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All sourcesNASA NTRSDOE OSTI
NASA NTRS1998

The Effect of Protein Impurities on Lysozyme Crystal Growth

While bulk crystallization from impure solutions is used industrially as a purification step for a wide variety of materials, it is a technique that has rarely been used for proteins. Proteins have a reputation for being difficult to crystallize and high purity of the initial crystallization solution is considered paramount for success in the crystallization. Although little is written on the purifying capability of protein crystallization or of the effect of impurities on the various aspects of the crystallization process, recent published reports show that crystallization shows promise and feasibility as a purification technique for proteins. In order to further examine the issue of purity in macromolecule crystallization this study investigates the effect of the protein impurities, avidin, ovalbumin and conalbumin, at concentrations up to 50%, on the solubility, crystal face growth rates and crystal purity, of the protein lysozyme. Solubility was measured in batch experiments while a computer controlled video microscope system was used to measure the f {101} and {101} lysozyme crystal face growth rates. While little effect was observed on solubility and high crystal purity was obtained (>99.99%), the effect of the impurities on the face growth rates varied from no effect to a significant face specific effect leading to growth cessation, a phenomenon that is frequently observed in protein crystal growth. The results shed interesting light on the effect of protein impurities on protein crystal growth and strengthen the feasibility of using crystallization as a unit operation for protein purification.

Judge, Russell A.↗
NASA NTRS2000

The Effect of Hydrogen Annealing on the Impurity Content of Alumina-Forming Alloys

Previously, the effect of hydrogen annealing on increasing the adhesion of Al2O3 scales had been related to the effective desulfurization that occurred during this process. The simultaneous reduction of other impurities has now been re-examined for up to 20 impurity elements in the case of five different alloys (NiCrAl, FeCrAl, PWA 1480, Rene'142, and Rene'N5). Hydrogen annealing produced measurable reductions in elemental concentration for B, C, Na, Mg, P, K, Sr, or Sn in varying degrees for at least one and up to three of these alloys. No single element was reduced by hydrogen annealing for all the alloys except sulfur. In many cases spalling occurred at low levels of these other impurities, while in other cases the scales were adherent at high levels of the impurities. No impurity besides sulfur was strongly correlated with adhesion.

Smialek, James L.↗
NASA NTRS2000

Protein Crystal Growth Dynamics and Impurity Incorporation

The general concepts and theories of crystal growth are proven to work for biomolecular crystallization. This allowed us to extract basic parameters controlling growth kinetics - free surface energy, alpha, and kinetic coefficient, beta, for steps. Surface energy per molecular site in thermal units, alpha(omega)(sup 2/3)/kT approx. = 1, is close to the one for inorganic crystals in solution (omega is the specific molecular volume, T is the temperature). Entropic restrictions on incorporation of biomolecules into the lattice reduce the incorporation rate, beta, by a factor of 10(exp 2) - 10(exp 3) relative to inorganic crystals. A dehydration barrier of approx. 18kcal/mol may explain approx. 10(exp -6) times difference between frequencies of adding a molecule to the lattice and Brownian attempts to do so. The latter was obtained from AFM measurements of step and kink growth rates on orthorhombic lysozyme. Protein and many inorganic crystals typically do not belong to the Kossel type, thus requiring a theory to account for inequivalent molecular positions within its unit cell. Orthorhombic lysozyme will serve as an example of how to develop such a theory. Factors deteriorating crystal quality - stress and strain, mosaicity, molecular disorder - will be reviewed with emphasis on impurities. Dimers in ferritin and lysozyme and acetylated lysozyme, are microheterogeneous i.e. nearly isomorphic impurities that are shown to be preferentially trapped by tetragonal lysozyme and ferritin crystals, respectively. The distribution coefficient, K defined as a ratio of the (impurity/protein) ratios in crystal and in solution is a measure of trapping. For acetylated lysoyzme, K = 2.15 or, 3.42 for differently acetylated forms, is independent of both the impurity and the crystallizing protein concentration. The reason is that impurity flux to the surface is constant while the growth rate rises with supersaturation. About 3 times lower dimer concentration in space grown ferritin and lysozyme crystals might be examples explaining higher quality of the space grown protein crystal. Depletion of solution with respect to isomorphic impurities around a growing crystal may be K times deeper than with respect to the crystallizing protein.

Chernov, Alex A.↗
NASA NTRS2005

Impurity Studies of Cd(0.8)Zn(0.2)Te Crystals Using Photoluminescence and Glow Discharge Mass Spectroscopy

Cd(1-x)Zn(x)Te semiconductor crystal is a highly promising material for room temperature x- and gamma-ray detector applications because of its high resistivity, long carrier lifetime, and relatively high hole and electron mobilities. This paper reports the investigation of the impurities in several Cd(1-x)Zn(x)Te (x = 0.20) crystals grown using the vertical Bridgman method under a Cd overpressure. The impurity concentrations were measured using glow discharge mass spectroscopy (GDMS). The energy states of the impurities were studied using photoluminescence (PL) spectroscopy at liquid helium temperature. The PL spectra showed a series of sharp high energy lines which are associated with free excitons and excitons bound to impurities as donors and acceptors in the crystals. The impurities also contributed to donor-acceptor pair recombination. The correlation between the GDMS and PL results will be reported.

Su, Ching-Hua↗
NASA NTRS2004

Reference standard for carbonaceous impurity measurements in carbon nanotubes

Near-infrared spectroscopy is a convenient tool for measuring nanotube / carbonaceous impurities ratios in carbon nanotube samples. These measurements are based on separation of contributions from nanotubes and impurities to the near-infrared absorption of samples dispersed in DMF, and sample purity is expressed relative to some reference sample. In the current work we produced a reference standard for NIR measurements using purified laser nanotubes. The sample was oxidized slowly using a Temperature Programmed Oxidation (TPO) setup in 2% oxygen / 98 % helium atmosphere. In these conditions, the sample oxidized in several steps, which were attributed to carbonaceous impurities, nanotubes and graphitic shells based on TEM and Raman observations. Stopping oxidation at 625 C (this temperature is sample-specific) allowed us to produce a sample with no carbonaceous impurities and well-defined ratio of nanotubes, graphite and metal catalyst. Since carbonaceous impurities no longer hold nanotubes and particles together, further centrifuging allowed us to remove particles and use this sample as a reference standard in NIR measurements.

Nikolaev, Pavel↗
NASA NTRS2004

Reference standard for carbonaceous impurity measurements in carbon nanotubes.

Near-infrared spectroscopy is a convenient tool for measuring nanotube/carbonaceous impurities ratios in carbon nanotube samples. These measurements are based on separation of contributions from nanotubes and impurities to the near-infrared absorption of samples dispersed in DMF, and sample purity is expressed relative to some reference sample. In the current work we produced a reference standard for NIR measurements using purified laser nanotubes. The sample was oxidized slowly using a Temperature Programmed Oxidation (TPO) setup in 2% oxygen/98% helium atmosphere. In these conditions, the sample oxidized in several steps, which were attributed to carbonaceous impurities, nanotubes and graphitic shells based on TEM and Raman observations. Stopping oxidation at 625 C (this temperature is sample-specific) allowed us to produce a sample with no carbonaceous impurities and well-defined ratio of nanotubes, graphite and metal catalyst. Since carbonaceous impurities no longer hold nanotubes and particles together, further centrifuging allowed us to remove particles and use this sample as a reference standard in NIR measurements.

Nikolaev, Pavel↗
NASA NTRS1974

The effect of Be/+/ ion implanted exponential and uniform impurity profiles on the electrical characteristics of GaAs solar cells

The high surface recombination velocity is the major deterrent to obtaining efficient GaAs solar cells. If, however, an electric field is built in at the surface, the carriers will be swept away from the surface thus minimizing the surface recombination velocity problem. It has been previously shown theoretically that an exponential impurity distribution in the doped region of the cell results in a built-in electric field. Ion implantation was used to produce solar cells with an exponential impurity profile and cells with uniform profiles. It is shown that cells with an exponential impurity profile have higher open-circuit voltage, fill factors, and spectral response than those with a uniform impurity profile.

Vaidyanathan, K. V.↗
NASA NTRS1977

Oxygen impurity radiation from Tokamak-like plasmas

We have constructed a nonhydrodynamic coronal model for calculating radiation from impurity atoms in a heated plasma. Some recent developments in the calculation of dielectronic recombination rate coefficients and collisional excitation rate coefficients are included. The model is applied to oxygen impurity radiation during the first few milliseconds of a TFR Tokamak plasma discharge, and good agreement with experimental results is obtained. Estimates of total line and continuum radiation from the oxygen impurity are given. It is shown that impurity radiation represents a considerable energy loss.

Rogerson, J. E.↗
NASA NTRS1979

Analysis of the Effects of Impurities in Silicon

A solar cell fabrication and analysis program to determine the effects on the resultant solar cell efficiency of impurities incorporated into silicon is conducted. Flight quality technologies and quality assurance are employed to assure that variations in cell performance are due to the impurities incorporated in the silicon. The type and level of impurity doping in each test lot is given and the mechanism responsible for the degradation of cell performance is identified and correlated to the doped impurities.

Wohlgemuth, J. H.↗
NASA NTRS1980

Impurities in silicon solar cells

The paper investigates the effects of metallic impurities on the performance of silicon solar cells. Czochralski and polycrystalline ingots were employed with boron and phosphorus as primary dopants and with controlled additions of secondary impurities. The data obtained from over 200 crystals indicate that impurity-induced performance loss is primarily due to a reduction of the base diffusion length. Based on this observation, a model is developed which predicts cell performance as a function of secondary impurity concentrations. The model calculations are in good agreement with experimental values except for Cu, Ni, Fe, and to a lesser degree, carbon, which at higher concentrations degrade the cell by junction defect mechanisms.

Davis, J. R., Jr.↗
NASA NTRS1988

Influence of substrate misorientation on defect and impurity incorporation in GaAs/AlGaAs heterostructures grown by molecular-beam epitaxy

GaAS/AlGaAs heterostructures have been grown by molecular-beam epitaxy on GaAs substrates intentionally oriented (tilted) a few degrees (0-6.5) off the (001) plane towards either (111)A, (111)B, or (011). It was observed that the 4-K photoluminescence and low-field electron transport properties of these structures may be functions of the substrate tilt angle and tilt direction, depending on the concentration of impurities incorporated during growth. A substrate tilt during molecular-beam epitaxy is observed to have the largest effect on these properties when the background impurity concentration in the molecular-beam epitaxial machine is high. This supports the contention that the observed changes in material characteristics are due to differences in the incorporation of defects and impurities. The incorporation of defects and impurities are reduced by using substrates tilted toward (111)A, in comparison to nominally flat (001) substrates or substrates tilted toward (111)B.

Radulescu, D. C.↗
NASA NTRS1998

Effects of Convective Solute and Impurity Transport in Protein Crystal Growth

High-resolution optical interferometry was used to investigate the effects of forced solution convection on the crystal growth kinetics of the model protein lysozyme. Most experiments were conducted with 99.99% pure protein solutions. To study impurity effects, approx. 1% of lysozyme dimer (covalently bound) was added in some cases. We show that the unsteady kinetics, corresponding to bunching of growth steps, can be characterized by the Fourier components of time traces of the growth rate. Specific Fourier spectra are uniquely determined by the solution conditions (composition, temperature, and flow rate) and the growth layer source activity. We found that the average step velocity and growth rate increase by approx. I0% with increasing flow rate, as a result of the enhanced solute supply to the interface. More importantly, faster convective transport results in lower fluctuation amplitudes. This observation supports our rationale for system-dependent effects of transport on the structural perfection of protein crystals. We also found that solution flow rates greater than 500 microns/s result in stronger fluctuations while the average growth rate is decreased. This can lead to growth cessation at low supersaturations. With the intentionally contaminated solutions, these undesirable phenomena occurred at about half the flow rates required in pure solutions. Thus, we conclude that they are due to enhanced convective supply of impurities that are incorporated into the crystal during growth. Furthermore, we found that the impurity effects are reduced at higher crystal growth rates. Since the exposure time of terraces is inversely proportional to the growth rate, this observation suggests that the increased kinetics instability results from impurity adsorption on the interface. Finally, we provide evidence relating earlier observations of "slow protein crystal growth kinetics" to step bunch formation in response to nonsteady step generation.

Vekilov, Peter G.↗
NASA NTRS1996

Repartitioning of NaCl and Protein Impurities in Lysozyme Crystallization

Nonuniform precipitant and impurity incorporation in protein crystals can cause lattice strain and, thus, possibly decrease the X-ray diffraction resolution. To address this issue, a series of crystallization experiments were carried out, in which initial supersaturation, NaCl concentration, protein purity level and crystallized fraction were varied. Lysozyme and protein impurities, as well as sodium and chloride were independently determined in the initial solution, supernatant and crystals. The segregation coefficients for Na(+) and Cl(-) were found to be independent of supersaturation and NaCl concentration, and decreased with crystallized fraction/crystal size. Numerical evaluation of the extensive body of data, based on a nucleation-growth- repartitioning model, suggests a core of approx. 40 microns in which salt is incorporated in much greater concentrations than during later growth. Small crystals containing higher amounts of incorporated NaCl also had higher protein impurity contents. This suggests that the excess salt is associated with the protein impurities in the core. X-ray topography revealed strain fields in the center of the crystals comparable in size to the inferred core. The growth rates of crystals smaller than 30-40 pm in size were consistently 1.5-2 times lower than those of larger crystals, presumably due to higher chemical potentials in the core.

Vekilov, Peter G.↗
NASA NTRS2001

Investigating the Effect of Impurities on Macromolecule Crystal Growth in Microgravity

Chicken egg-white lysozyme (CEWL) crystals were grown in microgravity and on the ground in the presence of various amounts of a naturally occurring lysozyme dimer impurity. No significant favorable differences in impurity incorporation between microgravity and ground crystal samples were observed. At low impurity concentration the microgravity crystals preferentially incorporated the dimer. The presence of the dimer in the crystallization solutions in microgravity reduced crystal size, increased mosaicity and reduced the signal to noise ratio of the X-ray data. Microgravity samples proved more sensitive to impurity. Accurate indexing of the reflections proved critical to the X-ray analysis. The largest crystals with the best X-ray diffraction properties were grown from pure solution in microgravity.

Snell, Edward H.↗
NASA NTRS2014

The GOddard SnoW Impurity Module (GOSWIM) for the NASA GEOS-5 Earth System Model: Preliminary Comparisons with Observations in Sapporo, Japan

The snow darkening module evaluating dust, black carbon, and organic carbon depositions on mass and albedo has been developed for the NASA Goddard Earth Observing System, Version 5 (GEOS-5) Earth System Model, as the GOddard SnoW Impurity Module (GOSWIM). GOSWIM consists of the snow albedo scheme from a previous study (Yasunari et al. 2011) with updates and a newly developed mass concentration scheme, using aerosol depositions from the chemical transport model (GOCART) in GEOS-5. Compared to observations at Sapporo, the numerical experiments, forced by observation-based meteorology and aerosol depositions from GOES-5, better simulated the seasonal migration of snow depth, albedos, and impurities of dust, BC, and OC in the snow surface. However, the magnitude of the impurities is underestimated, compared to the sporadic snow impurity measurements. Increasing the deposition rates of dust and BC could explain the differences on the snow darkening effect between observation and simulation. Ignoring BC deposition can possibly lead to an extension of snow cover duration in Sapporo for four days. Comparing the off-line GOSWIM and the GEOS-5 global simulations, we found that determining better local precipitation and deposition rates of the aerosols are key factors in generating better GOSWIM snow darkening simulation in NASA GEOS-5.

land surface processes↗
NASA NTRS2026

Spacecraft Water Impurity Monitor, a System for Water Quality Analysis on Exploration Missions Beyond Low Earth Orbit

Exploration missions beyond low-earth-orbit (LEO) will require advanced instrumentation to monitor water quality. Traveling beyond LEO means the transfer of water samples to an Earth-based laboratory for detailed analysis is not feasible. Detailed analysis of water composition during exploration is still necessary, because having the capability to determine the specific organic chemical causing a change in total organic carbon (TOC) or the specific metal or ionic species causing a change in conductivity has the potential to inform the crew health and system management decisions. On a new vehicle such as a lunar or Mars surface habitat or a Mars transit vehicle, finding “new” impurities not seen on ISS should be expected. The key is to identify the impurity so the correct action can be taken. On ISS we can measure TOC, conductivity, and other physical properties but do not have the capability for detailed analysis using vehicle instrumentation. This is acceptable because ISS can send samples down to Earth for further analysis and obtain the detailed composition. The Spacecraft Water Impurity Monitor (SWIM) will provide detailed water quality analysis for missions in which sample down mass is not available. SWIM is a system comprising organic and inorganic analysis modules. For organic chemicals, a gas chromatograph mass spectrometer (GCMS) detects and identifies organic impurities. For inorganic species, a capillary electrophoresis capacitively coupled contactless conductivity detection (CE-C4D) system as well as ion specific electrodes detect and identify metal ions and other inorganic salts / acids. The SWIM technology demonstration project has completed a System Requirements Review (SRR) to finalize detection requirements and is currently working to refine vehicle interface requirements for a future technology demonstration. The project also has begun preliminary flight design activities for the core analyzers in the instrument suite.

Water Monitoring↗
NASA NTRS2026

Spacecraft Water Impurity Monitor, a System for Water Quality Analysis on Exploration Missions Beyond Low Earth Orbit

Exploration missions beyond low-earth-orbit (LEO) will require advanced instrumentation to monitor water quality. Traveling beyond LEO means the transfer of water samples to an Earth-based laboratory for detailed analysis is not feasible. Detailed analysis of water composition during exploration is still necessary, because having the capability to determine the specific organic chemical causing a change in total organic carbon (TOC) or the specific metal or ionic species causing a change in conductivity has the potential to inform the crew health and system management decisions. On a new vehicle such as a lunar or Mars surface habitat or a Mars transit vehicle, finding “new” impurities not seen on ISS should be expected. The key is to identify the impurity so the correct action can be taken. On ISS we can measure TOC, conductivity, and other physical properties but do not have the capability for detailed analysis using vehicle instrumentation. This is acceptable because ISS can send samples down to Earth for further analysis and obtain the detailed composition. The Spacecraft Water Impurity Monitor (SWIM) will provide detailed water quality analysis for missions in which sample down mass is not available. SWIM is a system comprising organic and inorganic analysis modules. For organic chemicals, a gas chromatograph mass spectrometer (GCMS) detects and identifies organic impurities. For inorganic species, a capillary electrophoresis capacitively coupled contactless conductivity detection (CE-C4D) system as well as ion specific electrodes detect and identify metal ions and other inorganic salts / acids. The SWIM technology demonstration project has completed a System Requirements Review (SRR) to finalize detection requirements and is currently working to refine vehicle interface requirements for a future technology demonstration. The project also has begun preliminary flight design activities for the core analyzers in the instrument suite.

Water Monitoring↗
NASA NTRS1973

The influence of defects and impurities on the nucleation and growth of oriented films by evaporation

The influence of substrate imperfections on the nucleation and growth of fcc metals on alkali halides is discussed. Films deposited on well characterized substrated under well defined vacuum evaporation conditions are investigated. The experimental results of this work are correlated with similar work by other investigators. Models which have been proposed by various authors to explain experimental results are critically examined and areas of difficulty are pointed out. The influence of defects on nucleation rate and the orientation of the film is emphasized. Specific examples of impurity effects, irradiation effects and the influence of amorphous layers are discussed in detail. Evidence is shown that the formation of multiply twinned particles is a result of coalescence and growth. The only consistent model for the orienting influence of impurities is shown to be a chemical reaction effect. It is demonstrated that an alkali metal impurity is very likely responsible for the orienting influence of both water vapor exposure and irradiation. A negative result is found for the reported possibility of an orienting influence being transmitted through an amorphous layer.

Green, A. K.↗