

The primary payload for Space Shuttle Mission STS-42, launched January 22, 1992, was the International Microgravity Laboratory-1 (IML-1), a pressurized manned Spacelab module. The goal of IML-1 was to explore in depth the complex effects of weightlessness of living organisms and materials processing. Around-the-clock research was performed on the human nervous system's adaptation to low gravity and effects of microgravity on other life forms such as shrimp eggs, lentil seedlings, fruit fly eggs, and bacteria. Materials processing experiments were also conducted, including crystal growth from a variety of substances such as enzymes, mercury iodide, and a virus. The Huntsville Operations Support Center (HOSC) Spacelab Payload Operations Control Center (SL POCC) at the Marshall Space Flight Center (MSFC) was the air/ground communication channel used between the astronauts and ground control teams during the Spacelab missions. Featured are activities of the Organic Crystal Growth Facility (OCGF) and Radiation Monitoring Container Device (RMCD) groups in the SL POCC during the IML-1 mission.

Kinetics of liquid-mediated crystallization of amorphous Ge from multi-frame dynamic transmission electron microscopy

DOE PAGES

Santala, M. K.; Raoux, S.; Campbell, G. H.

2015-12-24

The kinetics of laser-induced, liquid-mediated crystallization of amorphous Ge thin films were studied using multi-frame dynamic transmission electron microscopy (DTEM), a nanosecond-scale photo-emission transmission electron microscopy technique. In these experiments, high temperature gradients are established in thin amorphous Ge films with a 12-ns laser pulse with a Gaussian spatial profile. The hottest region at the center of the laser spot crystallizes in ~100 ns and becomes nano-crystalline. Over the next several hundred nanoseconds crystallization continues radially outward from the nano-crystalline region forming elongated grains, some many microns long. The growth rate during the formation of these radial grains is measuredmore » with time-resolved imaging experiments. Crystal growth rates exceed 10 m/s, which are consistent with crystallization mediated by a very thin, undercooled transient liquid layer, rather than a purely solid-state transformation mechanism. The kinetics of this growth mode have been studied in detail under steady-state conditions, but here we provide a detailed study of liquid-mediated growth in high temperature gradients. Unexpectedly, the propagation rate of the crystallization front was observed to remain constant during this growth mode even when passing through large local temperature gradients, in stark contrast to other similar studies that suggested the growth rate changed dramatically. As a result, the high throughput of multi-frame DTEM provides gives a more complete picture of the role of temperature and temperature gradient on laser crystallization than previous DTEM experiments.« less

Kinetics of liquid-mediated crystallization of amorphous Ge from multi-frame dynamic transmission electron microscopy

DOE Office of Scientific and Technical Information (OSTI.GOV)

Santala, M. K., E-mail: melissa.santala@oregonstate.edu; Campbell, G. H.; Raoux, S.

2015-12-21

The kinetics of laser-induced, liquid-mediated crystallization of amorphous Ge thin films were studied using multi-frame dynamic transmission electron microscopy (DTEM), a nanosecond-scale photo-emission transmission electron microscopy technique. In these experiments, high temperature gradients are established in thin amorphous Ge films with a 12-ns laser pulse with a Gaussian spatial profile. The hottest region at the center of the laser spot crystallizes in ∼100 ns and becomes nano-crystalline. Over the next several hundred nanoseconds crystallization continues radially outward from the nano-crystalline region forming elongated grains, some many microns long. The growth rate during the formation of these radial grains is measured withmore » time-resolved imaging experiments. Crystal growth rates exceed 10 m/s, which are consistent with crystallization mediated by a very thin, undercooled transient liquid layer, rather than a purely solid-state transformation mechanism. The kinetics of this growth mode have been studied in detail under steady-state conditions, but here we provide a detailed study of liquid-mediated growth in high temperature gradients. Unexpectedly, the propagation rate of the crystallization front was observed to remain constant during this growth mode even when passing through large local temperature gradients, in stark contrast to other similar studies that suggested the growth rate changed dramatically. The high throughput of multi-frame DTEM provides gives a more complete picture of the role of temperature and temperature gradient on laser crystallization than previous DTEM experiments.« less

Thaumatin crystallization aboard the International Space Station using liquid-liquid diffusion in the Enhanced Gaseous Nitrogen Dewar (EGN).

PubMed

Barnes, Cindy L; Snell, Edward H; Kundrot, Craig E

2002-05-01

This paper reports results from the first biological crystal-growth experiment on the International Space Station (ISS). Crystals of thaumatin were grown using liquid-liquid diffusion in Tygon tubing transported in the Enhanced Gaseous Nitrogen Dewar (EGN). Different volume ratios and concentrations of protein and precipitant were used to test different adaptations of the vapor-diffusion crystallization recipe to the liquid-liquid diffusion method. The EGN warmed up from 77 to 273 K in about 4 d, about the same time it took to warm from 273 to 293 K. The temperature within the EGN was 293-297 K for the majority of the experiment. Air gaps that blocked liquid-liquid diffusion formed in the tubes. Nonetheless, crystals were grown. Synchrotron diffraction data collected from the best space-grown crystal extended to 1.28 A, comparable to previous studies of space-grown thaumatin crystals. The resolution of the best ground-control crystal was only 1.47 A. It is not clear if the difference in diffraction limit arises from factors other than crystal size. Improvements in temperature control and the elimination of air gaps are needed, but the results show that the EGN on the ISS can be used to produce space-grown crystals that diffract to high resolution.

Thaumatin Crystallization Aboard the International Space Station Using Liquid-Liquid Diffusion in the Enhanced Gaseous Nitrogen Dewar (EGN)

NASA Technical Reports Server (NTRS)

Kundrot, Craig; Barnes, Cindy L.; Snell, Edward H.; Stinson, Thomas N. (Technical Monitor)

2002-01-01

This paper reports results from the first biological crystal growth experiment on the International Space Station (ISS). Crystals of thaumatin were grown using liquid-liquid diffusion in Tygon tubing transported in the Enhanced Gaseous Nitrogen Dewar (EGN). Different Volume ratios and concentrations of protein and precipitant were used to test different adaptations of the vapor diffusion crystallization recipe to the liquid-liquid diffusion method. The EGN warmed up from -196 C to 0 C in about four days, about the same time it took to warm from 0 C to 20 C. The temperature within the EGN was 20 - 24 C for the majority of the experiment. Air gaps that blocked liquid-liquid diffusion formed in the tubes. Nonetheless, crystals were grown. Synchrotron diffraction data collected from the best space grown crystal extended to 1.28 Angstroms, comparable to previous studies of space-grown thaumatin crystals. The resolution of the best ground control crystal was only 1.47 Angstroms. It is not clear if the difference in diffraction limit is due to factors other than crystal size. Improvements in temperature control and the elimination of air gaps are needed, but the results show that EGN on the ISS can be used to produce space grown crystals that diffract to high resolution.

A simple technique to reduce evaporation of crystallization droplets by using plate lids with apertures for adding liquids.

PubMed

Zipper, Lauren E; Aristide, Xavier; Bishop, Dylan P; Joshi, Ishita; Kharzeev, Julia; Patel, Krishna B; Santiago, Brianna M; Joshi, Karan; Dorsinvil, Kahille; Sweet, Robert M; Soares, Alexei S

2014-12-01

A method is described for using plate lids to reduce evaporation in low-volume vapor-diffusion crystallization experiments. The plate lids contain apertures through which the protein and precipitants were added to different crystallization microplates (the reservoir was filled before fitting the lids). Plate lids were designed for each of these commonly used crystallization microplates. This system minimizes the dehydration of crystallization droplets containing just a few nanolitres of protein and precipitant, and results in more reproducible diffraction from the crystals. For each lid design, changes in the weight of the plates were used to deduce the rate of evaporation under different conditions of temperature, air movement, droplet size and precipitant. For comparison, the state of dehydration was also visually assessed throughout the experiment. Finally, X-ray diffraction methods were used to compare the diffraction of protein crystals that were conventionally prepared against those that were prepared on plates with plate lids. The measurements revealed that the plate lids reduced the rate of evaporation by 63-82%. Crystals grown in 5 nl drops that were set up with plate lids diffracted to higher resolution than similar crystals from drops that were set up without plate lids. The results demonstrate that plate lids can be instrumental for improving few-nanolitre crystallizations.

Crystallization of the collagen-like polypeptide (PPG)10 aboard the International Space Station. 1. Video observation.

PubMed

Vergara, Alessandro; Corvino, Ermanno; Sorrentino, Giosué; Piccolo, Chiara; Tortora, Alessandra; Carotenuto, Luigi; Mazzarella, Lelio; Zagari, Adriana

2002-10-01

Single chains of the collagen model polypeptide with sequence (Pro-Pro-Gly)(10), hereafter referred to as (PPG)(10), aggregate to form rod-shaped triple helices. Crystals of (PPG)(10) were grown in the Advanced Protein Crystallization Facility (APCF) both onboard the International Space Station (ISS) and on Earth. The experiments allow the direct comparison of four different crystallization environments for the first time: solution in microgravity ((g), agarose gel in (g, solution on earth, and gel on earth. Both on board and on ground, the crystal growth was monitored by a CCD video camera. The image analysis provided information on the spatial distribution of the crystals, their movement and their growth rate. The analysis of the distribution of crystals reveals that the crystallization process occurs as it does in batch conditions. Slow motions have been observed onboard the ISS. Different to Space-Shuttle experiment, the crystals onboard the ISS moved coherently and followed parallel trajectories. Growth rate and induction time are very similar both in gel and in solution, suggesting that the crystal growth rate is controlled by the kinetics at the interface under the used experimental conditions. These results provide the first data in the crystallogenesis of (PPG)(10), which is a representative member of non-globular, rod-like proteins.

Protein Crystal Growth (PCG) experiment aboard mission STS-66

NASA Technical Reports Server (NTRS)

2000-01-01

On the Space Shuttle Orbiter Atlantis' middeck, Astronaut Joseph R. Tarner, mission specialist, works at an area amidst several lockers which support the Protein Crystal Growth (PCG) experiment during the STS-66 mission. This particular section is called the Crystal Observation System, housed in the Thermal Enclosure System (COS/TES). Together with the Vapor Diffusion Apparatus (VDA), housed in Single Locker Thermal Enclosure (SLTES), the COS/TES represents the continuing research into the structure of proteins and other macromolecules such as viruses.

Ultra-Rapid Crystallization of L-alanine Using Monomode Microwaves, Indium Tin Oxide and Metal-Assisted and Microwave-Accelerated Evaporative Crystallization.

PubMed

Lansiquot, Carisse; Boone-Kukoyi, Zainab; Shortt, Raquel; Thompson, Nishone; Ajifa, Hillary; Kioko, Bridgit; Constance, Edward Ned; Clement, Travis; Ozturk, Birol; Aslan, Kadir

2017-01-01

The use of indium tin oxide (ITO) and focused monomode microwave heating for the ultra-rapid crystallization of L-alanine (a model amino acid) is reported. Commercially available ITO dots (< 5 mm) attached to blank poly(methyl)methacrylate (PMMA, 5 cm in diameter with 21-well silicon isolators: referred to as the iCrystal plates) were found to withstand prolonged microwave heating during crystallization experiments. Crystallization of L-alanine was performed at room temperature (a control experiment), with the use of two microwave sources: a 2.45 GHz conventional microwave (900 W, power level 1, a control experiment) and 8 GHz (20 W) solid state, monomode microwave source with an applicator tip that focuses the microwave field to a 5-mm cavity. Initial appearance of L-alanine crystals and on iCrystal plates with ITO dots took 47 ± 2.9 min, 12 ± 7.6 min and 1.5 ± 0.5 min at room temperature, using a conventional microwave and focused monomode microwave heating, respectively. Complete evaporation of the solvent using the focused microwaves was achieved in 3.2 ± 0.5 min, which is ~52-fold and ~172-fold faster than that observed at room temperature and using conventional microwave heating, respectively. The size and number of L-alanine crystals was dependent on the type of the 21-well iCrystal plates and the microwave heating method: 33 crystals of 585 ± 137 μm in size at room temperature > 37 crystals of 542 ± 100 μm in size with conventional microwave heating > 331 crystals of 311 ± 190 μm in size with focused monomode microwave. FTIR, optical microscopy and powder X-ray diffraction analysis showed that the chemical composition and crystallinity of the L-alanine crystals did not change when exposed to microwave heating and ITO surfaces. In addition, theoretical simulations for the binding of L-alanine molecules to ITO and other metals showed the predicted nature of hydrogen bonds formed between L-alanine and these surfaces.

Ultra-Rapid Crystallization of L-alanine Using Monomode Microwaves, Indium Tin Oxide and Metal-Assisted and Microwave-Accelerated Evaporative Crystallization

PubMed Central

Lansiquot, Carisse; Boone-Kukoyi, Zainab; Shortt, Raquel; Thompson, Nishone; Ajifa, Hillary; Kioko, Bridgit; Constance, Edward Ned; Clement, Travis; Ozturk, Birol; Aslan, Kadir

2018-01-01

The use of indium tin oxide (ITO) and focused monomode microwave heating for the ultra-rapid crystallization of L-alanine (a model amino acid) is reported. Commercially available ITO dots (< 5 mm) attached to blank poly(methyl)methacrylate (PMMA, 5 cm in diameter with 21-well silicon isolators: referred to as the iCrystal plates) were found to withstand prolonged microwave heating during crystallization experiments. Crystallization of L-alanine was performed at room temperature (a control experiment), with the use of two microwave sources: a 2.45 GHz conventional microwave (900 W, power level 1, a control experiment) and 8 GHz (20 W) solid state, monomode microwave source with an applicator tip that focuses the microwave field to a 5-mm cavity. Initial appearance of L-alanine crystals and on iCrystal plates with ITO dots took 47 ± 2.9 min, 12 ± 7.6 min and 1.5 ± 0.5 min at room temperature, using a conventional microwave and focused monomode microwave heating, respectively. Complete evaporation of the solvent using the focused microwaves was achieved in 3.2 ± 0.5 min, which is ~52-fold and ~172-fold faster than that observed at room temperature and using conventional microwave heating, respectively. The size and number of L-alanine crystals was dependent on the type of the 21-well iCrystal plates and the microwave heating method: 33 crystals of 585 ± 137 μm in size at room temperature > 37 crystals of 542 ± 100 μm in size with conventional microwave heating > 331 crystals of 311 ± 190 μm in size with focused monomode microwave. FTIR, optical microscopy and powder X-ray diffraction analysis showed that the chemical composition and crystallinity of the L-alanine crystals did not change when exposed to microwave heating and ITO surfaces. In addition, theoretical simulations for the binding of L-alanine molecules to ITO and other metals showed the predicted nature of hydrogen bonds formed between L-alanine and these surfaces. PMID:29657884

The Release of Trapped Gases from Amorphous Solid Water Films: I. “Top-Down” Crystallization-Induced Crack Propagation Probed using the Molecular Volcano

DOE Office of Scientific and Technical Information (OSTI.GOV)

May, Robert A.; Smith, R. Scott; Kay, Bruce D.

In this (Paper I) and the companion paper (Paper II) we investigate the mechanisms for the release of trapped gases from underneath of amorphous solid water (ASW) films. In prior work, we reported the episodic release of trapped gases in concert with the crystallization ASW, a phenomenon that we termed the "molecular volcano". The observed abrupt desorption is due to the formation of cracks that span the film to form a connected pathway for release. In this paper we utilize the "molecular volcano" desorption peak to characterize the formation of crystallization-induced cracks. We find that the crack length and distributionmore » are independent of the trapped gas (Ar, Kr, Xe, CH4, N2, O2 or CO). Selective placement of the inert gas layer is used to show that cracks form near the top of the film and propagate downward into the film. Isothermal experiments reveal that, after some induction time, cracks propagate linearly in time with an Arrhenius dependent velocity corresponding to an activation energy of 54 kJ/mol. This value is consistent with the crystallization growth rate reported by others and establishes a direct connection between crystallization growth rate and the crack propagation rate. A two-step model in which nucleation and crystallization occurs in an induction zone near the top of the film followed by the propagation of a crystallization/crack front into the film is in good agreement with the temperature programmed desorption results.« less

Crystal-to-Crystal Transition of Ultrasoft Colloids under Shear

NASA Astrophysics Data System (ADS)

Ruiz-Franco, J.; Marakis, J.; Gnan, N.; Kohlbrecher, J.; Gauthier, M.; Lettinga, M. P.; Vlassopoulos, D.; Zaccarelli, E.

2018-02-01

Ultrasoft colloids typically do not spontaneously crystallize, but rather vitrify, at high concentrations. Combining in situ rheo-small-angle-neutron-scattering experiments and numerical simulations we show that shear facilitates crystallization of colloidal star polymers in the vicinity of their glass transition. With increasing shear rate well beyond rheological yielding, a transition is found from an initial bcc-dominated structure to an fcc-dominated one. This crystal-to-crystal transition is not accompanied by intermediate melting but occurs via a sudden reorganization of the crystal structure. Our results provide a new avenue to tailor colloidal crystallization and the crystal-to-crystal transition at the molecular level by coupling softness and shear.

In situ diagnostics of the crystal-growth process through neutron imaging: application to scintillators

DOE PAGES

Tremsin, Anton S.; Makowska, Małgorzata G.; Perrodin, Didier; ...

2016-04-12

Neutrons are known to be unique probes in situations where other types of radiation fail to penetrate samples and their surrounding structures. In this paper it is demonstrated how thermal and cold neutron radiography can provide time-resolved imaging of materials while they are being processed (e.g.while growing single crystals). The processing equipment, in this case furnaces, and the scintillator materials are opaque to conventional X-ray interrogation techniques. The distribution of the europium activator within a BaBrCl:Eu scintillator (0.1 and 0.5% nominal doping concentrations per mole) is studiedin situduring the melting and solidification processes with a temporal resolution of 5–7 s.more » The strong tendency of the Eu dopant to segregate during the solidification process is observed in repeated cycles, with Eu forming clusters on multiple length scales (only for clusters larger than ~50 µm, as limited by the resolution of the present experiments). It is also demonstrated that the dopant concentration can be quantified even for very low concentration levels (~0.1%) in 10 mm thick samples. The interface between the solid and liquid phases can also be imaged, provided there is a sufficient change in concentration of one of the elements with a sufficient neutron attenuation cross section. Tomographic imaging of the BaBrCl:0.1%Eu sample reveals a strong correlation between crystal fractures and Eu-deficient clusters. The results of these experiments demonstrate the unique capabilities of neutron imaging forin situdiagnostics and the optimization of crystal-growth procedures.« less

A simple apparatus for controlling nucleation and size in protein crystal growth

NASA Technical Reports Server (NTRS)

Gernert, Kim M.; Smith, Robert; Carter, Daniel C.

1988-01-01

A simple device is described for controlling vapor equilibrium in macromolecular crystallization as applied to the protein crystal growth technique commonly referred to as the 'hanging drop' method. Crystal growth experiments with hen egg white lysozyme have demonstrated control of the nucleation rate. Nucleation rate and final crystal size have been found to be highly dependent upon the rate at which critical supersaturation is approached. Slower approaches show a marked decrease in the nucleation rate and an increase in crystal size.

Microgravity

NASA Image and Video Library

1992-02-21

Vapor Crystal Growth System developed in IML-1, Mercuric Iodide Crystal grown in microgravity FES/VCGS (Fluids Experiment System/Vapor Crystal Growth Facility). During the mission, mercury iodide source material was heated, vaporized, and transported to a seed crystal where the vapor condensed. Mercury iodide crystals have practical uses as sensitive X-ray and gamma-ray detectors. In addition to their excellent optical properties, these crystals can operate at room temperature, which makes them useful for portable detector devices for nuclear power plant monitoring, natural resource prospecting, biomedical applications, and astronomical observing.

Realization of a complementary medium using dielectric photonic crystals.

PubMed

Xu, Tao; Fang, Anan; Jia, Ziyuan; Ji, Liyu; Hang, Zhi Hong

2017-12-01

By exploiting the scaling invariance of photonic band diagrams, a complementary photonic crystal slab structure is realized by stacking two uniformly scaled double-zero-index dielectric photonic crystal slabs together. The space cancellation effect in complementary photonic crystals is demonstrated in both numerical simulations and microwave experiments. The refractive index dispersion of double-zero-index dielectric photonic crystal is experimentally measured. Using pure dielectrics, our photonic crystal structure will be an ideal platform to explore various intriguing properties related to a complementary medium.

CORC: An Online Data Quality Tool For CUORE

NASA Astrophysics Data System (ADS)

Welliver, Bradford

2017-09-01

The Cryogenic Underground Observatory for Rare Events (CUORE) is a large neutrinoless double beta decay search experiment. Currently CUORE is actively taking data at the Laboratori Nazionali del Gran Sasso (LNGS). These searches can address fundamental questions about the nature of the neutrino and may provide insight into the observed matter-antimatter asymmetry in the universe leading to beyond standard model physics via lepton number violation. CUORE is the largest array of crystal bolometers in the world, containing a total of 988 TeO2 crystals with a mass of 742kg and is expected to achieve a sensitivity on the 130Te 0 νββ half-life of T1 / 2 = 9 × 1025 years (90% C.L.) after 5 years of operation. The large number of individual crystals in CUORE presents challenges for monitoring data quality and determination of time periods of detector behavior suitable for analysis. We will discuss the current state of the online run diagnostic system that allows for easy monitoring of all crystals, provides an overview of performance over time, and gives an ability to set flags for periods of bad detector behavior as well as set phone and email alarms on various cryostat parameters.

First- and second-order Raman scattering from MoTe2 single crystal

NASA Astrophysics Data System (ADS)

Caramazza, Simone; Collina, Arianna; Stellino, Elena; Ripanti, Francesca; Dore, Paolo; Postorino, Paolo

2018-02-01

We report on Raman experiments performed on a MoTe2 single crystal. The system belongs to the wide family of transition metal dichalcogenides which includes several of the most interesting two-dimensional materials for both basic and applied physics. Measurements were performed in the standard basal plane configuration, by placing the ab plane of the crystal perpendicular to the wave vector k i of the incident beam to explore the in-plane vibrational modes, and in the edge plane configuration with k i perpendicular to the crystal c axis, thus mainly exciting out-of-plane modes. For both configurations we performed a polarization-dependent study of the first-order Raman components and detailed computation of the corresponding selection rules. We were thus able to provide a complete assignment of the observed first-order Raman peaks, in agreement with previous literature results. A thorough analysis of the second-order Raman bands, as observed in both basal and edge plane configurations, provides new information and allows a precise assignment of these spectral structures. In particular, we have observed and assigned Raman active modes of the M point of the Brillouin zone previously predicted by ab initio calculations but never previously measured.

Delayed, disequilibrium degassing in rhyolite magma: Decompression experiments and implications for explosive volcanism

USGS Publications Warehouse

Mangan, M.; Sisson, T.

2000-01-01

Recent numerical models and analog shock tube experiments show that disequilibrium degassing during magma ascent may lead to violent vesiculation very near the surface. In this study a series of decompression experiments using crystal-free, rhyolite melt were conducted to examine the development of large supersaturations due to delayed, homogenous (spontaneous) bubble nucleation. Melts were saturated at 900??C and 200 MPa with either 5.2 wt% dissolved H2O, or with 4.2 wt% H2O and 640 ppm CO2, and isothermally decompressed at linear rates of either 0.003, 0.025, or 8.5 MPa/s to final pressures between 25 and 175 MPa. Additional isobaric saturation experiments (900??C, 200-25 MPa) using pure H2O or mixed H2O-CO2 fluids establish reference equilibrium solubility curves/values. Homogenous nucleation is triggered in both H2O-only and H2O-CO2 experiments once the supersaturation pressure (??Pss) reaches ?? 120-150 MPa and the melt contains ?? two times its equilibrium water contents. Bubble number density and nucleation rate depend on the supersaturation pressure, with values on the order of 102/cm3 and < 1/cm3/s for ??Pss~120 MPa; 106/cm3 and 103-105/cm3/s for ??Pss??~130-150 MPa; and 107/cm3 and 106/cm3/s for ??Pss??160-175 MPa. Nucleation rates are consistent with classical nucleation theory, and infer an activation energy for nucleation of 1.5 x 10-18 J/nucleus, a critical bubble radius of 2 x 10-9 m, and an effective surface tension for rhyolite at 5.2 wt% H2O and 900??C of 0.10-0.11 N/m. The long nucleation delay limits the time available for subsequent diffusion such that disequilibrium dissolved H2O and CO2 contents persist to the end of our runs. The disequilibrium degassing paths inferred from our experiments contrast markedly with the equilibrium or quasi-equilibrium paths found in other studies where bubble nucleation occurs heterogenously on crystals or other discontinuities in the melt at low ??Pss. Homogenous and heterogenous nucleation rates are comparable, however, as are bubble number densities, so that at a given decompression rate it appears that nucleation mechanism, rather than nucleation rate, determines degassing efficiency by fixing the pressure (depth) at which vesiculation commences and hence the time available for equilibration prior to eruption. Although real systems are probably never truly crystal-free, our results show that rhyolitic magmas containing up to 104 crystals/cm3, and perhaps as high as 106 crystals/cm3, are controlled by homogenous, rather than heterogenous, nucleation during ascent. ?? 2000 Elsevier Science B.V. All rights reserved.

Three-dimensional crystals of ribosomes and their subunits from eu- and archaebacteria.

PubMed

Glotz, C; Müssig, J; Gewitz, H S; Makowski, I; Arad, T; Yonath, A; Wittmann, H G

1987-11-01

Ordered three-dimensional crystals of 70S ribosomes as well as of 30S and 50S ribosomal subunits from various bacteria (E. coli, Bacillus stearothermophilus, Thermus thermophilus and Halobacterium marismortui) have been grown by vapour diffusion in hanging drops using mono- and polyalcohols. A new compact crystal form of 50S subunits has been obtained, and it is suitable for crystallographic studies at medium resolution. In addition, from one crystal form large crystals could be grown in X-ray capillaries. In all cases the crystals were obtained from functionally active ribosomal particles, and the particles from dissolved crystals retained their integrity and biological activity.

Formation Of Amplitude Grating In Real-Time Holographic Recording Medium BSO Crystal

NASA Astrophysics Data System (ADS)

Yuan, Yan; Wei-shu, Wu; Ying-li, Chen

1988-01-01

The intensity-dependent absorption was discovered through experiments in photorefractive crystal BSO. The nonlinear coupled-wave equation describing the dynamic mixed volume gratings was derived, in which self-diffraction and the intensity-dependent absorption was considered. The calculated results are in agreement with the experiment.

Improving Student Results in the Crystal Violet Chemical Kinetics Experiment

ERIC Educational Resources Information Center

Kazmierczak, Nathanael; Vander Griend, Douglas A.

2017-01-01

Despite widespread use in general chemistry laboratories, the crystal violet chemical kinetics experiment frequently suffers from erroneous student results. Student calculations for the reaction order in hydroxide often contain large asymmetric errors, pointing to the presence of systematic error. Through a combination of "in silico"…

Astronaut Jan Davis monitors Commercial Protein Crystal Growth experiment

NASA Image and Video Library

1994-02-03

STS060-21-031 (3-11 Feb 1994) --- Using a lap top computer, astronaut N. Jan Davis monitors systems for the Commercial Protein Crystal Growth (CPCG) experiment onboard the Space Shuttle Discovery. Davis joined four other NASA astronauts and a Russian cosmonaut for eight days in space aboard Discovery.

A FIRE-ACE/SHEBA Case Study of Mixed-Phase Arctic Boundary Layer Clouds: Entrainment Rate Limitations on Rapid Primary Ice Nucleation Processes

NASA Technical Reports Server (NTRS)

Fridlin, Ann; vanDiedenhoven, Bastiaan; Ackerman, Andrew S.; Avramov, Alexander; Mrowiec, Agnieszka; Morrison, Hugh; Zuidema, Paquita; Shupe, Matthew D.

2012-01-01

Observations of long-lived mixed-phase Arctic boundary layer clouds on 7 May 1998 during the First International Satellite Cloud Climatology Project (ISCCP) Regional Experiment (FIRE)Arctic Cloud Experiment (ACE)Surface Heat Budget of the Arctic Ocean (SHEBA) campaign provide a unique opportunity to test understanding of cloud ice formation. Under the microphysically simple conditions observed (apparently negligible ice aggregation, sublimation, and multiplication), the only expected source of new ice crystals is activation of heterogeneous ice nuclei (IN) and the only sink is sedimentation. Large-eddy simulations with size-resolved microphysics are initialized with IN number concentration N(sub IN) measured above cloud top, but details of IN activation behavior are unknown. If activated rapidly (in deposition, condensation, or immersion modes), as commonly assumed, IN are depleted from the well-mixed boundary layer within minutes. Quasi-equilibrium ice number concentration N(sub i) is then limited to a small fraction of overlying N(sub IN) that is determined by the cloud-top entrainment rate w(sub e) divided by the number-weighted ice fall speed at the surface v(sub f). Because w(sub c)< 1 cm/s and v(sub f)> 10 cm/s, N(sub i)/N(sub IN)<< 1. Such conditions may be common for this cloud type, which has implications for modeling IN diagnostically, interpreting measurements, and quantifying sensitivity to increasing N(sub IN) (when w(sub e)/v(sub f)< 1, entrainment rate limitations serve to buffer cloud system response). To reproduce observed ice crystal size distributions and cloud radar reflectivities with rapidly consumed IN in this case, the measured above-cloud N(sub IN) must be multiplied by approximately 30. However, results are sensitive to assumed ice crystal properties not constrained by measurements. In addition, simulations do not reproduce the pronounced mesoscale heterogeneity in radar reflectivity that is observed.

Effects of mutations on active site conformation and dynamics of RNA-dependent RNA polymerase from Coxsackievirus B3.

PubMed

Shen, Hujun; Deng, Mingsen; Zhang, Yachao

2017-10-01

Recent crystal structures of RNA-dependent RNA polymerase (3D pol ) from Coxsackievirus B3 (CVB3) revealed that a tyrosine mutation at Phe364 (F364Y) resulted in structures with open active site whereas a hydrophobic mutation at Phe364 (F364A) led to conformations with closed active site. Besides, the crystal structures showed that the F364W mutation had no preference between the open and closed active sites, similar to wild-type. In this paper, we present a molecular dynamics (MD) study on CVB3 3D pol in order to address some important questions raised by experiments. First, MD simulations of F364Y and F364A were carried out to explore how these mutations at Phe364 influence active site dynamics and conformations. Second, MD simulations of wild-type and mutants were performed to discover the connection between active site dynamics and polymerase function. MD simulations reveal that the effect of mutations on active site dynamics is associated with the interaction between the structural motifs A and D in CVB3 3D pol . Interestingly, we discover that the active site state is influenced by the formation of a hydrogen bond between backbone atoms of Ala231 (in motif A) and Ala358 (in motif D), which has never been revealed before. Copyright © 2017 Elsevier Inc. All rights reserved.

On the role of convective motion during dendrite growth: Experiments under variable gravity, revised

NASA Technical Reports Server (NTRS)

Hallett, J.; Cho, N.; Harrison, K.; Lord, A.; Wedum, E.; Purcell, R.; Saunders, C. P. R.

1987-01-01

Experiments show the effect of self induced convection on individual dendrite growth in uniformly supercooled samples and solidification of the resulting mush under conditions of high and low g. Convection is visualized by a Schlieren optical system or a Mach Zender interferometer. For ice crystals growing from the vapor in air, a slight reduction in linear growth rate occur under low g. For ice crystals growing from NaCl solution, dendrite tip velocities are unchanged, but subsequent mush solidification is enhanced through drainage channels under higher g. By contrast, sodium sulfate decahydrate dendrites growing from solution produce convective plumes which lead to higher tip growth rate only as the crystal growth direction approaches that of gravity. Convective plumes are laminar for small crystals under conditions of these experiments; the rise velocity of such plumes is greater than individual vortex rings under identical conditions. Convection effects are only present in solution under a critical supercooling less than about 5 C for sodium sulfate and 2 C for ice in NaCl since at higher supercooling the crystallization velocity, proportional to the square of the supercooling, exceeds the convective velocity, proportional to the square root of the supercooling. The role of convective velocity in bulk solidification is to give a large scale flow which under extreme cases may lead to extensive secondary crystal production, which alters the resulting crystal texture of the completely solidified melt.

Observable Protein Crystal Growth Apparatus

NASA Technical Reports Server (NTRS)

2001-01-01

This diagram shows a cross sectrion of the fluid volume of an individual cell in the Observable Protein Crystal Growth Apparatus (OPCGA) to be operated aboard the International Space Station (ISS). The principal investigator is Dr. Alex McPherson of the University of California, Irvine. Each individual cell comprises two sample chambers with a rotating center section that isolates the two from each other until the start of the experiment and after it is completed. The cells are made from optical-quality quartz glass to allow photography and interferometric observations. Each cell has a small light-emitting diode and lens to back-light the solution. In protein crystal growth experiments, a precipitating agent such as a salt solution is used to absorb and hold water but repel the protein molecules. This increases the concentration of protein until the molecules nucleate to form crystals. This cell is one of 96 that make up the experiment module portion of the OPCGA.

Classification of the crystallization behavior of amorphous active pharmaceutical ingredients in aqueous environments.

PubMed

Van Eerdenbrugh, Bernard; Raina, Shweta; Hsieh, Yi-Ling; Augustijns, Patrick; Taylor, Lynne S

2014-04-01

To classify the crystallization behavior of amorphous active pharmaceutical ingredients (API) exposed to aqueous environments. A set of approximately 50 chemically and physically diverse active pharmaceutical ingredients (APIs) was selected for this study. Two experimental setups were employed to characterize the crystallization behavior of the amorphous API in an aqueous environment. For the first approach, precipitation, as evidenced by the development of turbidity, was induced using the solvent shift method, by mixing concentrated API solutions in DMSO with an aqueous buffer in a capillary. Subsequently, crystallization was monitored in situ over time using synchrotron radiation (simultaneous SAXS/WAXS beamline 12-ID-B at the Advanced Photon Source, Argonne National Laboratories, Argonne, IL). In the second approach, amorphous films were prepared by melt quenching; after adding buffer, crystallization was monitored with time using polarized light microscopy. In general, the crystallization behavior of a given compound was similar irrespective of the experimental method employed. However, the crystallization behavior among different compounds varied significantly, ranging from immediate and complete crystallization to no observable crystallization over biorelevant time scales. Comparison of the observed behavior with previous studies of crystallization tendency in non-aqueous environments revealed that the crystallization tendency of individual APIs was somewhat similar regardless of the crystallization environment. API properties, rather than the method by which amorphous materials are generated, tend to dictate crystallization behavior in aqueous media.

Transient rheology of crystallizing andesitic magmas

NASA Astrophysics Data System (ADS)

de Biasi, L. J.; Chevrel, M. O.; Hanson, J. B.; Cimarelli, C.; Lavallée, Y.; Dingwell, D. B.

2012-04-01

The viscosity of magma strongly influences its rheological behaviour, which is a key determinant of magma transport processes and volcanic eruptions. Understanding the factors controlling the viscosity of magma is important to our assessment of hazards posed by active volcanoes. In nature, magmas span a very wide range in viscosity (10-1 to 1014 Pa s), depending on chemical composition (including volatile content), temperature, and importantly, crystal fraction, which further induces a complex strain rate dependence (i.e. non-Newtonian rheology). Here, we present results of transient viscosities of a crystallizing andesitic melt (57 wt.% SiO2) from Tungurahua volcano (Ecuador). We followed the experimental method developed by Vona et al. (2011) for the concentric cylinder apparatus, but optimized its implementation by leaving the spindle in situ before quenching the experimental products, to preserve the complete developed texture of the sample. The viscosity is investigated under super-liquidus (1400 ° C) and sub-liquidus temperatures (1162 and 1167 ° C). For each temperature increment, thermal equilibrium is achieved over a period of days while the spindle constantly stirs the magma. Simultaneous monitoring of the torque is used to calculate the apparent viscosity of the transient suspension. To get a better understanding of the nucleation and crystal growth processes that are involved at sub-liquidus conditions, further time-step experiments were carried out, where the samples were quenched at various equilibration stages. The mineralogical assemblage, as well as the crystal fraction, distribution and preferential alignment were then quantitatively analyzed. At temperatures below the liquidus, the suspension shows a progressive, but irregular increase of the relative shear viscosity. First, the viscosity slightly increases, possibly due to the crystallization of small, equant oxides and the formation of plagioclase nuclei. After some time (1.5-2.5 days), crystallization of large, tabular plagioclase begins, inducing a significantly stronger increase in apparent viscosity until thermo-chemical equilibration is achieved. After continued stirring the apparent viscosity slightly decreases, likely due to increasing crystal alignment. The analysis of pre-equilibrium quenched samples indicates that crystals nucleate and grow preferentially in proximity to both the spindle and the crucible wall. Furthermore, decreasing the stirring rate (aka strain rate) results in an increase in the apparent viscosity, which evidences the non-Newtonian characteristics of the magmatic suspension. In conclusion, these experiments indicate that natural andesitic magmas undergo significant rheological changes at the onset of crystallization. The observed thermo-chemical variations elucidate a transient viscosity, which deserves consideration into all problems of magma transport. Reference: Vona, A., Romano, C., Dingwell, D.B., Giordano, D. 2011. The rheology of crystal-bearing basaltic magmas from Stromboli and Etna. Geochim. Cosmochim. Acta, 75, 3214-3236.

Third harmonic frequency generation by type-I critically phase-matched LiB3O5 crystal by means of optically active quartz crystal.

PubMed

Gapontsev, Valentin P; Tyrtyshnyy, Valentin A; Vershinin, Oleg I; Davydov, Boris L; Oulianov, Dmitri A

2013-02-11

We present a method of third harmonic generation at 355 nm by frequency mixing of fundamental and second harmonic radiation of an ytterbium nanosecond pulsed all-fiber laser in a type-I phase-matched LiB(3)O(5) (LBO) crystal where originally orthogonal polarization planes of the fundamental and second harmonic beams are aligned by an optically active quartz crystal. 8 W of ultraviolet light at 355 nm were achieved with 40% conversion efficiency from 1064 nm radiation. The conversion efficiency obtained in a type-I phase-matched LBO THG crystal was 1.6 times higher than the one achieved in a type-II LBO crystal at similar experimental conditions. In comparison to half-wave plates traditionally used for polarization alignment the optically active quartz crystal has much lower temperature dependence and requires simpler optical alignment.

The Effects of Gravity on the Crystallization Behavior of Heavy Metal Fluoride Glasses

NASA Technical Reports Server (NTRS)

Tucker, Dennis S.; Smith, Guy A.

2004-01-01

Heavy metal fluoride glasses are used in such applications as fiber lasers and laser amplifiers. ZrF4-BaF2-LaF3-AlF3-NaF (ZBLAN) is one of the more commonly used heavy metal fluoride glasses. ZBLAN is an infrared transmitter and has a theoretical attenuation coefficient of 0.002 db/km. However, due to impurities and small crystallites this attenuation coefficient has not been achieved to date. ZBLAN is a fragile glass which can lead to rapid crystallization, if the glass is not cooled rapidly to below the glass transition temperature or if the glass is reheated near the crystallization temperature for any period of time. Studies carried on at Marshall Space Flight Center and the University of Alabama in Huntsville since 1993 have shown that heating ZBLAN glass at the crystallization temperature in reduced gravity results in a suppression of crystallization when compared to ZBLAN processed in unit gravity. These studies utilized NASA's KC-135 aircraft and the Conquest sounding rocket. In the first series of experiments, short lengths of ZBLAN fiber were heated to the crystallization temperature in reduced gravity on board the KC- 135 and the Conquest sounding rocket and compared with fibers heated in unit gravity. The fibers processed in reduced gravity showed no evidence of crystallization when studied with x-ray diffraction and scanning electron microscopy. However, the fibers processed in unit gravity were completely crystallized. Subsequent experiments included heating small pieces of ZBLAN glass at the crystallization temperature while viewing with a video camera to follow the crystallization phenomenon. In this experiment crystallization was observed in reduced gravity, however, it was suppressed when compared to heating in unit gravity. In the most recent experiment on board the KC-135, rapid thermal analysis of ZBLAN was performed. A mechanism to explain the observations has been proposed. This mechanism is based on shear thinning whereby, the glass undergoes a reduction in viscosity in the 10(exp 5) - 10(exp 7) poise range, allowing more rapid diffusion and thus crystallization. It is proposed that this mechanism is suppressed in reduced gravity. An experiment is presently being conducted to test this theory. With increased knowledge of ZBLAN behavior in reduced gravity, three low earth orbit tiber drawing facilities have been designed. One would be suitable for use on the International Space Station, another while aboard the Space Shuttle and the third system is a fully automated facility which would operate independently of the ISS or Shuttle in a free float mode. The primary benefits of free floating a facility in LEO includes a higher quality of microgravity and reduced safety concerns since it is not in a manned environment.

A discrete dislocation dynamics model of creeping single crystals

NASA Astrophysics Data System (ADS)

Rajaguru, M.; Keralavarma, S. M.

2018-04-01

Failure by creep is a design limiting issue for metallic materials used in several high temperature applications. Current theoretical models of creep are phenomenological with little connection to the underlying microscopic mechanisms. In this paper, a bottom-up simulation framework based on the discrete dislocation dynamics method is presented for dislocation creep aided by the diffusion of vacancies, known to be the rate controlling mechanism at high temperature and stress levels. The time evolution of the creep strain and the dislocation microstructure in a periodic unit cell of a nominally infinite single crystal is simulated using the kinetic Monte Carlo method, together with approximate constitutive laws formulated for the rates of thermal activation of dislocations over local pinning obstacles. The deformation of the crystal due to dislocation glide between individual thermal activation events is simulated using a standard dislocation dynamics algorithm, extended to account for constant stress periodic boundary conditions. Steady state creep conditions are obtained in the simulations with the predicted creep rates as a function of stress and temperature in good agreement with experimentally reported values. Arrhenius scaling of the creep rates as a function of temperature and power-law scaling with the applied stress are also reproduced, with the values of the power-law exponents in the high stress regime in good agreement with experiments.

Synchronized cell attachment triggered by photo-activatable adhesive ligands allows QCM-based detection of early integrin binding

PubMed Central

Iturri, Jagoba; García-Fernández, Luis; Reuning, Ute; García, Andrés J.; Campo, Aránzazu del; Salierno, Marcelo J.

2015-01-01

The Quartz Crystal Microbalance with dissipation (QCM-D) technique was applied to monitor and quantify integrin-RGD recognition during the early stages of cell adhesion. Using QCM-D crystals modified with a photo-activatable RGD peptide, the time point of presentation of adhesive ligand at the surface of the QCM-D crystal could be accurately controlled. This allowed temporal resolution of early integrin-RGD binding and the subsequent cell spreading process, and their separate detection by QCM-D. The specificity of the integrin-RGD binding event was corroborated by performing the experiments in the presence of soluble cyclicRGD as a competitor, and cytochalasin D as inhibitor of cell spreading. Larger frequency change in the QCM-D signal was observed for cells with larger spread area, and for cells overexpressing integrin αvβ3 upon stable transfection. This strategy enables quantification of integrin activity which, in turn, may allow discrimination among different cell types displaying distinct integrin subtypes and expression levels thereof. On the basis of these findings, we believe the strategy can be extended to other photoactivatable ligands to characterize cell membrane receptors activity, a relevant issue for cancer diagnosis (and prognosis) as other several pathologies. PMID:25825012

Effect of pH on the morphology of kidney stones

NASA Astrophysics Data System (ADS)

Agarwal, Neelesh; Sova, Stacey; Singh, N. B.; Arnold, Brad; Choa, Fow-Sen; Cullum, Brian; Su, Ching-Hua

2016-05-01

The process for the formation of kidney stone is very complex phenomena and has some similarity to the crystal growth from a solution. It is very much dependent on the acidity pH of the fluids. This pH variation affects the content and amount of filtering residue and its morphology. In this study we have performed experiments using carbonate, oxides and urea to simulate and understand the morphologies of the residue filtered and coarsened in different conditions. We observed that different of morphologies of kidney stones can be explained on the basis of acidity and hydration conditions. At lower pH fat prism crystals are observed and as pH increases, long fat needle crystals with large aspect ratio are observed. The coarsening experiments showed further growth of crystals. The remelting experiments showed that during dissolution of kidney stones the joining material breaks first leaving the large faceted crystals undissolved when attempts are made to dissolve into small crystallites. However, the morphology did not change. It was also observed that impurities such as magnesium oxide (MgO) affect the morphology significantly.

Modeling ultrasonic compression wave absorption during the seeded crystallization of copper (II) sulphate pentahydrate from aqueous solution.

PubMed

Marshall, Thomas; Challis, Richard E; Holmes, Andrew K; Tebbutt, John S

2002-11-01

Ultrasonic compression wave absorption is investigated as a means to monitor the seeded crystallization of copper (II) sulphate pentahydrate from aqueous solution. Simple models are applied to predict crystal yield, crystal size distribution, and the changing nature of the continuous phase. The Allegra-Hawley scattering formulation is used to simulate ultrasonic absorption as crystallization proceeds. Experiments confirm that simulated attenuation is in agreement with measured results.

Carbocation/Polyol Systems as Efficient Organic Catalysts for the Preparation of Cyclic Carbonates.

PubMed

Rulev, Yuri A; Gugkaeva, Zalina T; Lokutova, Anastasia V; Maleev, Victor I; Peregudov, Alexander S; Wu, Xiao; North, Michael; Belokon, Yuri N

2017-03-22

Carbocation/polyol systems are shown to be highly efficient catalysts for the synthesis of cyclic carbonates from epoxides and carbon dioxide at 50 °C and 5 MPa CO 2 pressure. The best activity was shown by the combination of crystal violet and 1,1'-bi-2-naphthol (BINOL), which could be recycled five times with no loss of activity. The presence of specific interactions between the amino groups of the carbocation and the hydroxyl protons was confirmed by NMR experiments. The Job plots for the crystal violet iodide/BINOL and brilliant green iodide/BINOL systems showed that the catalytic systems consist of one molecule of the carbocation and one molecule of BINOL. Mechanistic studies using a deuterated epoxide indicate that there was some loss of epoxide stereochemistry during the reaction, but predominant retention of stereochemistry is observed. On this basis, a catalytic cycle is proposed. © 2017 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim.

Lattice dynamics of A Sb2O6 (A =Cu , Co) with trirutile structure

NASA Astrophysics Data System (ADS)

Maimone, D. T.; Christian, A. B.; Neumeier, J. J.; Granado, E.

2018-03-01

Raman spectroscopy experiments on single crystals of CuSb2O6 and CoSb2O6 quasi-one-dimensional antiferromagnets with trirutile crystal structure were performed, with a focus on the first material. The observed Raman-active phonon modes and previously reported infrared-active modes were identified with the aid of ab initio lattice dynamics calculations. The structural transition between monoclinic β -CuSb2O6 and tetragonal α -CuSb2O6 phases at Ts=400 K is manifested in our spectra by a "repulsion" of two accidentally quasidegenerate symmetric modes below Ts, caused by a phonon mixing effect that is only operative in the monoclinic β -CuSb2O6 phase due to symmetry restrictions. Also, two specific phonons, associated with CuO6 octahedra rotation and with a Jahn-Teller elongation mode, soften and broaden appreciably as T →Ts . A crossover from a displacive to an order-disorder transition at Ts is inferred.

The International Microgravity Laboratory, a Spacelab for materials and life sciences

NASA Technical Reports Server (NTRS)

Snyder, Robert S.

1992-01-01

The material science experiments performed on the International Microgravity Laboratory (IML-1), which is used to perform investigations which require the low gravity environment of space, are discussed. These experiments, the principal investigator, and associated organization are listed. Whether the experiment was a new development or was carried on an earlier space mission, such as the third Spacelab (SL-3) or the Shuttle Middeck, is also noted. The two major disciplines of materials science represented on IML-1 were the growth of crystals from the melt, solution, or vapor and the study of fluids (liquids and gases) in a reduced gravity environment. The various facilities on board IML-1 and their related experiments are described. The facilities include the Fluids Experiment System (FES) Vapor Crystal Growth System (VCGS) Organic Crystal Growth Facility (OCGF), Cryostat (CRY), and the Critical Point Facility (CPF).

Evidence for an early wet Moon from experimental crystallization of the lunar magma ocean

NASA Astrophysics Data System (ADS)

Lin, Yanhao; Tronche, Elodie J.; Steenstra, Edgar S.; van Westrenen, Wim

2017-01-01

The Moon is thought to have been covered initially by a deep magma ocean, its gradual solidification leading to the formation of the plagioclase-rich highland crust. We performed a high-pressure, high-temperature experimental study of lunar mineralogical and geochemical evolution during magma ocean solidification that yields constraints on the presence of water in the earliest lunar interior. In the experiments, a deep layer containing both olivine and pyroxene is formed in the first ~50% of crystallization, β-quartz forms towards the end of crystallization, and the last per cent of magma remaining is extremely iron rich. In dry experiments, plagioclase appears after 68 vol.% solidification and yields a floatation crust with a thickness of ~68 km, far above the observed average of 34-43 km based on lunar gravity. The volume of plagioclase formed during crystallization is significantly less in water-bearing experiments. Using the relationship between magma water content and the resulting crustal thickness in the experiments, and considering uncertainties in initial lunar magma ocean depth, we estimate that the Moon may have contained at least 270 to 1,650 ppm water at the time of magma ocean crystallization, suggesting the Earth-Moon system was water-rich from the start.

Shock Hugoniot of single crystal copper

NASA Astrophysics Data System (ADS)

Chau, R.; Stölken, J.; Asoka-Kumar, P.; Kumar, M.; Holmes, N. C.

2010-01-01

The shock Hugoniot of single crystal copper is reported for stresses below 66 GPa. Symmetric impact experiments were used to measure the Hugoniots of three different crystal orientations of copper, [100], [110], and [111]. The photonic doppler velocimetry (PDV) diagnostic was adapted into a very high precision time of arrival detector for these experiments. The measured Hugoniots along all three crystal directions were nearly identical to the experimental Hugoniot for polycrystalline Cu. The predicted orientation dependence of the Hugoniot from molecular dynamics calculations was not observed. At the lowest stresses, the sound speed in Cu was extracted from the PDV data. The measured sound speeds are in agreement with values calculated from the elastic constants for Cu.

Solubility and crystal nucleation in organic solvents of two polymorphs of curcumin.

PubMed

Liu, Jin; Svärd, Michael; Hippen, Perschia; Rasmuson, Åke C

2015-07-01

Two crystal polymorphs of 1,7-bis-(4-hydroxy-3-methoxyphenyl)-1,6-heptadiene-3,5-dione (curcumin) have been obtained by crystallization from ethanol (EtOH) solution. The polymorphs have been characterized by differential scanning calorimetry, infrared spectroscopy, and X-ray powder diffraction and shown to be the previously described forms I and III. The solubility of both polymorphs in EtOH and of one polymorph in ethyl acetate (EA) has been measured between 10°C and 50°C with a gravimetric method. Primary nucleation of curcumin from EtOH solution has been investigated in 520 constant temperature crystallization experiments in sealed, magnetically stirred vials under different conditions of supersaturation, temperature, and agitation rate. By a thermodynamic analysis of the melting data and solubility of form I, the solid-state activity is estimated from 10°C up to the melting point. The solubility is lower in EtOH than in EA, and in both solvents, a positive deviation from Raoult's law is observed. Form I has lower solubility than form III and is accordingly thermodynamically more stable over the investigated temperature interval. Extrapolation of solubility regression models indicates that there should be a low-temperature enantiotropic transition point, below which form I will be metastable. By slurry conversion experiments, it is established that this temperature is below -30°C. All nucleation experiments resulted in the stable form I. The induction time is observed to decrease with increasing agitation rate up to a certain point, and then increase with further increasing agitation rate; a trend previously observed for other compounds. By correlating the induction time data obtained at different supersaturation and temperature, the interfacial energy of form I in EtOH is estimated to be 3.0 mJ/m(2) . © 2015 Wiley Periodicals, Inc. and the American Pharmacists Association.

Drug crystallization - implications for topical and transdermal delivery.

PubMed

Hadgraft, Jonathan; Lane, Majella E

2016-06-01

Crystallization of actives in skin following topical application was suggested by studies in the 1950s and 1960s but is poorly understood. In contrast, the problem of crystallization of actives on skin and in transdermal formulations has been known for many years. With respect to crystallization in skin, this review describes early reports of a skin 'reservoir' and possible reasons underlying its genesis. Techniques to study crystallization on and in skin and in transdermal patches are outlined. The role of the vehicle in skin delivery is emphasised. Studies which have investigated permeation from crystalline particles are described. Approaches to limit crystallization of actives are discussed. Using supersaturation and antinuclean polymers, control of crystal size is possible; controlled release from crystals is also employed in transdermal patches. Drug crystallization has significant implications for topical and transdermal delivery. Approaches have been developed to counteract the issue for transdermal patches but crystallization in and on the skin for other formulations remains unresolved. Greater knowledge of residence time of excipients and their interaction with skin at the molecular level is critical in order to address the problem. This will lay the foundations for better design of topical/transdermal formulations.

Determining heterogeneous slip activity on multiple slip systems from single crystal orientation pole figures

DOE PAGES

Pagan, Darren C.; Miller, Matthew P.

2016-09-01

A new experimental method to determine heterogeneity of shear strains associated with crystallographic slip in the bulk of ductile, crystalline materials is outlined. The method quantifies the time resolved evolution of misorientation within plastically deforming crystals using single crystal orientation pole figures (SCPFs) measured in-situ with X-ray diffraction. A multiplicative decomposition of the crystal kinematics is used to interpret the distributions of lattice plane orientation observed on the SCPFs in terms of heterogeneous slip activity (shear strains) on multiple slip systems. Here, to show the method’s utility, the evolution of heterogeneous slip is quantified in a silicon single crystal plasticallymore » deformed at high temperature at multiple load steps, with slip activity in sub-volumes of the crystal analyzed simultaneously.« less

Microgravity

NASA Image and Video Library

1996-01-25

Dan Carter and Charles Sisk center a Lysozyme Protein crystal grown aboard the USML-2 shuttle mission. Protein isolated from hen egg-white and functions as a bacteriostatic enzyme by degrading bacterial cell walls. First enzyme ever characterized by protein crystallography. It is used as an excellent model system for better understanding parameters involved in microgravity crystal growth experiments. The goal is to compare kinetic data from microgravity experiments with data from laboratory experiments to study the equilibrium.

Enhancing the blue shift of SHG signal in GaSe:B/Ce crystal

NASA Astrophysics Data System (ADS)

Karatay, Ahmet; Yuksek, Mustafa; Ertap, Hüseyin; Elmali, Ayhan; Karabulut, Mevlut

2018-02-01

The influence of Ce3+ on the wavelength of second harmonic generation (SHG) signal in boron doped GaSe crystals have been investigated. We found that by substitution of Ce3+ with B3+, SHG signal shifted to lower wavelength. In addition, the nonlinear absorption (NA) properties and ultrafast dynamics of pure, 1 at.% B3+ and 0.5 at.% B3++ 0.5 at.% Ce3+ doped GaSe crystals have been studied by open aperture Z-scan and ultrafast pump probe spectroscopy techniques. From the open aperture Z-scan experiments we observed that all of the crystals showed nonlinear absorption (NA). However, pump-probe experiments revealed that when GaSe crystal is doped, the NA signal turns into a bleaching signal with different lifetimes depending on the type and concentration of the dopant atoms.

Large-area sheet task advanced dendritic web growth development

NASA Technical Reports Server (NTRS)

Duncan, C. S.; Seidensticker, R. G.; Mchugh, J. P.; Hopkins, R. H.; Meier, D. L.; Schruben, J.

1982-01-01

Thermal models were developed that accurately predict the thermally generated stresses in the web crystal which, if too high, cause the crystal to degenerate. The application of the modeling results to the design of low-stress experimental growth configurations will allow the growth of wider web crystals at higher growth velocities. A new experimental web growth machine was constructed. This facility includes all the features necessary for carrying out growth experiments under steady thermal conditions. Programmed growth initiation was developed to give reproducible crystal starts. Width control permits the growth of long ribbons at constant width. Melt level is controlled to 0.1 mm or better. Thus, the capability exists to grow long web crystals of constant width and thickness with little operator intervention, and web growth experiments can now be performed with growth variables controlled to a degree not previously possible.

A Novel N-Acetylglutamate Synthase Architecture Revealed by the Crystal Structure of the Bifunctional Enzyme from Maricaulis maris

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shi, Dashuang; Li, Yongdong; Cabrera-Luque, Juan

2012-05-24

Novel bifunctional N-acetylglutamate synthase/kinases (NAGS/K) that catalyze the first two steps of arginine biosynthesis and are homologous to vertebrate N-acetylglutamate synthase (NAGS), an essential cofactor-producing enzyme in the urea cycle, were identified in Maricaulis maris and several other bacteria. Arginine is an allosteric inhibitor of NAGS but not NAGK activity. The crystal structure of M. maris NAGS/K (mmNAGS/K) at 2.7 {angstrom} resolution indicates that it is a tetramer, in contrast to the hexameric structure of Neisseria gonorrhoeae NAGS. The quaternary structure of crystalline NAGS/K from Xanthomonas campestris (xcNAGS/K) is similar, and cross-linking experiments indicate that both mmNAGS/K and xcNAGS aremore » tetramers in solution. Each subunit has an amino acid kinase (AAK) domain, which is likely responsible for N-acetylglutamate kinase (NAGK) activity and has a putative arginine binding site, and an N-acetyltransferase (NAT) domain that contains the putative NAGS active site. These structures and sequence comparisons suggest that the linker residue 291 may determine whether arginine acts as an allosteric inhibitor or activator in homologous enzymes in microorganisms and vertebrates. In addition, the angle of rotation between AAK and NAT domains varies among crystal forms and subunits within the tetramer. A rotation of 26{sup o} is sufficient to close the predicted AcCoA binding site, thus reducing enzymatic activity. Since mmNAGS/K has the highest degree of sequence homology to vertebrate NAGS of NAGS and NAGK enzymes whose structures have been determined, the mmNAGS/K structure was used to develop a structural model of human NAGS that is fully consistent with the functional effects of the 14 missense mutations that were identified in NAGS-deficient patients.« less

Visible-light-driven photocatalytic activation of peroxymonosulfate by Cu2(OH)PO4 for effective decontamination.

PubMed

Liu, Guoshuai; Zhou, Yanan; Teng, Jie; Zhang, Jinna; You, Shijie

2018-06-01

The advanced oxidation process (AOP) based on SO 4 - radicals draws an increasing interest in water and wastewater treatment. Producing SO 4 - radicals from the activation of peroxymonosulfate (PMS) by transition metal ions or oxides may be problematic due to high operational cost and potential secondary pollution caused by metal leaching. To address this challenge, the present study reports the efficient production of SO 4 - radicals through visible-light-driven photocatalytic activation (VL-PCA) of PMS by using Cu 2 (OH)PO 4 single crystal for enhanced degradation of a typical recalcitrant organic pollutant, i.e., 2,4-dichlorophenol (2,4-DCP). It took only 7 min to achieve almost 100% removal of 2,4-DCP in the Cu 2 (OH)PO 4 /PMS system under visible-light irradiation and pH-neutral condition. The 2,4-DCP degradation was positively correlated to the amount of Cu 2 (OH)PO 4 and PMS. Both OH and SO 4 - radicals were responsible for enhanced degradation performance, indicated by radical scavenger experiments and electron spin resonance (ESR) measurements. The Cu 2 (OH)PO 4 single crystal exhibited good cyclic stability and negligible metal leaching. According to density functional theory (DFT) calculations, the visible-light-driven transformation of two copper states between trigonal bipyramidal sites and octahedral sites in the crystal structure of Cu 2 (OH)PO 4 facilitates the generation of OH and SO 4 - radicals from the activation of PMS and cleavage of O-O bonds. This study provides the proof-in-concept demonstration of activation of PMS driven by visible light, making the SO 4 - radicals-based AOPs much easier, more economical and more sustainable in engineering applications for water and wastewater treatment. Copyright © 2018 Elsevier Ltd. All rights reserved.

Finite-size Scaling of the Density of States in Photonic Band Gap Crystals

NASA Astrophysics Data System (ADS)

Hasan, Shakeeb Bin; Mosk, Allard P.; Vos, Willem L.; Lagendijk, Ad

2018-06-01

The famous vanishing of the density of states (DOS) in a band gap, be it photonic or electronic, pertains to the infinite-crystal limit. In contrast, all experiments and device applications refer to finite crystals, which raises the question: Upon increasing the linear size L of a crystal, how fast does the DOS approach the infinite-crystal limit? We present a theory for finite crystals that includes Bloch-mode broadening due to the presence of crystal boundaries. Our results demonstrate that the DOS for frequencies inside a band gap has a 1 /L scale dependence for crystals in one, two and three dimensions.

Summary Report of mission acceleration measurements for STS-66. Launched November 3, 1994

NASA Technical Reports Server (NTRS)

Rogers, Melissa J. B.; Delombard, Richard

1995-01-01

Experiments flown in the middeck of Atlantis during the STS-66 mission were supported by the Space Acceleration Measurement System (SAMS). In particular, the three triaxial SAMS sensor heads collected data in support of protein crystal growth experiments. Data collected during STS-66 are reviewed in this report. The STS-66 SAMS data represent the microgravity environment in the 0.01 Hz to 10 Hz range. Variations in the environment related to differing levels of crew activity are discussed in the report. A comparison is made among times when the crew was quiet during a public affairs conference, working quietly, and exercising. These levels of activity are also compared to levels recorded by a SAMS unit in the Spacelab on Columbia during the STS-65 mission.

Shape Evolution of Detached Bridgman Crystals Grown in Microgravity

NASA Technical Reports Server (NTRS)

Volz, M. P.; Mazuruk, K.

2015-01-01

A theory describing the shape evolution of detached Bridgman crystals in microgravity has been developed. A starting crystal of initial radius r0 will evolve to one of the following states: Stable detached gap; Attachment to the crucible wall; Meniscus collapse. Only crystals where alpha plus omega is great than 180 degrees will achieve stable detached growth in microgravity. Results of the crystal shape evolution theory are consistent with predictions of the dynamic stability of crystallization (Tatarchenko, Shaped Crystal Growth, Kluwer, 1993). Tests of transient crystal evolution are planned for ICESAGE, a series of Ge and GeSi crystal growth experiments planned to be conducted on the International Space Station (ISS).

Macromolecular Crystallization in Microgravity

NASA Technical Reports Server (NTRS)

Snell, Edward H.; Helliwell, John R.

2004-01-01

The key concepts that attracted crystal growers, macromolecular or solid state, to microgravity research is that density difference fluid flows and sedimentation of the growing crystals are greatly reduced. Thus, defects and flaws in the crystals can be reduced, even eliminated, and crystal volume can be increased. Macromolecular crystallography differs from the field of crystalline semiconductors. For the latter, crystals are harnessed for their electrical behaviors. A crystal of a biological macromolecule is used instead for diffraction experiments (X-ray or neutron) to determine the three-dimensional structure of the macromolecule. The better the internal order of the crystal of a biological macromolecule then the more molecular structure detail that can be extracted. This structural information that enables an understanding of how the molecule functions. This knowledge is changing the biological and chemical sciences with major potential in understanding disease pathologies. Macromolecular structural crystallography in general is a remarkable field where physics, biology, chemistry, and mathematics meet to enable insight to the basic fundamentals of life. In this review, we examine the use of microgravity as an environment to grow macromolecular crystals. We describe the crystallization procedures used on the ground, how the resulting crystals are studied and the knowledge obtained from those crystals. We address the features desired in an ordered crystal and the techniques used to evaluate those features in detail. We then introduce the microgravity environment, the techniques to access that environment, and the theory and evidence behind the use of microgravity for crystallization experiments. We describe how ground-based laboratory techniques have been adapted to microgravity flights and look at some of the methods used to analyze the resulting data. Several case studies illustrate the physical crystal quality improvements and the macromolecular structural advances. Finally, limitations and alternatives to microgravity and future directions for this research are covered.

Identification and Control of Gravity Related Defect Formation During Melt Growth of Electro-Optic Single Crystals Bismuth Silicate(Bi12SiO20)

NASA Technical Reports Server (NTRS)

Becia, Piotr; Wiegel, Michaela E. K.

2004-01-01

A research carried out under Award Number NAG8-1487 was aimed at to the design, conduct and analysis of experiments directed at the identification and control of gravitational effects on crystal growth, segregation and defect formation in the Sillenite system: bismuth silicate (Bi(12)SiO(20)). Correlation analyses was conducted in order to establish the influence of gravity related defects introduced during crystal growth on critical, application specific properties. Achievement of the states objective was conducted during the period from Feb. 01, 1998 to Dec. 31, 2003 with the following anticipated milestones: 1. Establishment of capabilities for (a) reproducible Czochralski and Bridgman-type growth of BSO single crystals and (b) for comprehensive analysis of crystalline and chemical defects as well as for selective property characterization of grown crystals (year 1). 2. Design and execution of critical space growth experiment(s) based on analyses of prefatory space results (experiments aimed at establishing the viability of planned approaches and procedures) and on unresolved issues related to growth, segregation and defect formation associated with conventional growth in Bridgman geometries. Comparative analysis of growth under conventional and under mu-g conditions; identification of gravity related defect formation during conventional Bridgman growth and formulation of approaches for their control (years 2 and 3). Development of charge confinement system which permits growth interface demarcation (in a mu-g environment) as well as minimization of confinement related stress and contamination during growth; design of complementary mu-g growth experiments aimed at quantitative mu-g growth and segregation analyses (year 4). 3. Conduct of quantitative mu-g growth experiments directed at: (a) identification and control of gravity related crystalline and chemical defect formation during single crystal growth of Bi(12)SiO(20) and at (b) defect engineering -the development of approaches to the controlled generation during crystal growth of specified point defects in homogeneous distribution (year 5). The proposed research places focus on a class of materials which have outstanding electrical and optical properties but have so far failed to reach their potential, primarily because of our inability to control adequately their stoichiometry and crystal defect formation as well as confinement related contamination and lattice stress.

On the Coupling Mechanism of Equiaxed Crystal Generation with the Liquid Flow Driven by Natural Convection During Solidification

NASA Astrophysics Data System (ADS)

Stefan-Kharicha, Mihaela; Kharicha, Abdellah; Wu, Menghuai; Ludwig, Andreas

2018-02-01

The influence of the melt flow on the solidification structure is bilateral. The flow plays an important role in the solidification pattern, via the heat transfer, grain distribution, and segregations. On the other hand, the crystal structure, columnar or equiaxed, impacts the flow, via the thermosolutal convection, the drag force applied by the crystals on the melt flow, etc. As the aim of this research was to further explore the solidification-flow interaction, experiments were conducted in a cast cell (95 * 95 * 30 mm3), in which an ammonium chloride-water solution (between 27 and 31 wt pct NH4Cl) was observed as it solidified. The kinetic energy (KE) of the flow and the average flow velocity were calculated throughout the process. Measurements of the volume extension of the mush in the cell and the velocity of the solid front were also taken during the solidification experiment. During the mainly columnar experiments (8 cm liquid height) the flow KE continuously decreased over time. However, during the later series of experiments at higher liquid height (9.5 cm), the flow KE evolution presented a strong peak shortly after the start of solidification. This increase in the total flow KE correlated with the presence of falling equiaxed crystals. Generally, a clear correlation between the strength of the flow and the occurrence of equiaxed crystals was evident. The analysis of the results strongly suggests a fragmentation origin of equiaxed crystals appearing in the melt. The transition from purely columnar growth to a strongly equiaxed rain (CET) was found to be triggered by (a) the magnitude of the coupling between the flow intensity driven by the equiaxed crystals, and (b) the release and transport of the fragments by the same flow recirculating within the mushy zone.

The Stanford Automated Mounter: Enabling High-Throughput Protein Crystal Screening at SSRL

DOE Office of Scientific and Technical Information (OSTI.GOV)

Smith, C.A.; Cohen, A.E.

2009-05-26

The macromolecular crystallography experiment lends itself perfectly to high-throughput technologies. The initial steps including the expression, purification, and crystallization of protein crystals, along with some of the later steps involving data processing and structure determination have all been automated to the point where some of the last remaining bottlenecks in the process have been crystal mounting, crystal screening, and data collection. At the Stanford Synchrotron Radiation Laboratory, a National User Facility that provides extremely brilliant X-ray photon beams for use in materials science, environmental science, and structural biology research, the incorporation of advanced robotics has enabled crystals to be screenedmore » in a true high-throughput fashion, thus dramatically accelerating the final steps. Up to 288 frozen crystals can be mounted by the beamline robot (the Stanford Auto-Mounting System) and screened for diffraction quality in a matter of hours without intervention. The best quality crystals can then be remounted for the collection of complete X-ray diffraction data sets. Furthermore, the entire screening and data collection experiment can be controlled from the experimenter's home laboratory by means of advanced software tools that enable network-based control of the highly automated beamlines.« less

Methods for Neutron Spectrometry

DOE R&D Accomplishments Database

Brockhouse, Bertram N.

1961-01-09

The appropriate theories and the general philosophy of methods of measurement and treatment of data neutron spectrometry are discussed. Methods of analysis of results for liquids using the Van Hove formulation, and for crystals using the Born-von Karman theory, are reviewed. The most useful of the available methods of measurement are considered to be the crystal spectrometer methods and the pulsed monoenergetic beam/time-of-flight method. Pulsed-beam spectrometers have the advantage of higher counting rates than crystal spectrometers, especially in view of the fact that simultaneous measurements in several counters at different angles of scattering are possible in pulsed-beam spectrometers. The crystal spectrometer permits several valuable new types of specialized experiments to be performed, especially energy distribution measurements at constant momentum transfer. The Chalk River triple-axis crystal-spectrometer is discussed, with reference to its use in making the specialized experiments. The Chalk River rotating crystal (pulsed-beam) spectrometer is described, and a comparison of this type instrument with other pulsed-beam spectrometers is made. A partial outline of the theory of operation of rotating-crystal spectrometers is presented. The use of quartz-crystal filters for fast neutron elimination and for order elimination is discussed. (auth)

Nanoscale-driven crystal growth of hexaferrite heterostructures for magnetoelectric tuning of microwave semiconductor integrated devices.

PubMed

Hu, Bolin; Chen, Zhaohui; Su, Zhijuan; Wang, Xian; Daigle, Andrew; Andalib, Parisa; Wolf, Jason; McHenry, Michael E; Chen, Yajie; Harris, Vincent G

2014-11-25

A nanoscale-driven crystal growth of magnetic hexaferrites was successfully demonstrated at low growth temperatures (25-40% lower than the temperatures required often for crystal growth). This outcome exhibits thermodynamic processes of crystal growth, allowing ease in fabrication of advanced multifunctional materials. Most importantly, the crystal growth technique is considered theoretically and experimentally to be universal and suitable for the growth of a wide range of diverse crystals. In the present experiment, the conical spin structure of Co2Y ferrite crystals was found to give rise to an intrinsic magnetoelectric effect. Our experiment reveals a remarkable increase in the conical phase transition temperature by ∼150 K for Co2Y ferrite, compared to 5-10 K of Zn2Y ferrites recently reported. The high quality Co2Y ferrite crystals, having low microwave loss and magnetoelectricity, were successfully grown on a wide bandgap semiconductor GaN. The demonstration of the nanostructure materials-based "system on a wafer" architecture is a critical milestone to next generation microwave integrated systems. It is also practical that future microwave integrated systems and their magnetic performances could be tuned by an electric field because of the magnetoelectricity of hexaferrites.

Reconstructing three-dimensional protein crystal intensities from sparse unoriented two-axis X-ray diffraction patterns

PubMed Central

Lan, Ti-Yen; Wierman, Jennifer L.; Tate, Mark W.; Philipp, Hugh T.; Elser, Veit

2017-01-01

Recently, there has been a growing interest in adapting serial microcrystallography (SMX) experiments to existing storage ring (SR) sources. For very small crystals, however, radiation damage occurs before sufficient numbers of photons are diffracted to determine the orientation of the crystal. The challenge is to merge data from a large number of such ‘sparse’ frames in order to measure the full reciprocal space intensity. To simulate sparse frames, a dataset was collected from a large lysozyme crystal illuminated by a dim X-ray source. The crystal was continuously rotated about two orthogonal axes to sample a subset of the rotation space. With the EMC algorithm [expand–maximize–compress; Loh & Elser (2009). Phys. Rev. E, 80, 026705], it is shown that the diffracted intensity of the crystal can still be reconstructed even without knowledge of the orientation of the crystal in any sparse frame. Moreover, parallel computation implementations were designed to considerably improve the time and memory scaling of the algorithm. The results show that EMC-based SMX experiments should be feasible at SR sources. PMID:28808431

Evolution of Morphology and Crystallinity of Silica Minerals Under Hydrothermal Conditions

NASA Astrophysics Data System (ADS)

Isobe, H.

2011-12-01

Silica minerals are quite common mineral species in surface environment of the terrestrial planets. They are good indicator of terrestrial processes including hydrothermal alteration, diagenesis and soil formation. Hydrothermal quartz, metastable low temperature cristobalite and amorphous silica show characteristic morphology and crystallinity depending on their formation processes and kinetics under wide range of temperature, pressure, acidity and thermal history. In this study, silica minerals produced by acidic hydrothermal alteration related to volcanic activities and hydrothermal crystallization experiments from diatom sediment are examined with crystallographic analysis and morphologic observations. Low temperature form of cistobalite is a metastable phase and a common alteration product occured in highly acidic hydrothermal environment around fumaroles in geothermal / volcanic areas. XRD analysis revealed that the alteration degree of whole rock is represented by abundance of cristobalite. Detailed powder XRD analysis show that the primary diffraction peak of cristobalite composed with two or three phases with different d-spacing and FWHM by peak profile fitting analysis. Shorter d-spacing and narrower FWHM cristobalite crystallize from precursor materials with less-crystallized, longer d-spacing and wider FWHM cristobalite. Textures of hydrothermal cristobalite in altered rock shows remnant of porphylitic texture of the host rock, pyroxene-amphibole andesite. Diatom has amorphous silica shell and makes diatomite sediment. Diatomite found in less diagenetic Quarternary formation keeps amorphous silica diatom shells. Hydrothermal alteration experiments of amorphous silica diatomite sediment are carried out from 300 °C to 550 °C. Mineral composition of run products shows crystallization of cristobalite and quartz progress depending on temperature and run durations. Initial crystallization product, cristobalite grains occur as characteristic lepispheres and granules with various surface structures. At the very initial stage of cristobalite crystallization within 2 days run duration, cristobalite shows lepispheres a few micron meters in diameter with irregular, submicron scale ridges and grooves on the surface. With the run duration up to 7 days, lepispheres change to granules with smooth surface remaining a few micron meters in diameter. Crystallinity of cristobalite lepispheres and granules corresponds to opal-CT. Euhedral quartz crystals grow with dissolution of cristobalite grains. Growth rate of cristobalite and quartz is controlled by crystallization kinetics with induction period strongly depending on temperature. Induction period of cristobalite crystallization from amorphous silica may exceed several million years at temperature below 100 °C. Crystallinity, morphology and growth rate of silica minerals occurred in various terrestrial and planetary processes are controlled by temperature and acidity of hydrothermal fluid and nucleation and growth kinetics of silica minerals.

Calcium Carbonate Crystal Growth in Porous Media, in the presence of Water Miscible and Non-Miscible Organic Fluids

NASA Astrophysics Data System (ADS)

Jaho, Sofia; Sygouni, Varvara; Paraskeva, Christakis A.

2015-04-01

The deposition of sparingly soluble salts (scaling) within porous media is a major problem encountered in many industrial and environmental applications. In the oil industry scaling causes severe operational malfunctions and, therefore, increasing the total operating and maintenance cost [1]. The most common types of sparingly soluble salts located in oil fields include carbonate and sulfate salts of calcium, strondium and barium[1,2]. Multiple phase flow and tubing surface properties are some of the factors affecting scale formation [3]. The main purpose of the present work was the investigation of the precipitation mechanisms of calcium carbonate (CaCO3) through in situ mixing of two soluble salt solutions in a flow granular medium, in the presence of water miscible organic fluid (ethylene glycol) or non-miscible organic fluid (n-dodecane). All series of experiments were carried out in a two dimensional porous medium made of Plexiglas. For all solutions used in the experiments, the contact angles with the surface of the porous medium and the interfacial tensions were measured. During the experiments, the calcium carbonate crystal growth was continuously monitored and recorded through an optical microscope equipped with a digital programmed video camera. The snap-shots were taken within specific time intervals and their detailed procession gave information concerning the crystal growth rate and kinetics. The pH of the effluent was measured and fluids samples were collected for calcium analysis using Atomic Absorption Spectroscopy (AAS). In all experiments effluent calcium concentration decreased as a function of time, suggesting that CaCO3 precipitation took place inside the porous medium. Crystals of the precipitated salt were identified using Infrared Spectroscopy (IR) and the morphology of the crystals was examined using Scanning Electron Microscopy (SEM). The induction time for precipitation of CaCO3 crystals in the presence of n-dodecane was significantly reduced compared to the induction time where no oil phase was present. The interface of n-dodecane and supersaturated solutions seems to be very active and favored the formation of the CaCO3 crystalline enhancing the heterogeneous nucleation which generally demands a decreased energy barrier. Acknowledgments This research was partially funded by the European Union (European Social Fund-ESF) and Greek National Funds through the Operational Program "Education and Lifelong Learning" under the action Aristeia II (Code No4420). References 1. Merdhah A. B. and Yassin A. A., Scale formation in oil reservoir during water injection at high-salinity formation water, Journal of Applied Sciences, 7, 3198-3207 (2007). 2. Moghadasi J., Muller-Steinhagen H., Jamialahmadi M. and Sharif A., Model study on the kinetics of oil field formation damage due to salt precipitation from injection, Journal of Petroleum Science and Engineering, 43, 201-217 (2004). 3. Nancollas G. H. and Reddy M. M., The crystallization of calcium carbonate II. Calcite growth mechanism, Journal of Colloid and Interface Science, 37, 824-830 (1971).

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zipper, Lauren E.; Aristide, Xavier; Bishop, Dylan P.

A method is described for using plate lids to reduce evaporation in low-volume vapor-diffusion crystallization experiments. The plate lids contain apertures through which the protein and precipitants were added to different crystallization microplates (the reservoir was filled before fitting the lids). Plate lids were designed for each of these commonly used crystallization microplates. This system minimizes the dehydration of crystallization droplets containing just a few nanolitres of protein and precipitant, and results in more reproducible diffraction from the crystals. For each lid design, changes in the weight of the plates were used to deduce the rate of evaporation under differentmore » conditions of temperature, air movement, droplet size and precipitant. For comparison, the state of dehydration was also visually assessed throughout the experiment. Finally, X-ray diffraction methods were used to compare the diffraction of protein crystals that were conventionally prepared against those that were prepared on plates with plate lids. The measurements revealed that the plate lids reduced the rate of evaporation by 63–82%. Crystals grown in 5 nl drops that were set up with plate lids diffracted to higher resolution than similar crystals from drops that were set up without plate lids. Ultimately, the results demonstrate that plate lids can be instrumental for improving few-nanolitre crystallizations.« less

Development and characterization of an ice-selecting pumped counterflow virtual impactor (IS-PCVI) to study ice crystal residuals

NASA Astrophysics Data System (ADS)

Hiranuma, Naruki; Möhler, Ottmar; Kulkarni, Gourihar; Schnaiter, Martin; Vogt, Steffen; Vochezer, Paul; Järvinen, Emma; Wagner, Robert; Bell, David M.; Wilson, Jacqueline; Zelenyuk, Alla; Cziczo, Daniel J.

2016-08-01

Separation of particles that play a role in cloud activation and ice nucleation from interstitial aerosols has become necessary to further understand aerosol-cloud interactions. The pumped counterflow virtual impactor (PCVI), which uses a vacuum pump to accelerate the particles and increase their momentum, provides an accessible option for dynamic and inertial separation of cloud elements. However, the use of a traditional PCVI to extract large cloud hydrometeors is difficult mainly due to its small cut-size diameters (< 5 µm). Here, for the first time we describe a development of an ice-selecting PCVI (IS-PCVI) to separate ice in controlled mixed-phase cloud system based on the particle inertia with the cut-off diameter ≥ 10 µm. We also present its laboratory application demonstrating the use of the impactor under a wide range of temperature and humidity conditions. The computational fluid dynamics simulations were initially carried out to guide the design of the IS-PCVI. After fabrication, a series of validation laboratory experiments were performed coupled with the Aerosol Interaction and Dynamics in the Atmosphere (AIDA) expansion cloud simulation chamber. In the AIDA chamber, test aerosol particles were exposed to the ice supersaturation conditions (i.e., RHice > 100 %), where a mixture of droplets and ice crystals was formed during the expansion experiment. In parallel, the flow conditions of the IS-PCVI were actively controlled, such that it separated ice crystals from a mixture of ice crystals and cloud droplets, which were of diameter ≥ 10 µm. These large ice crystals were passed through the heated evaporation section to remove the water content. Afterwards, the residuals were characterized with a suite of online and offline instruments downstream of the IS-PCVI. These results were used to assess the optimized operating parameters of the device in terms of (1) the critical cut-size diameter, (2) the transmission efficiency and (3) the counterflow-to-input flow ratio. Particle losses were characterized by comparing the residual number concentration to the rejected interstitial particle number concentration. Overall results suggest that the IS-PCVI enables inertial separation of particles with a volume-equivalent particle size in the range of ~ 10-30 µm in diameter with small inadvertent intrusion (~  5 %) of unwanted particles.

A new generation of 99.999% enriched 28Si single crystals for the determination of Avogadro’s constant

NASA Astrophysics Data System (ADS)

Abrosimov, N. V.; Aref'ev, D. G.; Becker, P.; Bettin, H.; Bulanov, A. D.; Churbanov, M. F.; Filimonov, S. V.; Gavva, V. A.; Godisov, O. N.; Gusev, A. V.; Kotereva, T. V.; Nietzold, D.; Peters, M.; Potapov, A. M.; Pohl, H.-J.; Pramann, A.; Riemann, H.; Scheel, P.-T.; Stosch, R.; Wundrack, S.; Zakel, S.

2017-08-01

A metrological challenge is currently underway to replace the present definition of the kilogram. One prerequisite for this is that the Avogadro constant, N A, which defines the number of atoms in a mole, needs to be determined with a relative uncertainty of better than 2  ×  10-8. The method applied in this case is based on the x-ray crystal density experiment using silicon crystals. The first attempt, in which silicon of natural isotopic composition was used, failed. The solution chosen subsequently was the usage of silicon highly enriched in 28Si from Russia. First, this paper reviews previous efforts from the very first beginnings to an international collaboration with the goal of producing a 28Si single crystal with a mass of 5 kg, an enrichment greater than 0.9999 and of sufficient chemical purity. Then the paper describes the activities of a follow-up project, conducted by PTB, to produce a new generation of highly enriched silicon in order to demonstrate the quasi-industrial and reliable production of more than 12 kg of the 28Si material with enrichments of five nines. The intention of this project is also to show the availability of 28Si single crystals as a guarantee for the future realisation of the redefined kilogram.

High power, high contrast hybrid femtosecond laser systems

NASA Astrophysics Data System (ADS)

Dabu, Razvan

2017-06-01

For many research applications a very high laser intensity of more than 1022 W/cm2 in the focused beam is required. If a laser intensity of about 1011W/cm2 is reached on the target before the main laser pulse, the generated pre-plasma disturbs the experiment. High power femtosecond lasers must be tightly focused to get high intensity and in the same time must have a high enough intensity contrast of the temporally compressed amplified pulses. Reaching an intensity contrast in the range of 1012 represents a challenging task for a Ti:sapphire CPA laser. Hybrid femtosecond lasers combine optical parametric chirped pulsed amplification (OPCPA) in nonlinear crystals with the chirped pulse amplification (CPA) in laser active media. OPCPA provides large amplification spectral bandwidth and improves the intensity contrast of the amplified pulses. A key feature of these systems consists in the adaptation of the parametric amplification phase-matching bandwidth of nonlinear crystals to the spectral gain bandwidth of laser amplifying Ti:sapphire crystals. OPCPA in BBO crystals up to mJ energy level in the laser Front-End, followed by CPA up to ten/hundred Joules in large aperture Ti:sapphire crystals, represents a suitable solution for PW-class femtosecond lasers. The configuration and expected output beam characteristics of the hybrid amplification 2 × 10 PW ELI-NP laser are described.

Drift mobility of photo-electrons in organic molecular crystals: Quantitative comparison between theory and experiment

NASA Astrophysics Data System (ADS)

Reineker, P.; Kenkre, V. M.; Kühne, R.

1981-08-01

A quantitative comparison of a simple theoretical prediction for the drift mobility of photo-electrons in organic molecular crystals, calculated within the model of the coupled band-like and hopping motion, with experiments in napthalene of Schein et al. and Karl et al. is given.

Using Magnetic Fields to Control Convection during Protein Crystallization: Analysis and Validation Studies

NASA Technical Reports Server (NTRS)

Ramachandran, N.; Leslie, F. W.

2004-01-01

The effect of convection during the crystallization of proteins is not very well understood. In a gravitational field, convection is caused by crystal sedimentation and by solutal buoyancy induced flow and these can lead to crystal imperfections. While crystallization in microgravity can approach diffusion limited growth conditions (no convection), terrestrially strong magnetic fields can be used to control fluid flow and sedimentation effects. In this work, we develop the analysis for magnetic flow control and test the predictions using analog experiments. Specifically, experiments on solutal convection in a paramagnetic fluid were conducted in a strong magnetic field gradient using a dilute solution of Manganese Chloride. The observed flows indicate that the magnetic field can completely counter the settling effects of gravity locally and are consistent with the theoretical predictions presented. This phenomenon suggests that magnetic fields may be useful in mimicking the microgravity environment of space for some crystal growth ana biological applications where fluid convection is undesirable.

Crystallization history of lunar picritic basalt sample 12002 - Phase-equilibria and cooling-rate studies

NASA Technical Reports Server (NTRS)

Walker, D.; Kirkpatrick, R. J.; Longhi, J.; Hays, J. F.

1976-01-01

Experimental crystallization of a lunar picrite composition (sample 12002) at controlled linear cooling rates produces systematic changes in the temperature at which crystalline phases appear, in the texture, and in crystal morphology as a function of cooling rate. Phases crystallize in the order olivine, chromium spinel, pyroxene, plagioclase, and ilmenite during equilibrium crystallization, but ilmenite and plagioclase reverse their order of appearance and silica crystallizes in the groundmass during controlled cooling experiments. The partition of iron and magnesium between olivine and liquid is independent of cooling rate, temperature, and pressure. Comparison of the olivine nucleation densities in the lunar sample and in the experiments indicates that the sample began cooling at about 1 deg C/hr. Pyroxene size, chemistry, and growth instability spacings, as well as groundmass coarseness, all suggest that the cooling rate subsequently decreased by as much as a factor of 10 or more. The porphyritic texture of this sample, then, is produced at a decreasing, rather than a discontinuously increasing, cooling rate.

Rebamipide Suppresses Monosodium Urate Crystal-Induced Interleukin-1β Production Through Regulation of Oxidative Stress and Caspase-1 in THP-1 Cells.

PubMed

Kim, Seong-Kyu; Choe, Jung-Yoon; Park, Ki-Yeun

2016-02-01

This study investigated the effect of rebamipide on activation of the NLRP3 inflammasome and generation of reactive oxygen species (ROS) in monosodium urate (MSU) crystal-induced interleukin-1β (IL-1β) production. Human monocyte cell line THP-1 and human umbilical venous endothelial cells (HUVECs) were used to assess the inflammatory response to MSU crystals. NADP/NADPH activity assays were used as a marker of ROS generation. Quantitative real-time polymerase chain reaction (qRT-PCR) and western blotting were performed to evaluate levels of IL-1β, caspase-1, NLRP3, associated speck-like protein (ASC), nuclear factor-κB (NF-κB), p65, IκBα, intercellular adhesion molecule 1 (ICAM-1), and vascular cell adhesion molecule 1 (VCAM-1). Experimental pharmaceuticals included rebamipide, colchicine, dexamethasone, and ascorbic acid. In THP-1 cells, treatment with MSU crystals increased NADP/NADPH ratios and IL-1β expression, and both of these responses were potently inhibited by addition of rebamipide. Rebamipide also attenuated enhanced expression of caspase-1 gene by MSU crystals (p < 0.05). Western blotting demonstrated that MSU crystals stimulated caspase-1 but not NLRP3 and ASC activation. Similarly, MSU crystals activated the NF-κB pathway, which in turn was blocked by rebamipide. Stimulation of HUVECs with MSU crystals increased expression of VCAM-1 and ICAM-1, which were markedly inhibited by both rebamipide and dexamethasone. This study demonstrated that rebamipide inhibits IL-1β activation through suppression of ROS-mediated NF-κB signaling pathways and caspase-1 activation in MSU crystal-induced inflammation.

STS-72 Space Shuttle Mission Report

NASA Technical Reports Server (NTRS)

Fricke, Robert W., Jr.

1996-01-01

The STS-72 Space Shuttle Program Mission Report summarizes the Payload activities as well as the Orbiter, External Tank (ET), Solid Rocket Booster (SRB), Reusable Solid Rocket Motor (RSRM), and the Space Shuttle main engine (SSME) systems performance during the seventy-fourth flight of the Space Shuttle Program, the forty-ninth flight since the return-to-flight, and the tenth flight of the Orbiter Endeavour (OV-105). In addition to the Orbiter, the flight vehicle consisted of an ET that was designated ET-75; three Block I SSME's that were designated as serial numbers 2028, 2039, and 2036 in positions 1, 2, and 3, respectively; and two SRB's that were designated BI-077. The RSRM's, designated RSRM-52, were installed in each SRB and the individual RSRM's were designated as 36OW052A for the left SRB, and 36OW052B for the right SRB. Appendix A lists the sources of data, both formal and informal, that were used to prepare this report. The primary objectives of this flight were to retrieve the Japanese Space Flyer Unit (JSFU) and deploy and retrieve the Office of Aeronautics and Space Technology-Flyer (OAST-Flyer). Secondary objectives were to perform the operations of the Shuttle Solar Backscatter Ultraviolet (SSBUV/A) experiment, Shuttle Laser Altimeter (SLA)/get-Away Special (GAS) payload, Physiological and Anatomical Rodent Experiment/National Institutes of Health-Cells (STL/NIH-C) experiment, Protein Crystal Growth-Single Locker Thermal Enclosure System (PCG-STES) experiment, Commercial Protein Crystal Growth (CPCG) payload and perform two extravehicular activities (EVA's) to demonstrate International Space Station Alpha (ISSA) assembly techniques). Appendix B provides the definition of acronyms and abbreviations used throughout the report. All times during the flight are given in Greenwich mean time (GMT) and mission elapsed time (MET).

Li2MoO4 crystal growth from solution activated by low-frequency vibrations

NASA Astrophysics Data System (ADS)

Barinova, Olga; Sadovskiy, Andrey; Ermochenkov, Ivan; Kirsanova, Svetlana; Sukhanova, Ekaterina; Kostikov, Vladimir; Belov, Stanislav; Mozhevitina, Elena; Khomyakov, Andrew; Kuchuk, Zhanna; Zharikov, Eugeny; Avetissov, Igor

2017-01-01

The possibility of Li2MoO4 crystal growth from aqueous solutions activated by axial vibrational control (AVC) technique was investigated. It was found out that a low-frequency mechanical activation of the solution led to an increase of Li2MoO4 equilibrium solubility in aqueous solution for 11 rel% in the 25-29 °C temperature range. The changes in solution structure were analyzed in situ by Raman study of the solution. The AVC activation of solution resulted in a re-faceting of growing crystals, a smoothing of a face surface morphology and reduction of water content in the crystal.

Did an Impact Make the Mysterious Microscopic Magnetite Crystals in ALH 84001?

NASA Astrophysics Data System (ADS)

Taylor, G. J.

2007-10-01

Fervent debate swirls around microscopic crystals of magnetite (Fe3O4) in Martian meteorite ALH 84001. Some investigators suggest that the crystals are evidence of past life on Mars, citing magnetite crystals of similar chemical compositions and sizes made by magnetotactic bacteria on Earth. Others cite assorted experiments and observations to argue that the important little crystals formed entirely by non-biological processes, hence say nothing about life on Mars. One of those processes is the decomposition of iron carbonate (the mineral siderite), which occurs in ALH 84001. Researchers argue that heating this mineral causes it to decompose into magnetite and CO2 gas. Experiments showing this were done by heating siderite and observing that it decomposed and formed magnetite, but nobody had shock-heated siderite to see if magnetite crystals formed. (Shock is a rapid, strong rise and fall in pressure. It happens under many circumstances, including meteorite impacts.) The lack of shock experiments has been solved by Mary Sue Bell (University of Houston and Jacobs Engineering). She experimentally shocked samples of siderite at the Experimental Impact Laboratory at the Johnson Space Center. She shows that magnetite crystals of the right size and composition formed when samples were shocked to 49 GPa (about 500,000 times the pressure at the Earth's surface). This is more evidence for a non-biological origin for the magnetite crystals in ALH 84001 and is consistent with what we know about the impact history of the rock. There seems to be growing evidence against a biological origin, but don't expect these results to completely settle the debate!

A Fiber Optic Probe for Monitoring Protein Aggregation, Nucleation, and Crystallization

NASA Technical Reports Server (NTRS)

Ansari, Rafat R.; Suh, Kwang I.; Arabshahi, Alireza; Wilson, William W.; Bray, Terry L.; DeLucas, Lawrence J.

1996-01-01

Protein crystals are experimentally grown in hanging drops in microgravity experiments on-board the Space Shuttle orbiter. The technique of dynamic light scattering (DLS) can be used to monitor crystal growth process in hanging droplets (approx. 30 (L)) in microgravity experiments, but elaborate instrumentation and optical alignment problems have made in-situ applications difficult. In this paper we demonstrate that such experiments are now feasible. We apply a newly developed fiber optic probe to various earth and space (micro- gravity) bound protein crystallization system configurations to test its capability. These include conventional batch (cuvette or capillary) systems, hanging drop method in a six-pack hanging drop vapor diffusion apparatus (HDVDA), a modified HDVDA for temperature- induced nucleation and aggregation studies, and a newly envisioned dynamically controlled vapor diffusion system (DCVDS) configuration. Our compact system exploits the principles of DLS and offers a fast (within a few seconds) means of quantitatively and non-invasively monitoring the various growth stages of protein crystallization. In addition to DLS capability, the probe can also be used for performing single-angle static light scattering measurements. It utilizes extremely low levels of laser power (approx. few (W)) without a need of having any optical alignment and vibration isolation. The compact probe is also equipped with a miniaturized microscope for visualization of macroscopic protein crystals. This new optical diagnostic system opens up enormous opportunity for exploring new ways to grow good quality crystals suitable for x-ray crystallographic analysis and may help develop a concrete scientific basis for understanding the process of crystallization.

Experimental Plan for Crystal Accumulation Studies in the WTP Melter Riser

DOE Office of Scientific and Technical Information (OSTI.GOV)

Miller, D.; Fowley, M.

2015-04-28

This experimental plan defines crystal settling experiments to be in support of the U.S. Department of Energy – Office of River Protection crystal tolerant glass program. The road map for development of crystal-tolerant high level waste glasses recommends that fluid dynamic modeling be used to better understand the accumulation of crystals in the melter riser and mechanisms of removal. A full-scale version of the Hanford Waste Treatment and Immobilization Plant (WTP) melter riser constructed with transparent material will be used to provide data in support of model development. The system will also provide a platform to demonstrate mitigation or recoverymore » strategies in off-normal events where crystal accumulation impedes melter operation. Test conditions and material properties will be chosen to provide results over a variety of parameters, which can be used to guide validation experiments with the Research Scale Melter at the Pacific Northwest National Laboratory, and that will ultimately lead to the development of a process control strategy for the full scale WTP melter. The experiments described in this plan are divided into two phases. Bench scale tests will be used in Phase 1 (using the appropriate solid and fluid simulants to represent molten glass and spinel crystals) to verify the detection methods and analytical measurements prior to their use in a larger scale system. In Phase 2, a full scale, room temperature mockup of the WTP melter riser will be fabricated. The mockup will provide dynamic measurements of flow conditions, including resistance to pouring, as well as allow visual observation of crystal accumulation behavior.« less

A simple technique to reduce evaporation of crystallization droplets by using plate lids with apertures for adding liquids

PubMed Central

Zipper, Lauren E.; Aristide, Xavier; Bishop, Dylan P.; Joshi, Ishita; Kharzeev, Julia; Patel, Krishna B.; Santiago, Brianna M.; Joshi, Karan; Dorsinvil, Kahille; Sweet, Robert M.; Soares, Alexei S.

2014-01-01

A method is described for using plate lids to reduce evaporation in low-volume vapor-diffusion crystallization experiments. The plate lids contain apertures through which the protein and precipitants were added to different crystallization microplates (the reservoir was filled before fitting the lids). Plate lids were designed for each of these commonly used crystallization microplates. This system minimizes the dehydration of crystallization droplets containing just a few nanolitres of protein and precipitant, and results in more reproducible diffraction from the crystals. For each lid design, changes in the weight of the plates were used to deduce the rate of evaporation under different conditions of temperature, air movement, droplet size and precipitant. For comparison, the state of dehydration was also visually assessed throughout the experiment. Finally, X-ray diffraction methods were used to compare the diffraction of protein crystals that were conventionally prepared against those that were prepared on plates with plate lids. The measurements revealed that the plate lids reduced the rate of evaporation by 63–82%. Crystals grown in 5 nl drops that were set up with plate lids diffracted to higher resolution than similar crystals from drops that were set up without plate lids. The results demonstrate that plate lids can be instrumental for improving few-nanolitre crystallizations. PMID:25484231

A simple technique to reduce evaporation of crystallization droplets by using plate lids with apertures for adding liquids

DOE PAGES

Zipper, Lauren E.; Aristide, Xavier; Bishop, Dylan P.; ...

2014-11-28

A method is described for using plate lids to reduce evaporation in low-volume vapor-diffusion crystallization experiments. The plate lids contain apertures through which the protein and precipitants were added to different crystallization microplates (the reservoir was filled before fitting the lids). Plate lids were designed for each of these commonly used crystallization microplates. This system minimizes the dehydration of crystallization droplets containing just a few nanolitres of protein and precipitant, and results in more reproducible diffraction from the crystals. For each lid design, changes in the weight of the plates were used to deduce the rate of evaporation under differentmore » conditions of temperature, air movement, droplet size and precipitant. For comparison, the state of dehydration was also visually assessed throughout the experiment. Finally, X-ray diffraction methods were used to compare the diffraction of protein crystals that were conventionally prepared against those that were prepared on plates with plate lids. The measurements revealed that the plate lids reduced the rate of evaporation by 63–82%. Crystals grown in 5 nl drops that were set up with plate lids diffracted to higher resolution than similar crystals from drops that were set up without plate lids. Ultimately, the results demonstrate that plate lids can be instrumental for improving few-nanolitre crystallizations.« less

Materials processing in space bibliography, 1983, revised

NASA Technical Reports Server (NTRS)

Pentecost, E. (Compiler)

1983-01-01

Flight experiments utilizing a low gravity environment to elucidate and control various processes, or ground based activities that provide supporting research are compiled. Six major categories: crystal growth; solidification of metals, alloys, and composites; fluids, transports, and chemical processes; glasses and ceramics; ultrahigh vacuum and containerless processing technologies; and combustion are included. A list of patents and appendices providing a compilation of anonymously authored collections and reports and a cross reference index are included.

Monosodium Urate Crystals Induce Upregulation of NK1.1-Dependent Killing by Macrophages and Support Tumor-Resident NK1.1+ Monocyte/Macrophage Populations in Antitumor Therapy.

PubMed

Steiger, Stefanie; Kuhn, Sabine; Ronchese, Franca; Harper, Jacquie L

2015-12-01

Macrophages display phenotypic and functional heterogeneity dependent on the changing inflammatory microenvironment. Under some conditions, macrophages can acquire effector functions commonly associated with NK cells. In the current study, we investigated how the endogenous danger signal monosodium urate (MSU) crystals can alter macrophage functions. We report that naive, primary peritoneal macrophages rapidly upregulate the expression of the NK cell-surface marker NK1.1 in response to MSU crystals but not in response to LPS or other urate crystals. NK1.1 upregulation by macrophages was associated with mechanisms including phagocytosis of crystals, NLRP3 inflammasome activation, and autocrine proinflammatory cytokine signaling. Further analysis demonstrated that MSU crystal-activated macrophages exhibited NK cell-like cytotoxic activity against target cells in a perforin/granzyme B-dependent manner. Furthermore, analysis of tumor hemopoietic cell populations showed that effective, MSU-mediated antitumor activity required coadministration with Mycobacterium smegmatis to induce IL-1β production and significant accumulation of monocytes and macrophages (but not granulocytes or dendritic cells) expressing elevated levels of NK1.1. Our findings provide evidence that MSU crystal-activated macrophages have the potential to develop tumoricidal NK cell-like functions that may be exploited to boost antitumor activity in vivo. Copyright © 2015 by The American Association of Immunologists, Inc.

Binary Colloidal Alloy Test Conducted on Mir

NASA Technical Reports Server (NTRS)

Hoffmann, Monica I.; Ansari, Rafat R.

1999-01-01

Colloids are tiny (submicron) particles suspended in fluid. Paint, ink, and milk are examples of colloids found in everyday life. The Binary Colloidal Alloy Test (BCAT) is part of an extensive series of experiments planned to investigate the fundamental properties of colloids so that scientists can make colloids more useful for technological applications. Some of the colloids studied in BCAT are made of two different sized particles (binary colloidal alloys) that are very tiny, uniform plastic spheres. Under the proper conditions, these colloids can arrange themselves in a pattern to form crystals. These crystals may form the basis of new classes of light switches, displays, and optical devices. Windows made of liquid crystals are already in the marketplace. These windows change their appearance from transparent to opaque when a weak electric current is applied. In the future, if the colloidal crystals can be made to control the passage of light through them, such products could be made much more cheaply. These experiments require the microgravity environment of space because good quality crystals are difficult to produce on Earth because of sedimentation and convection in the fluid. The BCAT experiment hardware included two separate modules for two different experiments. The "Slow Growth" hardware consisted of a 35-mm camera with a 250- exposure photo film cartridge. The camera was aimed toward the sample module, which contained 10 separate colloid samples. A rack of small lights provided backlighting for the photographs. The BCAT hardware was launched on the shuttle and was operated aboard the Russian space station Mir by American astronauts John Blaha and David Wolf (launched September 1996 and returned January 1997; reflown September 1997 and returned January 1998). To begin the experiment, one of these astronauts would mix the samples to disperse the colloidal particles and break up any crystals that might have already formed. Once the samples were mixed and the experiment was powered on, the hardware operated autonomously, taking photos of the colloidal samples over a 90-day period.

The Additive Coloration of Alkali Halides

ERIC Educational Resources Information Center

Jirgal, G. H.; and others

1969-01-01

Describes the construction and use of an inexpensive, vacuum furnace designed to produce F-centers in alkali halide crystals by additive coloration. The method described avoids corrosion or contamination during the coloration process. Examination of the resultant crystals is discussed and several experiments using additively colored crystals are…

Calcium oxalate crystals induces tight junction disruption in distal renal tubular epithelial cells by activating ROS/Akt/p38 MAPK signaling pathway.

PubMed

Yu, Lei; Gan, Xiuguo; Liu, Xukun; An, Ruihua

2017-11-01

Tight junction plays important roles in regulating paracellular transports and maintaining cell polarity. Calcium oxalate monohydrate (COM) crystals, the major crystalline composition of kidney stones, have been demonstrated to be able to cause tight junction disruption to accelerate renal cell injury. However, the cellular signaling involved in COM crystal-induced tight junction disruption remains largely to be investigated. In the present study, we proved that COM crystals induced tight junction disruption by activating ROS/Akt/p38 MAPK pathway. Treating Madin-Darby canine kidney (MDCK) cells with COM crystals induced a substantial increasing of ROS generation and activation of Akt that triggered subsequential activation of ASK1 and p38 mitogen-activated protein kinase (MAPK). Western blot revealed a significantly decreased expression of ZO-1 and occludin, two important structural proteins of tight junction. Besides, redistribution and dissociation of ZO-1 were observed by COM crystals treatment. Inhibition of ROS by N-acetyl-l-cysteine (NAC) attenuated the activation of Akt, ASK1, p38 MAPK, and down-regulation of ZO-1 and occludin. The redistribution and dissociation of ZO-1 were also alleviated by NAC treatment. These results indicated that ROS were involved in the regulation of tight junction disruption induced by COM crystals. In addition, the down-regulation of ZO-1 and occludin, the phosphorylation of ASK1 and p38 MAPK were also attenuated by MK-2206, an inhibitor of Akt kinase, implying Akt was involved in the disruption of tight junction upstream of p38 MAPK. Thus, these results suggested that ROS-Akt-p38 MAPK signaling pathway was activated in COM crystal-induced disruption of tight junction in MDCK cells.

Measurement of Microscopic Growth Rates in Float-Zone Silicon Crystals

NASA Technical Reports Server (NTRS)

Dold, P.; Schweizer, M.; Benz, K. W.; Rose, M. Franklin (Technical Monitor)

2001-01-01

Time dependent convective flows during crystal growth of doped semiconductors lead to fluctuations of the composition, so called dopant striations. In general, it is difficult to decide which is the main mechanism for the generation of these striations, it might be either the fluctuation of the concentration field in the melt and the extent of the solute boundary layer ahead of the solid-liquid interface or a variation of the growth velocity. Direct access to the concentration field is rather complicated to achieve, especially considering the high process temperature and the chemical activity of liquid silicon. The contribution of growth rate fluctuations to the formation of compositional fluctuations can be determined by measuring microscopic growth rates. The classical method of current pulses requires electrical feed-throughs and good electrical contacts, both are critical issues for the growth of high purity silicon crystals. Using a radiation based heating system, the heating power can be modulated very fast and effectively. We added to the normal heater power a sinusoidal off-set in the frequency range of 1 to 10 Hz, generating a narrow spaced weak rippling in the grown crystals which are superposed to the dopant striations caused by natural and by thermocapillary convection. The pulling speed was varied between 1 and 4mm/min. The microscope images of etched crystals slices have been analyzed by peak-search algorithms (measuring the spacing between each artificially induced marker) and by FFT. Performing growth experiments under a time-dependent flow regime, fluctuations of the microscopic growth velocity of Delta(v)/v(sub average) up to 50% have been measured. Damping the time-dependent convection by the use of an axial, static magnetic field of 500mT, the microscopic growth rate became constant within the resolution limit of this method. The results will be discussed using analytical methods for the calculation of microscopic growth velocity and by comparing them with measurements of temperature fluctuations in the melt during growth experiments itself.

Kinetics and pathways for crystallization of amorphous mullite and YAG

NASA Astrophysics Data System (ADS)

Johnson, Bradley Richard

The crystallization behavior of quenched mullite (3Al2O 3•2SiO2) and YAG (Y3Al5O 12) composition glasses (made using containerless methods) were characterized with the ultimate goal of producing single crystal, structural, ceramic oxide fibers from these materials. The kinetics for crystallization were determined from thermal analysis experiments. From the results, time-temperature-transformation (TTT) curves were calculated. The crystallization pathways were determined by examining the crystal structure, microstructure, and chemical composition of heat treated specimens using x-ray diffraction (XRD), scanning electron microscopy (SEM), and transmission electron microscopy (TEM). A machine was also designed and built to facilitate controlled crystallization of amorphous fibers. Quenched, Y3Al5O12 composition beads crystallized at temperatures as low as 840°C. The as-received specimens contained a few, small YAG crystals, in addition to a mixture of different amorphous phases. The coexistence of two different amorphous phases of the same composition, but having different densities is termed polyamorphism, and this has been reported to occur in Y3Al5O12 composition quenched melts. Although various crystallization pathways have been reported for chemically synthesized YAG precursors, these specimens crystallized directly into YAG, which was the only phase formed. Quenched, 3Al2O3•2SiO2 composition mullite beads and fibers crystallized at temperatures as low as 920°C. Due to phase separation in the quenched melts, multiple phases with slightly different compositions and different crystallization activation energies crystallized. These phases were not equilibrium, 3:2 mullite, but metastable, alumina-rich, pseudotetragonal mullite. The residual, amorphous, silica-rich phase existed as numerous, 7--10 nm sized inclusions embedded within pseudotetragonal mullite. A large amount of internal strain was detected in pseudotetragonal mullite, and the source of this strain was suggested to be the embedded, silica-rich inclusions. Pseudotetragonal mullite gradually converted to equilibrium, orthorhombic, 3:2 mullite between 1000--1400°C. This was characterized by assimilation of the embedded, silica-rich inclusions and the elimination of internal strain. Additionally, recrystallization of numerous, small, strain- and inclusion-free, 3:2 mullite grains was observed to occur as the process proceeded to completion.

REE Incorporation into Calcite Individual Crystals as One Time Spike Addition

DOE Office of Scientific and Technical Information (OSTI.GOV)

Gabitov, Rinat; Sadekov, Aleksey; Migdisov, Artas

Experiments on the incorporation of trace elements into calcite were performed, and rare earth elements (REE) were used to mark the growth zones of individual crystals. Experiments were conducted at different pH (7.7 to 8.8) and temperatures (2 °C to 24.6 °C) in NH 4Cl + CaCl 2 solutions, where REE were rapidly consumed by growing calcite. LA-ICP-MS line-scans yielded the distribution of (REE/Ca) calcite within individual crystals in a manner consistent with the addition of REE into fluid. A sharp decrease of (REE/Ca) calcite toward the crystal edge suggests the fast depletion of (REE/Ca) fluid due to strong REEmore » consumption by growing calcite. An attempt was made to estimate the lower limit of the partition coefficients between calcite and fluid using selected REE/Ca data within individual calcite crystals and the amount of REE added into fluid.« less

Modern Possibilities for Calculating Some Properties of Molecules and Crystals from the Experimental Electron Density

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stash, A.I.; Tsirelson, V.G.

2005-03-01

Methods for calculating some properties of molecules and crystals from the electron density reconstructed from a precise X-ray diffraction experiment using the multipole model are considered. These properties include, on the one hand, the characteristics of the electron density and the inner-crystal electrostatic field and, on the other hand, the local electronic energies (kinetic, potential, total), the exchange energy density, the electron-pair localization function, the localized-orbital locator, the effective crystal potential, and others. It is shown that the integration of these characteristics over pseudoatomic volumes bounded by the surfaces of the zero flux of the electron density gradient makes itmore » possible to characterize directly from an experiment the properties of molecules and crystals in terms of the atomic contributions. The computer program WinXPRO2004, realizing these possibilities, is briefly described.« less

Quantitative Schlieren analysis applied to holograms of crystals grown on Spacelab 3

NASA Technical Reports Server (NTRS)

Brooks, Howard L.

1986-01-01

In order to extract additional information about crystals grown in the microgravity environment of Spacelab, a quantitative schlieren analysis technique was developed for use in a Holography Ground System of the Fluid Experiment System. Utilizing the Unidex position controller, it was possible to measure deviation angles produced by refractive index gradients of 0.5 milliradians. Additionally, refractive index gradient maps for any recorded time during the crystal growth were drawn and used to create solute concentration maps for the environment around the crystal. The technique was applied to flight holograms of Cell 204 of the Fluid Experiment System that were recorded during the Spacelab 3 mission on STS 51B. A triglycine sulfate crystal was grown under isothermal conditions in the cell and the data gathered with the quantitative schlieren analysis technique is consistent with a diffusion limited growth process.

REE Incorporation into Calcite Individual Crystals as One Time Spike Addition

DOE PAGES

Gabitov, Rinat; Sadekov, Aleksey; Migdisov, Artas

2017-10-26

Experiments on the incorporation of trace elements into calcite were performed, and rare earth elements (REE) were used to mark the growth zones of individual crystals. Experiments were conducted at different pH (7.7 to 8.8) and temperatures (2 °C to 24.6 °C) in NH 4Cl + CaCl 2 solutions, where REE were rapidly consumed by growing calcite. LA-ICP-MS line-scans yielded the distribution of (REE/Ca) calcite within individual crystals in a manner consistent with the addition of REE into fluid. A sharp decrease of (REE/Ca) calcite toward the crystal edge suggests the fast depletion of (REE/Ca) fluid due to strong REEmore » consumption by growing calcite. An attempt was made to estimate the lower limit of the partition coefficients between calcite and fluid using selected REE/Ca data within individual calcite crystals and the amount of REE added into fluid.« less

Growth, density functional theory (DFT) and spectral studies on L-2-aminobutyric acid -biologically active material

NASA Astrophysics Data System (ADS)

Usha, C.; Santhakumari, R.; Meenakshi, R.; Jayasree, R.; Bhuvaneswari, M.

2017-12-01

Single crystal of L-2-aminobutyric acid (ABA) was grown from water by slow evaporation at room temperature. The crystalline nature of the grown crystal was confirmed using powder X-ray diffraction studies. The grown crystal was subjected to FT-IR, FT-Raman, 1H NMR and 13C NMR spectral analyses to confirm the presence of functional group and molecular structure respectively. Thermal properties were investigated by thermogravimetric and differential thermal analyses. The range and percentage of optical transmission was ascertained by recording UV-vis-NIR spectrum. The electronic charge distribution and reactivity of the molecules within the crystal were studied by HOMO and LUMO analysis and the molecular electrostatic potential (MEP) of the grown crystal was performed using the B3LYP method. The anti-bacterial activities of the crystal were performed by disk diffusion method against the standard bacteria E. coli. The crystal exhibits good anti-bacterial activity. Second harmonic generation efficiency of the powdered ABA crystal was tested using Nd:YAG laser and it is found to be ∼3.3 times that of potassium dihydrogen orthophosphate.

Modeling the SHG activities of diverse protein crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Haupert, Levi M.; DeWalt, Emma L.; Simpson, Garth J.

2012-10-18

A symmetry-additiveab initiomodel for second-harmonic generation (SHG) activity of protein crystals was applied to assess the likely protein-crystal coverage of SHG microscopy. Calculations were performed for 250 proteins in nine point-group symmetries: a total of 2250 crystals. The model suggests that the crystal symmetry and the limit of detection of the instrument are expected to be the strongest predictors of coverage of the factors considered, which also included secondary-structural content and protein size. Much of the diversity in SHG activity is expected to arise primarily from the variability in the intrinsic protein response as well as the orientation within themore » crystal lattice. Two or more orders-of-magnitude variation in intensity are expected even within protein crystals of the same symmetry. SHG measurements of tetragonal lysozyme crystals confirmed detection, from which a protein coverage of ~84% was estimated based on the proportion of proteins calculated to produce SHG responses greater than that of tetragonal lysozyme. Good agreement was observed between the measured and calculated ratios of the SHG intensity from lysozyme in tetragonal and monoclinic lattices.« less

Antilithiatic Activity of phlorotannin rich extract of Sarghassum Wightii on Calcium Oxalate Urolithiais – In Vitro and In Vivo Evaluation

PubMed Central

Sujatha, D.; Singh, Kiranpal; Vohra, Mursalin; Kumar, K. Vijay; Sunitha, S.

2015-01-01

ABSTRACT Purpose: Urolithiasis is a common urological disorder responsible for serious human affliction and cost to the society with a high recurrence rate. The aim of the present study was to systematically evaluate the phlorotannin rich extract of Sargassum wightii using suitable in vitro and in vivo models to provide scientific evidence for its antilithiatic activity. Materials and Methods: To explore the effect of Sargassum wightii on calcium oxalate crystallization, in vitro assays like crystal nucleation, aggregation and crystal growth were performed. Calcium oxalate urolithiasis was induced in male Sprague dawley rats using a combination of gentamicin and calculi producing diet (5% ammonium oxalate and rat pellet feed). The biochemical parameters like calcium, oxalate, magnesium, phosphate, sodium and potassium were evaluated in urine, serum and kidney homogenates. Histopathological studies were also done to confirm the biochemical findings. Results: The yield of Sargassum wightii extract was found to be 74.5 gm/kg and confirmed by quantitative analysis. In vitro experiments with Sargassum wightii showed concentration dependent inhibition of calcium oxalate nucleation, aggregation and growth supported by SEM analysis. In the in vivo model, Sargassum wightii reduced both calcium and oxalate supersaturation in urine, serum and deposition in the kidney. The biochemical results were supported by histopathological studies. Conclusion: The findings of the present study suggest that Sargassum wightii has the ability to prevent nucleation, aggregation and growth of calcium oxalate crystals. Sargassum wightii has better preventive effect on calcium oxalate stone formation indicating its strong potential to develop as a therapeutic option to prevent recurrence of urolithiasis. PMID:26200544

Twin nucleation and migration in FeCr single crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Patriarca, L.; Abuzaid, Wael; Sehitoglu, Huseyin, E-mail: huseyin@illinois.edu

2013-01-15

Tension and compression experiments were conducted on body-centered cubic Fe -47.8 at pct. Cr single crystals. The critical resolved shear stress (CRSS) magnitudes for slip nucleation, twin nucleation and twin migration were established. We show that the nucleation of slip occurs at a CRSS of about 88 MPa, while twinning nucleates at a CRSS of about 191 MPa with an associated load drop. Following twin nucleation, twin migration proceeds at a CRSS that is lower than the initiation stress ( Almost-Equal-To 114-153 MPa). The experimental results of the nucleation stresses indicate that the Schmid law holds to a first approximationmore » for the slip and twin nucleation cases, but to a lesser extent for twin migration particularly when considerable slip strains preceded twinning. The CRSSs were determined experimentally using digital image correlation (DIC) in conjunction with electron back scattering diffraction (EBSD). The DIC measurements enabled pinpointing the precise stress on the stress-strain curves where twins or slip were activated. The crystal orientations were obtained using EBSD and used to determine the activated twin and slip systems through trace analysis. - Highlights: Black-Right-Pointing-Pointer Digital image correlation allows to capture slip/twin initiation for bcc FeCr. Black-Right-Pointing-Pointer Crystal orientations from EBSD allow slip/twin system indexing. Black-Right-Pointing-Pointer Nucleation of slip always precedes twinning. Black-Right-Pointing-Pointer Twin growth is sustained with a lower stress than required for nucleation. Black-Right-Pointing-Pointer Twin-slip interactions provide high hardening at the onset of plasticity.« less

Crystal Creations.

ERIC Educational Resources Information Center

Whipple, Nona; Whitmore, Sherry

1989-01-01

Presents a many-faceted learning approach to the study of crystals. Provides instructions for performing activities including crystal growth and patterns, creating miniature simulations of crystal-containing rock formations, charcoal and sponge gardens, and snowflakes. (RT)

Experimental petrology and origin of rocks from the Descartes Highlands

NASA Technical Reports Server (NTRS)

Walker, D.; Longhi, J.; Grove, T. L.; Stolper, E.; Hays, J. F.

1973-01-01

Petrographic studies of Apollo 16 samples indicate that rocks 62295 and 68415 are crystallization products of highly aluminous melts. 60025 is a shocked, crushed and partially annealed plagioclase cumulate. 60315 is a recrystallized noritic breccia of disputed origin. 60335 is a feldspathic basalt filled with xenoliths and xenocrysts of anorthosite, breccia, and anorthite. The Fe/(Fe+Mg) of plagioclase appears to be a relative crystallization index. Low pressure melting experiments with controlled Po2 indicate that the igneous samples crystallized at oxygen fugacities well below the Fe/FeO buffer. Crystallization experiments at various pressures suggest that the 62295 and 68415 compositions were produced by partial or complete melting of lunar crustal materials, and not by partial melting of the deep lunar interior.

Inelastic neutron scattering experiments with the monochromatic imaging mode of the RITA-II spectrometer

NASA Astrophysics Data System (ADS)

Bahl, C. R. H.; Lefmann, K.; Abrahamsen, A. B.; Rønnow, H. M.; Saxild, F.; Jensen, T. B. S.; Udby, L.; Andersen, N. H.; Christensen, N. B.; Jakobsen, H. S.; Larsen, T.; Häfliger, P. S.; Streule, S.; Niedermayer, Ch.

2006-05-01

Recently a monochromatic multiple data taking mode has been demonstrated for diffraction experiments using a RITA type cold neutron spectrometer with a multi-bladed analyser and a position-sensitive detector. Here, we show how this mode can be used in combination with a flexible radial collimator to perform real inelastic neutron scattering experiments. We present the results from inelastic powder, single crystal dispersion and single crystal constant energy mapping experiments. The advantages and complications of performing these experiments are discussed along with a comparison between the imaging mode and the traditional monochromatic focussing mode.

Serial crystallography captures enzyme catalysis in copper nitrite reductase at atomic resolution from one crystal.

PubMed

Horrell, Sam; Antonyuk, Svetlana V; Eady, Robert R; Hasnain, S Samar; Hough, Michael A; Strange, Richard W

2016-07-01

Relating individual protein crystal structures to an enzyme mechanism remains a major and challenging goal for structural biology. Serial crystallography using multiple crystals has recently been reported in both synchrotron-radiation and X-ray free-electron laser experiments. In this work, serial crystallography was used to obtain multiple structures serially from one crystal (MSOX) to study in crystallo enzyme catalysis. Rapid, shutterless X-ray detector technology on a synchrotron MX beamline was exploited to perform low-dose serial crystallography on a single copper nitrite reductase crystal, which survived long enough for 45 consecutive 100 K X-ray structures to be collected at 1.07-1.62 Å resolution, all sampled from the same crystal volume. This serial crystallography approach revealed the gradual conversion of the substrate bound at the catalytic type 2 Cu centre from nitrite to nitric oxide, following reduction of the type 1 Cu electron-transfer centre by X-ray-generated solvated electrons. Significant, well defined structural rearrangements in the active site are evident in the series as the enzyme moves through its catalytic cycle, namely nitrite reduction, which is a vital step in the global denitrification process. It is proposed that such a serial crystallography approach is widely applicable for studying any redox or electron-driven enzyme reactions from a single protein crystal. It can provide a 'catalytic reaction movie' highlighting the structural changes that occur during enzyme catalysis. The anticipated developments in the automation of data analysis and modelling are likely to allow seamless and near-real-time analysis of such data on-site at some of the powerful synchrotron crystallographic beamlines.

Models of Mass Transport During Microgravity Crystal Growth of Alloyed Semiconductors in a Magnetic Field

NASA Technical Reports Server (NTRS)

Ma, Nancy

2003-01-01

Alloyed semiconductor crystals, such as germanium-silicon (GeSi) and various II-VI alloyed crystals, are extremely important for optoelectronic devices. Currently, high-quality crystals of GeSi and of II-VI alloys can be grown by epitaxial processes, but the time required to grow a certain amount of single crystal is roughly 1,000 times longer than the time required for Bridgman growth from a melt. Recent rapid advances in optoelectronics have led to a great demand for more and larger crystals with fewer dislocations and other microdefects and with more uniform and controllable compositions. Currently, alloyed crystals grown by bulk methods have unacceptable levels of segregation in the composition of the crystal. Alloyed crystals are being grown by the Bridgman process in space in order to develop successful bulk-growth methods, with the hope that the technology will be equally successful on earth. Unfortunately some crystals grown in space still have unacceptable segregation, for example, due to residual accelerations. The application of a weak magnetic field during crystal growth in space may eliminate the undesirable segregation. Understanding and improving the bulk growth of alloyed semiconductors in microgravity is critically important. The purpose of this grant to to develop models of the unsteady species transport during the bulk growth of alloyed semiconductor crystals in the presence of a magnetic field in microgravity. The research supports experiments being conducted in the High Magnetic Field Solidification Facility at Marshall Space Flight Center (MSFC) and future experiments on the International Space Station.

Modeling the SHG activities of diverse protein crystals

DOE Office of Scientific and Technical Information (OSTI.GOV)

Haupert, Levi M.; DeWalt, Emma L.; Simpson, Garth J., E-mail: gsimpson@purdue.edu

2012-11-01

The origins of the diversity in the SHG signal from protein crystals are investigated and potential protein-crystal coverage by SHG microscopy is assessed. A symmetry-additive ab initio model for second-harmonic generation (SHG) activity of protein crystals was applied to assess the likely protein-crystal coverage of SHG microscopy. Calculations were performed for 250 proteins in nine point-group symmetries: a total of 2250 crystals. The model suggests that the crystal symmetry and the limit of detection of the instrument are expected to be the strongest predictors of coverage of the factors considered, which also included secondary-structural content and protein size. Much ofmore » the diversity in SHG activity is expected to arise primarily from the variability in the intrinsic protein response as well as the orientation within the crystal lattice. Two or more orders-of-magnitude variation in intensity are expected even within protein crystals of the same symmetry. SHG measurements of tetragonal lysozyme crystals confirmed detection, from which a protein coverage of ∼84% was estimated based on the proportion of proteins calculated to produce SHG responses greater than that of tetragonal lysozyme. Good agreement was observed between the measured and calculated ratios of the SHG intensity from lysozyme in tetragonal and monoclinic lattices.« less

Single Crystal Membranes

NASA Technical Reports Server (NTRS)

Stormont, R. W.; Morrison, A.

1974-01-01

Single crystal a- and c-axis tubes and ribbons of sodium beta-alumina and sodium magnesium beta-alumina were grown from sodium oxide rich melts. Additional experiments grew ribbon crystals containing sodium magnesium beta, beta double prime, beta triple prime, and beta quadruple prime. A high pressure crystal growth chamber, sodium oxide rich melts, and iridium for all surfaces in contact with the melt were combined with the edge-defined, film-fed growth technique to grow the single crystal beta-alumina tubes and ribbons. The crystals were characterized using metallographic and X-ray diffraction techniques, and wet chemical analysis was used to determine the sodium, magnesium, and aluminum content of the grown crystals.

Crewmember working on the spacelab Zeolite Crystal Growth experiment.

NASA Technical Reports Server (NTRS)

1992-01-01

View showing Payload Specialists Bonnie Dunbar and Larry DeLucas in the aft section of the U. S. Microgravity Laboratory-1. Dunbar is preparing to load a sample in the Crystal Growth Furnace (CGF) Integrated Furnace Experiment Assembly (IFEA) in rack 9 of the Microgravity Laboratory. DeLucas is checking out the multi-purpose Glovebox Facility.

Liquid-Crystal Displays: Fabrication and Measurement of a Twisted Nematic Liquid-Crystal Cell

ERIC Educational Resources Information Center

Waclawik, Eric R.; Ford, Michael J.; Hale, Penny S.; Shapter, Joe G.; Voelcker, Nico H.

2004-01-01

An experiment is developed for a laboratory course on nanostructures, as part of the undergraduate Bachelor of Science degree in nanotechnology at Flinders University. Designed to demonstrate the relationship between molecular order and the optical dielectric properties of the liquid crystalline state, the experiment is shown to be a useful tool…

Crystallization Experiments of the Martian Meteorite QUE94201: Additional Constraints on Its Formation Condition

NASA Technical Reports Server (NTRS)

Koizumi, E.; McKay, G.; Mikouchi, T.; Le, L.; Schwandt, C.; Monkawa, A.; Miyamoto, M.

2002-01-01

We focused on the Al/Ti ratio in synthetic pyroxenes as a marker for the onset of plagioclase crystallization and discuss the effects of oxygen fugacity on the Kd(Fe/Mg)ol/gl in our experiments using the same composition of QUE94201. Additional information is contained in the original extended abstract.

Highly reproducible alkali metal doping system for organic crystals through enhanced diffusion of alkali metal by secondary thermal activation.

PubMed

Lee, Jinho; Park, Chibeom; Song, Intek; Koo, Jin Young; Yoon, Taekyung; Kim, Jun Sung; Choi, Hee Cheul

2018-05-16

In this paper, we report an efficient alkali metal doping system for organic single crystals. Our system employs an enhanced diffusion method for the introduction of alkali metal into organic single crystals by controlling the sample temperature to induce secondary thermal activation. Using this system, we achieved intercalation of potassium into picene single crystals with closed packed crystal structures. Using optical microscopy and Raman spectroscopy, we confirmed that the resulting samples were uniformly doped and became K 2 picene single crystal, while only parts of the crystal are doped and transformed into K 2 picene without secondary thermal activation. Moreover, using a customized electrical measurement system, the insulator-to-semiconductor transition of picene single crystals upon doping was confirmed by in situ electrical conductivity and ex situ temperature-dependent resistivity measurements. X-ray diffraction studies showed that potassium atoms were intercalated between molecular layers of picene, and doped samples did not show any KH- nor KOH-related peaks, indicating that picene molecules are retained without structural decomposition. During recent decades, tremendous efforts have been exerted to develop high-performance organic semiconductors and superconductors, whereas as little attention has been devoted to doped organic crystals. Our method will enable efficient alkali metal doping of organic crystals and will be a resource for future systematic studies on the electrical property changes of these organic crystals upon doping.

Mass-transfer and supersaturation in crystal growth in gels. Application to CaSO 4·2H 2O

NASA Astrophysics Data System (ADS)

Prieto, M.; Viedma, C.; López-Acevedo, V.; Martín-Vivaldi, J. L.; López-Andrés, S.

1988-10-01

Supersaturation evaluation is an essential requirement to describe, confront and explain crystal growth experiences. However, in the particular case of crystal growth in gels, experiences are often described by attending to the initial concentration of reagent. This fact is connected with deficiencies in the theoretical quantification of mass-transfer, and therefore in both time and location prediction for the first precipitate. In this paper laboratory experiences have been specifically designed to test supersaturation evolution through an actual (finite) diffusion system. The problem is carried out by keeping into account several complexity factors: free ions as well as complexes and silica gel Na + and Cl - "unloading" are considered to evaluate the supersaturation.

Demonstrations with a Liquid Crystal Shutter

ERIC Educational Resources Information Center

Kraftmakher, Yaakov

2012-01-01

The experiments presented show the response of a liquid crystal shutter to applied electric voltages and the delay of the operations. Both properties are important for liquid crystal displays of computers and television sets. Two characteristics of the shutter are determined: (i) the optical transmittance versus applied voltage of various…

Dancing Crystals: A Dramatic Illustration of Intermolecular Forces

ERIC Educational Resources Information Center

Mundell, Donald W.

2007-01-01

Crystals of naphthalene form on the surface of an acetone solution and dance about in an animated fashion illustrating surface tension, crystallization, and intermolecular forces. Additional experiments reveal the properties of the solution. Flows within the solutions can be visualized by various means. Previous demonstrations of surface motion…

The Growth and Characterization of the Bismuth Strontium-Calcium 2212 Superconductor

NASA Astrophysics Data System (ADS)

Moulton, Linda Vidale

A miniaturized float zone technique, sometimes referred to as the Laser-heated Pedestal Growth (LHPG) method, was used to produce high quality crystals of the incongruently melting rm Bi_2Sr_2CaCu _2O_{8+delta} (2212) superconductor. The main focus of this research was to (1) produce superconducting samples having different compositions, (2) identify the melt compositions and growth temperatures which produced these samples, and (3) determine the variation of their superconducting transition temperature (T _{rm C}) with composition and processing conditions. The rm Bi_2(Sr,Ca) _3Cu_2O_{8+delta} crystallization experiments were supplemented by a series of similar experiments on the incongruently melting compound rm Ca_3Al_2O_6. The phase equilibria in the CaO-rm Al_2O _3 system has been thoroughly studied, and by analyzing the float-zone growth of this simpler and better-characterized material, it was verified that phase equilibria information and solidification behavior could be extracted from and explained by these solidification experiments. Two different types of nonplanar, crystal/melt interface morphologies were observed in the rm Ca_3Al_2O_6 experiments. Each reflected the influence of the phase equilibria in the CaO-rm Al_2O_3 system and component segregation in the melt. The molten zone compositions were found to approach those predicted by the CaO-rm Al_2O_3 phase diagram as the growth rate decreased, in accordance with the Burton-Prim Slichter relationship. Excellent agreement was obtained between actual phases found to coexist at the rm Ca_3Al_2O_6 /melt interface and the predictions of classical crystal growth theory. Based on the results of the rm Ca _3Al_2O_6 crystallization study, the crystal/melt equilibria in the far more complex rm Bi_2O_3-SrO-CaO-CuO system was evaluated by determining the phases formed during the superconductor growth experiments. The melt compositions were found to be rm Bi_2O_3 -rich and SrO-poor relative to the compositions of the 2212 crystals grown from them. The CaO and CuO segregation coefficients, on the other hand, were observed to be near unity. As one would expect for an incongruently -melting compound, segregation at the solidification front generally decreased with increasing crystallization temperature, but all the segregation coefficients were not observed to simultaneously approach unity. The superconducting transition temperatures (T _{rm C}'s) of six as-crystallized samples having homogeneous crystal compositions were also measured. Sample T_{rm C} was observed to increase with increasing growth temperature and, therefore, change with crystal composition. The results of this study suggested that it is desirable to grow crystals at the highest possible crystallization temperature since they will: (1) have the highest as-grown T_{rm C} 's, and (2) solidify with the least component segregation at the growth interface. In addition, the analysis presented here suggests that such growth is not recommended at higher growth rates, since crystals with mid-range solidus compositions (and consequently, moderate growth temperatures) should crystallize most reliably as single-phase samples at higher growth rates.

SuperCDMS Underground Detector Fabrication Facility

DOE Office of Scientific and Technical Information (OSTI.GOV)

Platt, M.; Mahapatra, R.; Bunker, Raymond A.

The SuperCDMS SNOLAB dark matter experiment processes Ge and Si crystals into fully tested phonon and ionization detectors at surface fabrication and test facilities. If not mitigated, it is anticipated that trace-level production of radioisotopes in the crystals due to exposure to cosmic rays at (or above) sea level will result in the dominant source of background events in future dark matter searches using the current SuperCDMS detector technology. Fabrication and testing of detectors in underground facilities shielded from cosmic radiation is one way to directly reduce production of trace levels of radioisotopes, thereby improving experimental sensitivity for the discoverymore » of dark matter beyond the level of the current experiment. In this report, we investigate the cost and feasibility to establish a complete detector fabrication processing chain in an underground location to mitigate cosmogenic activation of the Ge and Si detector substrates. For a specific and concrete evaluation, we explore options for such a facility located at SNOLAB, an underground laboratory in Sudbury, Canada hosting the current and future experimental phases of SuperCDMS.« less

Effect of Hydraulic Activity on Crystallization of Precipitated Calcium Carbonate (PCC) for Eco-Friendly Paper

PubMed Central

Kim, Jung-Ah; Han, Gi-Chun; Lim, Mihee; You, Kwang-Suk; Ryu, Miyoung; Ahn, Ji-Whan; Fujita, Toyohisa; Kim, Hwan

2009-01-01

Wt% of aragonite, a CaCO3 polymorph, increased with higher hydraulic activity (°C) of limestone in precipitated calcium carbonate (PCC) from the lime-soda process (Ca(OH)2-NaOH-Na2CO3). Only calcite, the most stable polymorph, was crystallized at hydraulic activity under 10 °C, whereas aragonite also started to crystallize over 10 °C. The crystallization of PCC is more dependent on the hydraulic activity of limestone than CaO content, a factor commonly used to classify limestone ores according to quality. The results could be effectively applied to the determination of polymorphs in synthetic PCC for eco-friendly paper manufacture. PMID:20087470

Effect of hydraulic activity on crystallization of precipitated calcium carbonate (PCC) for eco-friendly paper.

PubMed

Kim, Jung-Ah; Han, Gi-Chun; Lim, Mihee; You, Kwang-Suk; Ryu, Miyoung; Ahn, Ji-Whan; Fujita, Toyohisa; Kim, Hwan

2009-11-11

Wt% of aragonite, a CaCO(3) polymorph, increased with higher hydraulic activity ( degrees C) of limestone in precipitated calcium carbonate (PCC) from the lime-soda process (Ca(OH)(2)-NaOH-Na(2)CO(3)). Only calcite, the most stable polymorph, was crystallized at hydraulic activity under 10 degrees C, whereas aragonite also started to crystallize over 10 degrees C. The crystallization of PCC is more dependent on the hydraulic activity of limestone than CaO content, a factor commonly used to classify limestone ores according to quality. The results could be effectively applied to the determination of polymorphs in synthetic PCC for eco-friendly paper manufacture.

Crystal structure, electronic structure, optical and scintillation properties of self-activated Cs 4YbI 6 [Crystal structure, optical and scintillation properties of self-activated Cs 4YbI 6

DOE Office of Scientific and Technical Information (OSTI.GOV)

Wu, Yuntao; Chakoumakos, Bryan C.; Shi, Hongliang

A self-activated Cs 4YbI 6 single crystal was grown by the vertical Bridgman method. Crystal structure refinements verified the phase purity and the trigonal crystal system with a space group of more » $$\\bar{R}$$3 c. By using differential scanning calorimetry, the melting and crystallization points were determined to be 550 and 510 °C, respectively. Luminescence and scintillation properties were systematically studied. Upon ultraviolet light (360 nm) excitation, the Cs 4YbI 6 crystal exhibits bluish-green emission centered at 450 and 480 nm due to spin-allowed and spin-forbidden transitions of Yb 2+ activators. The lifetimes of the corresponding emission bands at room temperature are tens and hundreds of nanoseconds, respectively. X-ray excited radioluminescence spectrum is dominated by the spin-forbidden transition of Yb 2+ at 480 nm. The absolute light yield is 2700 ± 200 photons/MeV with a principal scintillation decay time of 33 ns. In conclusion, the physical explanation for the low light yield observed is proposed from experimental and theoretical insights.« less

Crystal structure, electronic structure, optical and scintillation properties of self-activated Cs 4YbI 6 [Crystal structure, optical and scintillation properties of self-activated Cs 4YbI 6

DOE PAGES

Wu, Yuntao; Chakoumakos, Bryan C.; Shi, Hongliang; ...

2018-05-14

A self-activated Cs 4YbI 6 single crystal was grown by the vertical Bridgman method. Crystal structure refinements verified the phase purity and the trigonal crystal system with a space group of more » $$\\bar{R}$$3 c. By using differential scanning calorimetry, the melting and crystallization points were determined to be 550 and 510 °C, respectively. Luminescence and scintillation properties were systematically studied. Upon ultraviolet light (360 nm) excitation, the Cs 4YbI 6 crystal exhibits bluish-green emission centered at 450 and 480 nm due to spin-allowed and spin-forbidden transitions of Yb 2+ activators. The lifetimes of the corresponding emission bands at room temperature are tens and hundreds of nanoseconds, respectively. X-ray excited radioluminescence spectrum is dominated by the spin-forbidden transition of Yb 2+ at 480 nm. The absolute light yield is 2700 ± 200 photons/MeV with a principal scintillation decay time of 33 ns. In conclusion, the physical explanation for the low light yield observed is proposed from experimental and theoretical insights.« less

Growth of Si spherical crystals and the surface oxidation (M-9)

NASA Technical Reports Server (NTRS)

Nishinaga, Tatau

1993-01-01

Nearly 90 percent of semiconductor devices are produced with Si single crystals as the starting materials. For instance, the integrated circuits (IC), which are used in almost all electronic equipments such as TV, tape recorders, audio amplifiers, etc., are made after various processings of Si single crystal wafers. In these wafers, the same controlled amounts of impurities are added and the uniformities in their distributions are extremely important. Growth under microgravity makes it possible to eliminate the buoyancy-driven convection in the melt, which is one of the main origins of convections which results in non-uniformity of the impurity. Another source of convection is known as Marangoni convection which is driven on the free surface when a temperature gradient occurs. One of the merits of microgravity experimentation is that the detailed study of this convection becomes possible. Another important advantage of microgravity is that growth of crystals without a crucible is possible. This makes it possible to study melt growth without the strain which is usually introduced on the ground. Nevertheless, we should repeat and analyze many growth experiments in space to get reliable results. However, since in the FMPT, the time for the experiment is limited, we plan to carry out two kinds of very simple and basic experiments as the first step for the semiconductor growth experiment. In the first experiment, we use single crystal Si sphere as the starting material and as shown, this sphere is heated in the furnace at a slightly higher temperature than the melting point. After the melting front moves nearly half way to its center, the temperature is decreased to stop the melting and to start the growth from the seed for which we use the unmelted solid party of the sphere. The sphere is centered by quartz protuberances inside of the quartz crucible. There exists the possibility of temperature fluctuations being introduced when the molten sphere occasionally touches the protuberances. The total time needed for the melting and the growth processes is estimated to be 30 minutes. Infrared emission from the sphere is monitored in order to prevent the accidental loss of the central solid core. The schematical illustration of the second experient is shown. A single crystal, Si rod is used as the starting material. In the first stage, the rod is melted from one end to obtain a liquid sphere. In the second stage, the single crystal is grown by decreasing the temperature from the unmelted part of the rod which is used as the seed. The second experient somewhat resembles the Czochralski method used on the ground; however, in the space experiment, no crucible is employed and the temperature uniformity is much superior. In both experiments, phosphorous is doped to allow observation of the change in the shape of the liquid solid interface during crystal growth and the impurity striations, if any.

The crystal structure of the AgamOBP1•Icaridin complex reveals alternative binding modes and stereo-selective repellent recognition.

PubMed

Drakou, Christina E; Tsitsanou, Katerina E; Potamitis, Constantinos; Fessas, Dimitrios; Zervou, Maria; Zographos, Spyros E

2017-01-01

Anopheles gambiae Odorant Binding Protein 1 in complex with the most widely used insect repellent DEET, was the first reported crystal structure of an olfactory macromolecule with a repellent, and paved the way for OBP1-structure-based approaches for discovery of new host-seeking disruptors. In this work, we performed STD-NMR experiments to directly monitor and verify the formation of a complex between AgamOBP1 and Icaridin, an efficient DEET alternative. Furthermore, Isothermal Titration Calorimetry experiments provided evidence for two Icaridin-binding sites with different affinities (Kd = 0.034 and 0.714 mM) and thermodynamic profiles of ligand binding. To elucidate the binding mode of Icaridin, the crystal structure of AgamOBP1•Icaridin complex was determined at 1.75 Å resolution. We found that Icaridin binds to the DEET-binding site in two distinct orientations and also to a novel binding site located at the C-terminal region. Importantly, only the most active 1R,2S-isomer of Icaridin's equimolar diastereoisomeric mixture binds to the AgamOBP1 crystal, providing structural evidence for the possible contribution of OBP1 to the stereoselectivity of Icaridin perception in mosquitoes. Structural analysis revealed two ensembles of conformations differing mainly in spatial arrangement of their sec-butyl moieties. Moreover, structural comparison with DEET indicates a common recognition mechanism for these structurally related repellents. Ligand interactions with both sites and binding modes were further confirmed by 2D 1 H- 15 N HSQC NMR spectroscopy. The identification of a novel repellent-binding site in AgamOBP1 and the observed structural conservation and stereoselectivity of its DEET/Icaridin-binding sites open new perspectives for the OBP1-structure-based discovery of next-generation insect repellents.

The Question of Impurities in Macromolecule Crystal Quality Improvement in Microgravity

NASA Technical Reports Server (NTRS)

Judge, Russell A.; Snell, Edward H.; Pusey, Marc L.; Sportiello, Michael G.; Todd, Paul; Bellamy, Henry; Borgstahl, Gloria E.; Pokros, Matthew; Cassanto, John M.

2000-01-01

While macromolecule impurities may affect crystal size and morphology the over-riding question is how do macromolecule impurities effect crystal X-ray quality and diffraction resolution. In the case of chicken egg white lysozyme previous researchers have reported that crystals grown in the presence of ovalbumin, ovotransferrin, and turkey egg white lysozyme show no difference in diffraction resolution compared to those grown in pure solutions. One impurity however, a naturally occurring lysozyme dimer, does negatively impact the X-ray crystal properties. For this impurity it has been reported that crystal quality improvement in microgravity may be due to improved impurity partitioning during crystallization. In this study we have examined the incorporation of the dimer into lysozyme crystals, both on the ground and in microgravity experiments, and have performed detailed X-ray analysis of the crystals using a new technique for finely probing the mosaicity of the crystal at the Stanford Synchrotron Radiation Laboratory. Dimer partitioning was not significantly different in microgravity compared to the ground based experiments, although it is significantly better than that previously reported in microgravity. Mosaicity analysis of pure crystals, 1422 indexed reflections (microgravity) and 752 indexed reflections (ground), gave average results of 0.0066 and 0.0092 degrees (FWHM) respectively. The microgravity crystals also provided an increased signal to noise. Dimer incorporation increased the average mosaicity in microgravity but not on the ground. However, dimer incorporation did greatly reduce the resolution limit in both ground and microgravity grown crystals. The data is being treated anisotropically to explore these effects. These results indicate that impurity effects in microgravity are complex and that the conditions or techniques employed may greatly affect the role of impurities.

Flight Day 2 Highlights

NASA Technical Reports Server (NTRS)

2003-01-01

The STS-107 second flight day begins with a shot of the Spacehab Research Double Module. Live presentations of experiments underway inside of the Spacehab Module are presented. Six experiments are shown. As part of the Space Technology and Research Student Payload, students from Australia, China, Israel, Japan, New York, and Liechtenstein are studying the effect that microgravity has on ants, spiders, silkworms, fish, bees, granular materials, and crystals. Mission Specialist Kalpana Chawla is seen working with the zeolite crystal growth experiment.

Decompression Induced Crystallization of Basaltic Andesite Magma: Constraints on the Eruption of Arenal Volcano, Costa Rica.

NASA Astrophysics Data System (ADS)

Szramek, L. A.; Gardner, J. E.; Larsen, J. F.

2004-12-01

Arenal Volcano is a small stratovolcano located 90 km NW of San Jose, Costa Rica. In 1968 current activity began with a Plinian phase, and has continued to erupt lava flows and pyroclastic flows intermittently since. Samples from the Plinian, pyroclastic flow, strombolian, and effusive phases have been studied texturally. Little variation in crystallinity occurs amongst the different phases. Number density of crystals, both 2D and 3D are 50-70 mm-2 and 30,000-50,000 mm-3 in the Plinian sample, compared to the lesser values in other eruptive types. Characteristic crystal size also increases as explosivity decreases. Two samples, both lava flows collected while warm, overlap with the Plinian sample. This suggests that the variations seen may be a result of cooling history. Plagioclase differs between the Plinian sample, in which they are only tabular in shape, and the other eruptive types, which contain both tabular and equant crystals. To link decompression paths of the Arenal magma to possible pre-eruptive conditions, we have carried out hydrothermal experiments. The experiments were preformed in TZM pressure vessels buffered at a fugacity of Ni-NiO and water saturation. Phase equilibria results in conjunction with mineral compositions and temperature estimates by previous workers from active lava flows and two-pyroxene geothermometry, constrain the likely pre-eruptive conditions for the Arenal magma to 950-1040° C with a water pressure of 50-80 MPa. Samples that started from conditions that bracket our estimated pre-eruptive conditions were decompressed in steps of 5-30 MPa and held for various times at each step until 20 MPa was reached, approximating average decompression rates of 0.25, 0.025, 0.0013 MPa/s. Comparison of textures found in the natural samples to the experimentally produced textures suggest that the Plinian eruption likely was fed by magma ascending at 0.05-1 m/s, whereas the less explosive phases were fed by magma ascending at 0.05 m/s or less.

Crystal growth and electrical properties of CuFeO 2 single crystals

NASA Astrophysics Data System (ADS)

Dordor, P.; Chaminade, J. P.; Wichainchai, A.; Marquestaut, E.; Doumerc, J. P.; Pouchard, M.; Hagenmuller, P.; Ammar, A.

1988-07-01

Delafossite-type CuFeO 2 single crystals have been prepared by a flux method: crystals obtained in a Cu crucible with LiBO 2 as flux are n-type whereas those prepared in a Pt crucible with a Cu 2O flux are p-type. Electrical measurements have revealed that n-type crystals exhibit weak anisotropic conductivities with large activation energies and small mobilities (r.t. values perpendicular and parallel to the c-axis: μ⊥ = 5 × 10 -5 and μ‖ = 10 -7 cm -2 V -1 sec -1). p-type crystals, less anisotropic, are characterized by low activation energies and higher mobilities ( μ⊥ = 34 and μ‖ = 8.9 cm 2 V -1 sec -1). A two -conduction-band model is proposed to account for the difference observed between the energy gap value deduced from photoelectrochemical measurements and the activation energy of the electrical conductivity in the intrinsic domain.

Single crystal diamond membranes for nanoelectronics.

PubMed

Bray, Kerem; Kato, Hiromitsu; Previdi, Rodolfo; Sandstrom, Russell; Ganesan, Kumaravelu; Ogura, Masahiko; Makino, Toshiharu; Yamasaki, Satoshi; Magyar, Andrew P; Toth, Milos; Aharonovich, Igor

2018-02-22

Single crystal, nanoscale diamond membranes are highly sought after for a variety of applications including nanophotonics, nanoelectronics and quantum information science. However, so far, the availability of conductive diamond membranes has remained an unreachable goal. In this work we present a complete nanofabrication methodology for engineering high aspect ratio, electrically active single crystal diamond membranes. The membranes have large lateral directions, exceeding ∼500 × 500 μm 2 and are only several hundreds of nanometers thick. We further realize vertical single crystal p-n junctions made from the diamond membranes that exhibit onset voltages of ∼10 V and a current of several mA. Moreover, we deterministically introduce optically active color centers into the membranes, and demonstrate for the first time a single crystal nanoscale diamond LED. The robust and scalable approach to engineer the electrically active single crystal diamond membranes offers new pathways for advanced nanophotonic, nanoelectronic and optomechanical devices employing diamond.

New XAFS Facility for In-Situ Measurements at Beamline C at HASYLAB

DOE Office of Scientific and Technical Information (OSTI.GOV)

Rickers, K.; Drube, W.; Schulte-Schrepping, H.

2007-02-02

A XAFS-experiment allowing for in-situ experiments has been set up at DORIS bending magnet beamline C. For that purpose, a new double-crystal, UHV-compatible monochromator with fast scanning capability was designed. This fixed-exit monochromator uses two crystal sets on a common central rotation axis driven by an ex-vacuo goniometer. Bragg angles range from 5 deg. to 55.5 deg. resulting in a total energy range 2.3 - 43.4 keV using Si(111)/(311) crystal sets. Crystal pairs can be remotely selected by translating the vacuum chamber. Energy encoding is performed using an optical encoder system. The standard XAFS sample environment is set-up in vacuomore » and can be adapted for special sample environments. For in-situ experiments, the beamline is equipped with twelve gas lines. An exhaust line allows toxic/reactive gases to be handled. As an initial performance test of the instrument, Ti, Cr, Fe and Cu XAFS and Ce K-shell QEXAFS measurements were performed.« less

Experiments with crystal deflectors for high energy ion beams: Electromagnetic dissociation probability for well channeled ions

NASA Astrophysics Data System (ADS)

Scandale, W.; Taratin, A. M.; Kovalenko, A. D.

2013-01-01

The paper presents the current status with the use of the crystal defectors for high energy ion beams. The channeling properties of multicharged ions are discussed. The results of the experiments on the deflection and extraction (collimation) of high energy ion beams with bent crystals performed in the accelerator centers are shortly considered. The analysis of the recent collimation experiment with a Pb nuclei of 270GeV/c per charge at the CERN Super Proton Synchrotron showed that the channeling efficiency was as large as about 90%. For Pb ions of the LHC energies a new mechanism, which can reduce the channeling efficiency, appears. The electromagnetic dissociation (ED) becomes possible for well channeled particles. However, the estimations performed in the paper show that the ED probability is small and should not visibly reduce the collimation efficiency. On the other hand, the aligned crystal gives the possibility to study the ED processes of heavy nuclei in the conditions when nuclear interactions are fully suppressed.

Direct observation of interface instability during crystal growth

NASA Technical Reports Server (NTRS)

Tiller, W. A.; Feigelson, R. S.; Elwell, D.

1982-01-01

The general aim of this investigation was to study interface stability and solute segregation phenomena during crystallization of a model system. Emphasis was to be placed on direct observational studies partly because this offered the possibility at a later stage of performing related experiments under substantially convection-free conditions in the space shuttle. The major achievements described in this report are: (1) the development of a new model system for fundamental studies of crystal growth from the melt and the measurement of a range of material parameters necessary for comparison of experiment with theory. (2) The introduction of a new method of measuring segregation coefficient using absorption of a laser beam by the liquid phase. (3) The comparison of segregation in crystals grown by gradient freezing and by pulling from the melt. (4) The introduction into the theory of solute segregation of an interface field term and comparison with experiment. (5) The introduction of the interface field term into the theories of constitutional supercooling and morphological stability and assessment of its importance.

Observations on the crystallization of spodumene from aqueous solutions in a hydrothermal diamond-anvil cell

USGS Publications Warehouse

Li, Jianking; Chou, I-Ming; Yuan, Shunda; Burruss, Robert A.

2013-01-01

Crystallization experiments were conducted in a new type of hydrothermal diamond-anvil cell (HDAC; type V) using LiAlSi2O6 (S) gel and H2O (W) as starting materials. A total of 21 experiments were performed at temperatures up to 950°C and pressures up to 788 MPa. In the samples with relatively low W/S ratios, many small crystals formed in the melt phase during cooling. In those with high W/S ratios, only a few crystals with smooth surfaces crystallized from the aqueous fluid in the presence of melt droplets, which were gradually consumed during crystal growth, indicating rapid transfer of material from the melt to the crystals through the aqueous fluid. The nucleation of crystals started at 710 (±70)°C and 520 (±80) MPa, and crystal growth ended at 570 (±40)°C and 320 (±90) MPa, with the cooling P-T path within the stability field of spodumene + quartz in the S-W system. The observed linear crystal growth rates in the aqueous phase, calculated by dividing the maximum length of a single crystal by the duration of the entire growth step, were 4.7 × 10−6 and 5.7 × 10−6 cm s−1 for the cooling rates of 0.5 and 1°C min−1, respectively. However, a rapid crystal growth rate of 3.6 × 10−5 cm s−1 in the aqueous fluid was observed when the components were supplied by nearby melt droplets. Our results show that when crystals nucleate in the aqueous fluid instead of the melt phase, there are fewer nuclei formed, and they grow much faster due to the low viscosity of the aqueous fluid, which accelerates diffusion of components for the growth of crystals. Therefore, the large crystals in granitic pegmatite can crystallize directly from aqueous fluids rather than hydrosilicate melt.

The release of trapped gases from amorphous solid water films. I. "Top-down" crystallization-induced crack propagation probed using the molecular volcano.

PubMed

May, R Alan; Smith, R Scott; Kay, Bruce D

2013-03-14

In this (Paper I) and the companion paper (Paper II; R. May, R. Smith, and B. Kay, J. Chem. Phys. 138, 104502 (2013)), we investigate the mechanisms for the release of trapped gases from underneath amorphous solid water (ASW) films. In prior work, we reported the episodic release of trapped gases in concert with the crystallization of ASW, a phenomenon that we termed the "molecular volcano." The observed abrupt desorption is due to the formation of cracks that span the film to form a connected pathway for release. In this paper, we utilize the "molecular volcano" desorption peak to characterize the formation of crystallization-induced cracks. We find that the crack length distribution is independent of the trapped gas (Ar, Kr, Xe, CH4, N2, O2, or CO). Selective placement of the inert gas layer is used to show that cracks form near the top of the film and propagate downward into the film. Isothermal experiments reveal that, after some induction time, cracks propagate linearly in time with an Arrhenius dependent velocity corresponding to an activation energy of 54 kJ∕mol. This value is consistent with the crystallization growth rates reported by others and establishes a direct connection between crystallization growth rate and the crack propagation rate. A two-step model in which nucleation and crystallization occurs in an induction zone near the top of the film followed by the propagation of a crystallization∕crack front into the film is in good agreement with the temperature programmed desorption results.

JTEC panel on display technologies in Japan

NASA Technical Reports Server (NTRS)

Tannas, Lawrence E., Jr.; Glenn, William E.; Credelle, Thomas; Doane, J. William; Firester, Arthur H.; Thompson, Malcolm

1992-01-01

This report is one in a series of reports that describes research and development efforts in Japan in the area of display technologies. The following are included in this report: flat panel displays (technical findings, liquid crystal display development and production, large flat panel displays (FPD's), electroluminescent displays and plasma panels, infrastructure in Japan's FPD industry, market and projected sales, and new a-Si active matrix liquid crystal display (AMLCD) factory); materials for flat panel displays (liquid crystal materials, and light-emissive display materials); manufacturing and infrastructure of active matrix liquid crystal displays (manufacturing logistics and equipment); passive matrix liquid crystal displays (LCD basics, twisted nematics LCD's, supertwisted nematic LCD's, ferroelectric LCD's, and a comparison of passive matrix LCD technology); active matrix technology (basic active matrix technology, investment environment, amorphous silicon, polysilicon, and commercial products and prototypes); and projection displays (comparison of Japanese and U.S. display research, and technical evaluation of work).

Growth, Characterization and Applications of Beta-Barium Borate and Related Crystals

DTIC Science & Technology

1993-10-31

Crystal symmetry determines the form of the second order polarization tensor. The second order polarizability tensor is defined by the piezoelectric...cold finger. A temperature oscillation technique1 I was used to limit the number of nuclei formed . These experiments typically yielded thin crystal...statistically sampled to determine the optimal seeding orientation. % was reasoned that the large crystal plates were formed from nucleii which had a favorable

Preliminary experiments on phase conjugation for flow visualization. [barium titanate single crystals

NASA Technical Reports Server (NTRS)

Weimer, D.; Howes, W. L.

1984-01-01

Barium titanate single crystals are discussed in the context of: the procedure for polarizing a crystal; a test for phase conjugation; transients in the production of phase conjugation; real time readout by a separate laser of a hologram induced within the crystal, including conjugation response times to on-off switching of each beam; and a demonstration of a Twyman-Green interferometer utilizing phase conjugation.

Effects of Gravity on Processing Heavy Metal Fluoride Fibers

NASA Technical Reports Server (NTRS)

Tucker, Dennis S.; Workman, Gary L.; Smith, Guy A.

1997-01-01

The effects of gravity on the crystal nucleation of heavy metal fluoride fibers have been studied in preliminary experiments utilizing NASA's KC-135 reduced gravity aircraft and a microgravity sounding rocket flight. Commercially produced fibers were heated to the crystallization temperature in normal and reduced gravity. The fibers processed in normal gravity showed complete crystallization while the fibers processed in reduced gravity did not show signs of crystallization.

DHS Internship Summary-Crystal Assembly at Different Length Scales

DOE Office of Scientific and Technical Information (OSTI.GOV)

Mishchenko, L

2009-08-06

I was part of a project in which in situ atomic force microscopy (AFM) was used to monitor growth and dissolution of atomic and colloidal crystals. At both length scales, the chemical environment of the system greatly altered crystal growth and dissolution. Calcium phosphate was used as a model system for atomic crystals. A dissolution-reprecipitation reaction was observed in this first system, involving the conversion of brushite (DCPD) to octacalcium phosphate (OCP). In the second system, polymeric colloidal crystals were dissolved in an ionic solvent, revealing the underlying structure of the crystal. The dissolved crystal was then regrown through anmore » evaporative step method. Recently, we have also found that colloids can be reversibly deposited in situ onto an ITO (indium tin oxide) substrate via an electrochemistry setup. The overall goal of this project was to develop an understanding of the mechanisms that control crystallization and order, so that these might be controlled during material synthesis. Controlled assembly of materials over a range of length scales from molecules to nanoparticles to colloids is critical for designing new materials. In particular, developing materials for sensor applications with tailorable properties and long range order is important. In this work, we examine two of these length scales: small molecule crystallization of calcium phosphate (whose crystal phases include DCPD, OCP, and HAP) and colloidal crystallization of Poly(methyl methacrylate) beads. Atomic Force Microscopy is ideal for this line of work because it allows for the possibility of observing non-conducting samples in fluid during growth with high resolution ({approx} 10 nm). In fact, during atomic crystal growth one can observe changes in atomic steps, and with colloidal crystals, one can monitor the individual building blocks of the crystal. Colloids and atoms crystallize under the influence of different forces acting at different length scales as seen in Table 1. In particular, molecular crystals, which are typically dominated by ionic and covalent bonding, are an order of magnitude more strongly bonded than colloidal crystals. In molecular crystals, ordering is driven by the interaction potentials between molecules. By contrast, colloidal assembly is a competition between the repulsive electrostatic forces that prevent aggregation in solution (due to surface charge), and short-range van der Waals and entropic forces that leads to ordering. Understanding atomic crystallization is fundamentally important for fabrication of tailorable crystalline materials, for example for biological or chemical sensors. The transformation of brushite to OCP not only serves as a model system for atomic crystal growth (applicable to many other crystal growth processes), but is also important in bone cements. Colloidal crystals have unique optical properties which respond to chemical and mechanical stimuli, making them very important for sensing applications. The mechanism of colloidal crystal assembly is thus fundamentally important. Our in situ dissolution and regrowth experiments are one good method of analyzing how these crystals pack under different conditions and how defect sites are formed and filled. In these experiments, a silica additive was used to strengthen the colloidal crystal during initial assembly (ex situ) and to increase domain size and long range order. Reversible electrodeposition of colloids onto a conductive substrate (ITO in our case) is another system which can further our knowledge of colloidal assembly. This experiment holds promise of allowing in situ observation of colloidal crystal growth and the influence of certain additives on crystal order. The ultimate goal would be to achieve long range order in these crystals by changing the surface charge or the growth environment.« less

Preliminary crystallographic studies of four crystal forms of serum albumin

NASA Technical Reports Server (NTRS)

Carter, D. C.; Chang, B.; Ho, J. X.; Keeling, K.; Krishnasami, Z.

1994-01-01

Several crystal forms of serum albumin suitable for three-dimensional structure determination have been grown. These forms include crystals of recombinant and wild-type human serum albumin, baboon serum albumin, and canine serum albumin. The intrinsic limits of X-ray diffraction for these crystals are in the range 0.28-0.22 nm. Two of the crystal forms produced from human and canine albumin include incorporated long-chain fatty acids. Molecular replacement experiments have been successfully conducted on each crystal form using the previously determined atomic coordinates of human serum albumin illustrating the conserved tertiary structure.

Practical physics behind growing crystals of biological macromolecules.

PubMed

Candoni, Nadine; Grossier, Romain; Hammadi, Zoubida; Morin, Roger; Veesler, Stéphane

2012-07-01

The aim of this review is to provide biocrystallographers who intend to tackle protein-crystallization with theory and practical examples. Crystallization involves two separate processes, nucleation and growth, which are rarely completely unconnected. Here we give theoretical background and concrete examples illustrating protein crystallization. We describe the nucleation of a new phase, solid or liquid, and the growth and transformation of existing crystals obtained by primary or secondary nucleation or by seeding. Above all, we believe that a thorough knowledge of the phase diagram is vital to the selection of starting position and path for any crystallization experiment.

Crystallization of Spätzle, a cystine-knot protein involved in embryonic development and innate immunity in Drosophila melanogaster

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hoffmann, Anita; Neumann, Piotr; Schierhorn, Angelika

2008-08-01

Crystallization of the cystine-knot protein Spätzle occurred following serendipitous limited degradation of the pro-Spätzle propeptide during the crystallization experiment. The Spätzle protein is involved in both the definition of the dorsal–ventral axis during embryonic development and in the adult innate immune response. The disulfide-linked dimeric cystine-knot protein has been expressed as a proprotein in inclusion bodies in Escherichia coli and refolded in vitro by rapid dilution. Initial orthorhombic crystals that diffracted to 7 Å resolution were obtained after three months by the sitting-drop vapour-diffusion method. Optimization of the crystallization conditions resulted in orthorhombic crystals (space group P2{sub 1}2{sub 1}2{sub 1},more » with unit-cell parameters a = 53.0, b = 59.2, c = 62.5 Å) that diffracted to 2.8 Å resolution in-house. The small volume of the asymmetric unit indicated that it was not possible for the crystals to contain the complete pro-Spätzle dimer. Mass spectrometry, N-terminal sequencing and Western-blot analysis revealed that the crystals contained the C-terminal disulfide-linked cystine-knot dimer. Comparison of various crystallization experiments indicated that degradation of the N-terminal prodomain was dependent on the buffer conditions.« less

Research experiences on materials science in space aboard Salyut and Mir

NASA Technical Reports Server (NTRS)

Regel, Liya L.

1992-01-01

From 1980 through 1991 approximately 500 materials processing experiments were performed aboard the space stations Salyut 6, Salyut 7 and Mir. This includes work on catalysts, polymers, metals and alloys, optical materials, superconductors, electronic crystals, thin film semiconductors, super ionic crystals, ceramics, and protein crystals. Often the resulting materials were surprisingly superior to those prepared on earth. The Soviets were the first to fabricate a laser (CdS) from a crystal grown in space, the first to grow a heterostructure in space, the first super ionic crystal in space, the first crystals of CdTe and its alloys, the first zeolite crystals, the first protein crystals, the first chromium disilicide glass, etc. The results were used to optimize terrestrial materials processing operations in Soviet industry. The characteristics of these three space stations are reviewed, along with the advantages of a space station for materials research, and the problems encountered by the materials scientists who used them. For example, the stations and the materials processing equipment were designed without significant input from the scientific community that would be using them. It is pointed out that successful results have been achieved also by materials processing at high gravity in large centrifuges. This research is also continuing around the world, including at Clarkson University. It is recommended that experiments be conducted in centrifuges in space, in order to investigate the acceleration regime between earth's gravity and the microgravity achieved in orbiting space stations. One cannot expect to understand the influence of gravity on materials processing from only two data points, earth's gravity and microgravity. One must also understand the influence of fluctuations in acceleration on board space stations, the so-called 'g-jitter.' This paper is presented in outline and graphical form.