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At least 145 records · Page 8

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NASA NTRS1983

Synthesis and characterization of bisimide amines and bisimide amine-cured epoxy resins

An attempt is made to develop tough, moisture resistant, high char yield epoxy resins by means of novel bisimide amine (BIA) hardener curing agents and a state-of-the-art epoxy resin system. The BIAs are isolated as mixtures containing monomer, oligomer, and polymeric species, and then characterized by elemental analysis and high pressure liquid chromatography. The bisimide amine-cured epoxies (IMEs) were characterized with respect to moisture absorption, thermal properties, and physical and mechanical properties, as well as in the role of matrices in Celion 6000/IME composites. The relative toughness characteristics of each IME formulation was measured by the 10 deg off-axis tensile test, measuring the uniaxial tensile strength, shear strength, and shear-strain-to-failure of the composite systems.

Scola, D. A.↗

NASA NTRS1983

Partial Analysis of Insta-Foam

Insta-Foam, used as a thermal insulator for the non-critical area of the external tank during the prelaunch phase to minimize icing, is a two-component system. Component A has polyisocyanates, blowing agents, and stabilizers; Component B has the polyols, catalysts, blowing agents, stabilizers and fire retardant. The blowing agents are Freon 11 and Freon 12, the stabilizers are silicone surfactants, the catalysts are tertiary amines, and the fire retardant is tri-(beta-chloro-isopropyl) phosphate (PCF). High performance liquid chromatography (HPLC) was quantitatively identified polyols and PFC.

Chou, L. W.↗

NASA NTRS1984

Mammalian gravity receptors: Structure and metabolism

High performance liquid chromatography (HPLC) instrumentation was used for amino acid analysis of rat otoconial complexes. The amino acids of otoconial complexes pooled by origin from only 10 rats were analyzed. It is indicated that it should be possible to analyze complexes from only three rats, and perhaps fewer, which means that the method should be applicable to material from space flow rats. It is suggested that the organic otoconial phase is comparable in its complement of acidic amino acids to other calcium carbonate containing materials such as fish otoliths and certain mollusk shells. The organic material is high in acidic amino acids; and the relative proportions of aspirate, glutamate, threonine and serine appear to be similar to those found in neogastropod shells. Its significance to the evolution of biomineralization processes occurring in the animal kingdom is emphasized.

Ross, M.↗

NASA NTRS1983

Chlorophyll and carotenoid pigments of prochloron (prochlorophyta)

High-performance liquid chromatography (HPLC) with a gradient-elution technique was utilized to separate and quantify chlorophylls a and b as well as major carotenoid pigments present in freeze-dried preprations of prochloron-didemnid associations and in Prochloron cells separated from host colonies. Results confirm earlier spectrophotometric evidence for both chlorophylls a and b in this prokaryote. Chlorophyll a:b ratios range from 4.14 to 19.71; generally good agreement was found between ratios determined in isolated cell preprations and in symbiotic colonies (in hospite). These values are 1.5 to 5-fold higher than ratios determined in a variety of eukaryotic green plants. The carotenoids in Prochloron are quantitatively and qualitatively similar to those found in various freshwater and marine blue-green algae (cyanopbytes) from high-light environments. However, Prochloron differs from cyanophytes by the absence of myxoxanthophyll and related glycosidic carotenoids. It pigment characteristics are considered sufficiently different from those of cyanophytes to justify its assignment to a separate algal division.

Paerl, H. W.↗

NASA NTRS1984

Development of acceptance criteria for batches of silane primer for external tank thermal protection system bonding applications

Silane primers for use as thermal protection on external tanks were subjected to various analytic techniques to determine the most effective testing method for silane lot evaluation. The analytic methods included high performance liquid chromatography, gas chromatography, thermogravimetry (TGA), and fourier transform infrared spectroscopy (FTIR). It is suggested that FTIR be used as the method for silane lot evaluation. Chromatograms, TGA profiles, bar graphs showing IR absorbances, and FTIR spectra are presented.

Mikes, F.↗

NASA NTRS1985

SRM filament wound case resin characterization studies

The amine cured epoxy wet winding resin used in fabrication of the SRM filament wound case is analyzed. High pressure liquid chromatography (HPSC) is utilized extensively to study lot-to-lot variation in both resin and curing agent. The validity of quantitative hplc methodology currently under development in-process resin/catalyst assay is assessed.

Chou, L. W.↗

NASA NTRS1986

A Method for Characterizing PMR-15 Resin

Quantitative analysis technique based on reverse-phase, highperformance liquid chromatography (HPLC) and paired-ion chromatography (PIC) developed for PMR-15 resins. In reverse-phase HPLC experiment, polar solvent containing material to be analyzed passed through column packed with nonpolar substrate. Composition of PMR-15 Resin of 50 weight percent changes as resin ages at room temperature. Verification of proper resin formulation and analysis of changes in resin composition during storage important to manufacturers of PMR-15 polymer matrix composite parts. Technique especially suitable for commercial use by manufacturers of high-performance composite components.

Roberts, G. D.↗

NASA NTRS1985

Matrix resin development at NASA Langley Research Center

The polymer program at NASA Langley Research Center involves exploratory studies in polymer science. These include the synthesis of novel polymers and their characterization. Polymer synthesis programs involve the development of novel thermoplastics, pseudothermoplastics, and thermosets. Recent investigations have led to the development of more easily processable polyimides, solvent-resistant polysulfones and polyphenylquinoxalines, and tougher high and intermediate-temperature polymers. Characterization efforts have included high-pressure liquid chromatography methodology, the development of toughness tests for fiber-reinforced composites, a study of electrical properties of metal-ion-filled polyimides, and a study of the mutagenicity of aromatic diamines. Also the mechanism of cure/degradation of experimental polymers has been studied by rheology, mechanical behavior, separation techniques and spectroscopy. Some of these programs have involved the degradation crosslinking of alkyl-containing polyimides, the separation and identification of crosslinked phenylquinoxalines, the rheological behavior of hot-melt polyimides, and the elucidation of the cure of norbornene endcapped imides.

St.clair, T. L.↗

NASA NTRS1985

Characterization methodology for PMR-15

Characterization of model compounds, monomers, resin solutions and cure cycles of PMR-15 polyimide are performed. Successful separation of various reaction products is also accomplished by liquid chromatography. The PMR-15 cure analysis is performed by fourier transform spectroscopy and gas chromatograph - mass spectrometry. Characterization receiving inspection tests for Quality Control are recommended.

Hunter, A. B.↗

NASA NTRS1985

Quality assurance procedures for V378A matrix resin

A characterization methodology has been developed on which to base quality assurance procedures for U.S. Polymeric V378A bismaleimide matrix resin. Chemical composition is established by partition reverse phase and size exclusion liquid chromatography. Cure rheology behavior is quantitatively characterized by dynamic viscoelastic analysis using the parallel plate technique. The overall cure process is characterized by differential scanning calorimetry. The sensitivity of the procedures is evaluated by studying the effects of ambient out time on the chemical end behaviorial properties of the resin.

Hamermesh, C. L.↗

NASA NTRS1985

Direct coupling of microbore HPLC columns to MS systems

A detailed investigation using electron microscopy was conducted which examined the conditions of materials used in the construction of stable, high performance microbore liquid chromatography (LC) columns. Small details proved to be important. The effects of temperature on the elution of several homologous series used as probe compounds was examined in reverse phase systems. They showed that accessible temperature changes provide roughly half the increase in solvent strength that would be obtained going from a 100% aqueous to a 100% organic mobile phase, which is sufficient to warrant their use in many analyses requiring the use of gradients. Air circulation temperature control systems provide the easiest means of obtaining rapid, wide range changes in column temperature. However, slow heat transfer from the gas leads to thermal nonuniformity in the column and a decrease in resolution as the temperature program progresses.

Mcnair, H. M.↗

NASA NTRS1986

Analysis of a thioether lubricant by infrared Fourier microemission spectrophotometry

An infrared Fourier microemission spectrophotometer is used to obtain spectra (wavenumber range, 630 to 1230 0.1 cm) from microgram quantities of thioether lubricant samples deposited on aluminum foil. Infrared bands in the spectra are reproducible and could be identified as originating from aromatic species (1,3-disubstituted benzenes). Spectra from all samples (neat and formulated, used and unused) are very similar. Additives (an acid and a phosphinate) present in low concentration (0.10 percent) in the formulated fluid are not detected. This instrument appears to be a viable tool in helping to identify lubricant components separated by liquid chromatography.

Jones, W. R., Jr.↗

NASA NTRS1986

Development of LC-13C NMR

This study involves the development of C-13 nuclear resonance as an on-line detector for liquid chromatography (LC-C-13 NMR) for the chemical characterization of aviation fuels. The initial focus of this study was the development of a high sensitivity flow C-13 NMR probe. Since C-13 NMR sensitivity is of paramount concern, considerable effort during the first year was directed at new NMR probe designs. In particular, various toroid coil designs were examined. In addition, corresponding shim coils for correcting the main magnetic field (B sub 0) homogeneity were examined. Based on these initial probe design studies, an LC-C-13 NMR probe was built and flow C-13 NMR data was obtained for a limited number of samples.

Dorn, H. C.↗

NASA NTRS1986

Effect of solution concentration and aging conditions on PMR-15 resin

High performance liquid chromatography is utilized to evaluate the effect of temperature, solution concentration, and aging time on PMR-15 resin solutions. Fifty- and 70-wt percent PMR-15 resin solutions were prepared from the mixture of 5-norbornene-2,3-dicarboxylic ester (NE) acid, 4.4'-methylenedianiline (MDA), methanol, and 3,3',4.4.-benzophenonetetracarboxylic dimethyl ester (BTDE) acid solution. It is observed that in PMR-15 resin solution aged for 35 days at room temperature NE and MDA react to form amide and imide intermediates. The precipitation data reveal that in the 70-wt percent solution precipitation occurs after 12 days and in the 50-wt percent solution after 20 days; however, at lower temperatures (-11 C, and 2 C) no precipitation is detected. It is concluded that storage of resin solutions and powders at reduced temperatures extends shelf life by reducing the rate of imide formation.

Roberts, G. D.↗

NASA NTRS1986

A new technique for collection, concentration and determination of gaseous tropospheric formaldehyde

This article describes an improved technique for making in situ measurements of gaseous tropospheric formaldehyde (CH2O). The new technique is based on nebulization/reflux principles that have proved very effective in quantitatively scrubbing water soluble trace gases (e.g., CH2O) into aqueous mediums, which are subsequently analyzed. Atmospheric formaldehyde extractions and analyses have been performed with the nebulization/reflux concentrator using an acidified dinitrophenylhydrazine solution that indicate that quantitative analysis of CH2O at global background levels (about 0.1 ppbv) is feasible with 20-min extractions. Analysis of CH2O, once concentrated, is accomplished using high performance liquid chromatography with ultraviolet photometric detection. The CH2O-hydrazone derivative, produced by the reaction of 2,4-dinitrophenylhydrazine in H2SO4 acidified aqueous solution, is detected as CH2O.

Cofer, W. R., III↗

NASA NTRS1987

Changes in pituitary growth hormone cells prepared from rats flown on Spacelab 3

The effect of exposure to microgravity on pituitary gland was investigated by examining cells isolated from anterior pituitaries of rats flown on the 7-day Spacelab 3 mission and, subsequently, cultured for 6 days. Compared with ground controls, flight cells contained more intracellular growth hormone (GH); however, the flight cells released less GH over the 6-day culture period and after implantation into hypophysectomized rats than did the control cells. Compared with control rats, glands from large rats (400 g) contained more somatotrophs (44 percent compared with 37 percent in control rats); small rats (200 g) showed no difference. No major differences were found in the somatotroph ultrastructure (by TEM) or in the pattern of the immunoactive GH variants. However, high-performance liquid chromatography fractionation of culture media indicated that flight cells released much less of a biologically active high-molecular weight GH variant, suggesting that space flight may lead to secretory dysfunction.

Grindeland, R.↗

NASA NTRS1988

Surface and interfacial properties of carbon fibers

Differences in the adhesion of three carbon fibers (Hercules AS1 and AS4, and Hysol-Grafil XAS) to polycarbonate (PC) have been shown to correlate with the absorptivity of PC on the three fiber types. The absorptivity (energy of absorption) was determined using retention time liquid chromatography and the adhesion was measured using the single embedded filament tensile test. A correlation was also found between adhesion strength and the O/N surface element ratio using XPS analysis. The chemical details for these correlations have not yet been determined. A study of filament fracture statistics has been initiated using single and multiple embedded filament tensile tests. Filament fracture has been measured as a function of strain and for different interfiber distances. Preliminary results indicate that fiber fracture is a discontinuous function of increasing strain and may in fact occur at discrete strain intervals. Fiber-fiber interaction effects on fiber fracture have been found for interfiber distances of up to two to three fiber diameters.

Bascom, W. D.↗

NASA NTRS1988

The evolution of glutathione metabolism in phototrophic microorganisms

The low molecular weight thiol composition of a variety of phototropic microorganisms is examined in order to ascertain how evolution of glutathione (GSH) production is related to the evolution of oxygenic photosynthesis. Cells were extracted in the presence of monobromobimane (mBBr) to convert thiols (RSH) to fluorescent derivatives (RSmB) which were analyzed by high performance liquid chromatography (HPLC). Significant levels of GSH were not found in green sulfur bacteria. Substantial levels were present in purple bacteria, cyanobacteria, and eukaryotic algae. Other thiols measured included cysteine, gamma-glutamylcysteine, thiosulfate, coenzyme A, and sulfide. Many of the organisms also exhibited a marked ability to reduce mBBr to syn-(methyl,methyl)bimane, an ability which was quenched by treatment with 2-pyridyl disulfide or 5,5 prime-bisdithio - (2-nitrobenzoic acid) prior to reaction with mBBr. These observations indicate the presence of a reducing system capable of electron transfer to mBBr and reduction of reactive disulfides. The distribution of GSH in phototropic eubacteria indicates that GSH synthesis evolved at or around the time that oxygenic photosynthesis evolved.

Fahey, Robert C.↗