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At least 163 records · Page 9

Synthesis of N-Substituted Silaneamines: Monomeric Precursors of Silicon Carbide-Nitride Fibers

Silanetriamines are prepared by the condensation of methyl or phenyl trichlorosilane with a primary amine. The amines used were methyl, n-propyl, n-butyl and allyl. The silaneamines were prepared by adding the chlorosilane to a solution of the amine in either petroleum ether or toluene. The compounds were purified by distillation and characterized by infrared and nuclear magnetic resonance spectroscopy.

Crouse, D. J.↗

Physical aging and its influence on the reliability of network epoxies and epoxy-matrix composites

The matrix-dominated physical and mechanical properties of a carbon fiber reinforced epoxy composite and a neat epoxy resin were found to be affected by sub-Tg annealing in nitrogen and dark atmosphere. Postcured specimens of Thornel 300 carbon-fiber/Fiberite 934 epoxy as well as Fiberite 934 epoxy resin were quenched from above Tg and given annealing at 140 C, 110 C, or 80 C, for time up to one-hundred thousand minutes. No weight loss was observed during annealing at these temperatures. Significant variations were found in density, modulus, hardness, damping, moisture absorption ability, thermal expansivity. Moisture-epoxy interactious were also studied. The kinetics of aging as well as the molecular aggregation during this densification process were monitored by differential scanning calorimetry, dynamic mechanical analysis, density gradient column, microhardness tester, Instron, and solid-state nuclear magnetic resonance spectroscopy.

Heinemann, K.↗

Synthesis and characterization of phosphorus-containing polyamides and copolyamides based on 1methyl]-2,4- and -2,6-diaminobenzenes

Phosphorus containing polyamides and copolyamides were prepared from 1-(dialkoxyphosphinyl)methyl-2,4- and -2,6-diaminobenzenes. The polymers produced were characterized by infrared and proton nuclear magnetic resonance spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. Their thermal properties were compared with those of the corresponding common polyamides. In addition, by determining the limiting oxygen index value of some of these polyamides, their fire resistance was evaluated.

Mikroyannidis, J. A.↗

Physical aging in graphite/epoxy composites

Sub-Tg annealing has been found to affect the properties of graphite/epoxy composites. The network epoxy studied was based on the chemistry of tetraglycidyl 4,4'-diamino-diphenyl methane (TGDDM) crosslinked by 4,4'-diamino-diphenyl sulfone (DDS). Differential scanning calorimetry, thermal mechanical analysis, and solid-state cross-polarized magic-angle-spinning nuclear magnetic resonance spectroscopy have been utilized in order to characterize this process of recovery towards thermodynamic equilibrium. The volume and enthalpy recovery as well as the 'thermoreversibility' aspects of the physical aging are discussed. This nonequilibrium and time-dependent behavior of network epoxies are considered in view of the increasingly wide applications of TGDDM-DDS epoxies as matrix materials of structural composites in the aerospace industry.

Kong, E. S. W.↗

Binding constants of phenylalanine for the four mononucleotides

Earlier work has shown that several properties of amino acids correlate directly with properties of their anticodonic nucleotides. Furthermore, in precipitation studies with thermal proteinoids and homopolyribonucleotides, an anticodonic preference was displayed between Lys-rich, Pro-rich and Gly-rich thermal proteinoids and their anticodonic polyribonucleotides. However, Phe-rich thermal proteinoid displayed a preference for its codonic nucleotide, poly U. This inconsistency seemed to be explained by a folding in of the hydrophobic residues of Phe causing the proteinoid to appear more hydrophilic. The present work used nuclear magnetic resonance techniques to resolve a limited question: to which of the four nucleotides does Phe bind most strongly? The results show quite clearly that Phe binds most strongly to its anticodonic nucleotide, AMP.

Khaled, M. A.↗

Multispectral Analysis of NMR Imagery

Conference paper discusses initial efforts to adapt multispectral satellite-image analysis to nuclear magnetic resonance (NMR) scans of human body. Flexibility of these techniques makes it possible to present NMR data in variety of formats, including pseudocolor composite images of pathological internal features. Techniques do not have to be greatly modified from form in which used to produce satellite maps of such Earth features as water, rock, or foliage.

Butterfield, R. L.↗

Preparation and characterization of a siloxane containing bismaleimide

A novel siloxane containing bismaleimide has been prepared by reacting maleic anhydride, benzophenonetetracarboxylic dianhydride and bis(gamma-aminopropyl)tetramethyldisiloxane. Characterization of this monomer was done by comparing its nuclear magnetic resonance spectrum (NMR) to those of model compounds. Solubility of the prepolymer was tested in amide, chlorinated and ether solvents. Films were cast from solution as well as by melt processing and a cure cycle was determined. Infrared spectrum (IR) of the resulting film was obtained. Thermal polymerization was investigated by differential scanning calorimetry (DSC). Thermal properties of the cured resin were followed by means of thermogravimetric analysis (TGA), torsional braid analysis (TBA) and dynamic mechanical analysis (DMA). Thermomechanical analysis (TMA) was used to study the effect of postcure on the glass transition temperature (Tg) of the resin. Adhesive strength of the resin was obtained at ambient temperature.

Maudgal, S.↗

Synthesis and characterization of phosphorus-containing polyamides and copolyamides based on 1-(dialkoxyphosphinyl)methyl-2,4- and -2,6-diaminobenzenes

Phosphorus containing polyamides and copolyamides were prepared from 1-(dialkoxyphosphinyl)methyl-2,4- and -2,6-diaminobenzenes. The polymers produced were characterized by infrared and proton nuclear magnetic resonance spectroscopy, differential scanning calorimetry, and thermogravimetric analysis. Their thermal properties were compared with those of the corresponding common polyamides. In addition, by determining the limiting oxygen index value of some of these polyamides, their fire resistance was evaluated.

Mikroyannidis, J. A.↗

Synthesis and analysis in studies of chemical evolution

Studies of the various processes that may have given rise to life on the Earth have demonstrated the appropriateness of an approach that makes use of analysis and synthesis. Analysis of extraterrestrial samples in the form of meteorites has demonstrated the presence of several precursors of biomolecules, most notably a full suite of nucleic acid bases and nucleotides of biological significance. These species were determined after exhaustive extraction of the sample and subsequent analysis using HPLC, GC, MS, and GC-MS. Procedural blanks indicate that these molecules are likely not the result of contamination during the extraction and analysis process. Similar species were found as products of spark discharge experiments in atmospheres thought to mimic primitive Earth conditions. These results indicate that the basic chemistry underlying these syntheses is common, and that life may not be unique to the Earth. Studies underway in the laboratory make use of proton nuclear magnetic resonance spectroscopy as a probe to assess associations between selected amino acids and any of several nucleotides comprising their genetic code and genetic anticode sequences. These studies demonstrate a clear selectivity by the anticode sequences, thus confirming the hydrophobicity studies performed by Lacey et al. These studies further support the contention that life is likely a natural result of the physics and chemistry of the universe.

Ponnamperuma, C.↗

Origin and evolution of osmoregulatory mechanisms in blue-green algae (cyanobacteria) as a function of metabolic and structural complexity: Reflections of Precambrian paleobiology

Major accomplishments underlying the basic understanding of cyanobacterial resistance to salt tolerance and osmotic stress were made. The methodology proposed included: the tracing of the pathways of formation of osmoregulatory solutes by traditional methods involving C-14 labelled substrates; gas chromatography; amino acid analysis; X-ray analysis using scanning transmission electron microscopy; and most importantly, C-13 labelled substrates, followed by Nuclear Magnetic Resonance (NMR) spectroscopy. It was found that the cyanobacteria employ a diversity of organic, osmoregulatory solutes. Osmoregulatory solutes were found to serve four functions: adjustment of water activity, noninhibition of enzymes; lowering of K sub m of enzymes to allow functioning at normal levels when the intracellular salt accumulates, and extending the pH optimum of enzymes as intracellular pH rises due to proton-potassium ion pump action during osmoregulation. Differences in osmoregulatory solutes may, but are not always, be attributed to differences in nutritional capabilities. The mechanism of osmoregulation and concomitant salt tolerance in halophilic cyanobacteria was elucidated. The activities of betaine and S-Adenosylhomocysteine hydrolase are discussed.

Yopp, John H.↗

Physical aging in epoxy matrices and composites

Postcured specimens of Thornell 300 carbon-fiber/Fiberite 934 epoxy as well as Fiberite 934 epoxy resin were quenched from above the glass transition temperature and annealed at 140, 110, or 80 C for times up to 100,000 min. No weight gain or loss was observed during annealing at these temperatures, but significant time-dependent variations were observed in density, modulus, hardness, damping, moisture absorption ability, and thermal expansion characteristics. The relations between the excess thermodynamic properties of epoxy glasses and their time-dependent behavior are discussed. The discussion is illustrated by results obtained by differential scanning calorimetry, dynamic mechanical analysis, tensile testing, solid state nuclear magnetic resonance spectroscopy, and small-angle X-ray scattering.

Kong, Eric Siu-Wai↗

Growth of large zeolite crystals in space

Synthesis studies performed using close analogs of triethanolamine (TEA) have shown that all three hydroxyl groups and the amine group in this molecule are necessary to provide nucleation suppression. Studies using C-13 nuclear magnetic resonance (NMR) revealed that the hydroxyl ions and the amine group are involved in the formation of an aluminum complex. It was also shown that silicate species fo not interact this way with TEA in an alkaline solution. These results suggest that successful aluminum complexation leads to nucleation in zeolite-A crystallization.

Sacco, A., Jr.↗

Addition polymers from 1,4,5,8-tetrahydro-1,4;5,8-diepoxyanthracene and Bis-dienes. 2: Evidence for thermal dehydration occurring in the cure process

Diels-Alder cycloaddition copolymers from 1,4,5,8-tetrahydro-1,4;5,8-diepoxyanthracene and anthracene end-capped polyimide oligomers appear, by thermogravimetric analysis (TGA), to undergo dehydration at elevated temperatures. This would produce thermally stable pentiptycene units along the polymer backbone, and render the polymers incapable of unzipping through a retro-Diels-Alder pathway. High resolution solid 13C nuclear magnetic resonance (NMR) of one formulation of the polymer system before and after heating at elevated temperatures, shows this to indeed be the case. NMR spectra of solid samples of the polymer before and after heating correlated well with those of the parent pentiptycene model compound before and after acid-catalyzed dehydration. Isothermal gravimetric analyses and viscosities of the polymer before and after heat treatment support dehydration as a mechanism for the cure reaction.

Meador, Mary Ann B.↗

A (13)C NMR analysis of the effects of electron radiation on graphite/polyetherimide composites

Initial investigations have been made into the use of high resolution nuclear magnetic resonance (NMR) for the characterization of radiation effects in graphite and Kevlar fibers, polymers, and the fiber/matrix interface in graphite/polyetherimide composites. Sample preparation techniques were refined. Essential equipment has been procured. A new NMR probe was constructed to increase the proton signal-to-noise ratio. Problem areas have been identified and plans developed to resolve them.

Ferguson, Milton W.↗

The origin, composition and history of cometary ices from spectroscopic studies

The spectroscopic analysis of pristine cometary material provides a very important probe of the chemical identity of the material as well as of the physical and chemical conditions which prevailed during the comet's history. Concerning classical spectroscopy, the spectral regions which will most likely prove most useful are the infrared, the visible and ultraviolet. Newer spectroscopic techniques which have the potential to provide equally important information include nuclear magnetic resonance (NMR) and electron spin resonance (ESR). Each technique is summarized with emphasis placed on the kind of information which can be obtained.

Allamandola, L. J.↗

The Chemical Basis for the Origin of the Genetic Code and the Process of Protein Synthesis

A model for the origin of protein synthesis. The essential features of the model are that 5'-AMP and perhaps other monoribonucleotides can serve as catalysts for the selective synthesis of L-based peptides. A unique set of characteristics of 5'-AMP is responsible for the selective catalysts and these characteristics are described in detail. The model involves the formation of diesters as intermediates and selectivity for use of the L-isomer occurs principally at the step of forming the diester. However, in the formation of acetyl phenylalanine-AMP monoester there is a selectivity for esterification by the D-isomer. Data showing this selectivity is presented. This selectivity for D-isomer disappears after the first step. The identity was confirmed of all four of possible diesters of acetyl-D- and -L phenylaline with 5'-AMP by nuclear magnetic resonance (NMR). The data using flourescence and NMR show the Trp ring can associate with the adenine ring more strongly when the D-isomer is in the 2' position than it can when in the 3' position. These same data also suggest a molecular mechanisim for the faster esterificaton of 5'-AMP by acetyl-D-phenylaline. Some new data is also presented on the possible structure of the 2' isomer of acetyl-D-tryptophan-AMP monoester. The HPLC elution times of all four possible acetyl diphenylalanine esters of 5'-AMP were studied, these peptidyl esters will be products in the studies of peptide formation on the ribose of 5'-AMP. Other studies were on the rate of synthesis and the identity of the product when producing 3'Ac-Phe-2'tBOC-Phe-AMP diester. HPLC purification and identification of this product were accomplished.

Lacey, James C., Jr.↗

Magnetic properties of high-T(sub c) superconductors: Rigid levitation, flux pinning, thermal depinning, and fluctuation

The levitation of high-T(sub c) superconductors is quite conspicuous: Above magnets of low symmetry a disk of these ceramics floats motionless, without vibration or rotation; it has a continuous range of stable positions and orientations as if it were stuck in sand. Some specimens may even be suspended above or below the same magnet. This fascinating stability, inherent to no other type of levitation, is caused by the pinning of magnetic flux lines by inhomogeneities inside these extreme type-2 superconductors. The talk deals with pinning of magnetic flux in these materials, with flux flow, flux creep, thermally activated depinning, and the thermal fluctuation of the vortex positions in the flux line lattice (often called flux lattice melting). Also discussed are the fluctuations of the (nearly periodic) magnetic field inside these superconductors which are caused by random pinning sites and by the finite temperature. These fluctuations broaden the van-Hove singularities observed in the density of the magnetic field by nuclear magnetic resonance and by muon spin rotation.

Brandt, E. H.↗

Magnetic correlations in La(2-x)Sr(x)CuO4 from NQR relaxation and specific heat

La-139 and Cu-63 Nuclear Quadrupole Resonance (NQR) relaxation measurements in La(2-x)Sr(x)CuO4 for O = to or less than 0.3 and in the temperature range 1.6 + 450 K are analyzed in terms of Cu(++) magnetic correlations and dynamics. It is described how the magnetic correlations that would result from Cu-Cu exchange are reduced by mobile charge defects related to x-doping. A comprehensive picture is given which explains satisfactorily the x and T dependence of the correlation time, of the correlation length and of the Neel temperature T(sub n)(x) as well as being consistent with known electrical resistivity and magnetic susceptibility measurements. It is discussed how, in the superconducting samples, the mobile defects also cause the decrease, for T yields T(sub c)(+) of the hyperfine Cu electron-nucleus effective interaction, leading to the coexistence of quasi-localized, reduced magnetic moments from 3d Cu electrons and mobile oxygen p-hole carriers. The temperature dependence of the effective hyperfine field around the superconducting transition yields an activation energy which could be related to the pairing energy. New specific heat measurements are also presented and discussed in terms of the above picture.

Borsa, F.↗