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At least 343 records · Page 19

A new approach to the isolation of milligram amounts of significant geochemical compounds.

The modification of an automatic preparative collection system for gas-liquid chromatography is described that is designed to make the system operational for milligram-scale high-efficiency separations of selected components in a geological sample. The sample in question is an organic extract from the Green River Formation Oil Shale, and the compounds selected are the sterane and triterpane hydrocarbons.

Wszolek, P. C.↗

Planetary quarantine: Supporting research and technology

Planetary quarantine strategies for advanced missions are described, along with natural space environment studies and post launch recontamination studies. Spacecraft cleaning and decontamination techniques and assay activities are reviewed. Teflon ribbon experiments and pyrolsis gas-liquid chromatography study are also considered.

Taylor, D. M.↗

Thermal alteration of young kerogen in relation to petroleum genesis

Kerogen, humic acid, and lipid material were separated from a young marine sediment and heated in sealed tubes in a nitrogen atmosphere at 150 and 410 C. Gaseous and liquid products generated during heating, and also the residual organic material, were characterized by gas-liquid chromatography, elemental analysis, infrared and electron spin resonance spectroscopy, and X-ray diffraction.

Ishiwatari, R.↗

The stereoisomeric composition of phytanyl chains in lipids of Dead Sea sediments

Lipid extracts from five recent Dead Sea sediments were analyzed for isoprenoid compounds and the following were isolated: free and phospholipid-bound di-O-phytanylglycerol, free phytanol and free and esterified phytanic acid. The phytanyl groups of the diether and the free phytanol were oxidized to the corresponding phytanic acid; the stereoisomeric composition of the derived phytanic acids as well as of the ester-bound phytanic acid was determined by open-tubular gas-liquid chromatography of the corresponding methyl esters on butanediolsuccinate polyester. Only the 3R, 7R, 11R-isomer of phytanic acid was detected in each of the phytanate samples, indicating that these phytanyl chains in the Dead Sea sediments are most likely derived from extremely halophilic bacteria rather than from phytol of chlorophyll origin. These findings also provide further evidence that the mixtures of RRR and SRR-phytanic acids previously isolated from organic-rich shales were most likely derived from the phytyl chain in chlorophyll.

Anderson, R.↗

HPLC for quality control of polyimides

High Pressure Liquid Chromatography (HPLC) as a quality control tool for polyimide resins and prepregs are presented. A data base to help establish accept/reject criteria for these materials was developed. This work is intended to supplement, not replace, standard quality control tests normally conducted on incoming resins and prepregs. To help achieve these objectives, the HPLC separation of LARC-160 polyimide precursor resin was characterized. Room temperature resin aging effects were studied. Graphite reinforced composites made from fresh and aged resin were fabricated and tested to determine if changes observed by HPLC were significant.

Young, P. R.↗

Thermal reaction of ethynylphthalimides and hydration of N-/4-ethynylphenyl/phthalimide

Three ethynyl substituted phenylphthalimides were prepared and characterized by high pressure liquid chromatography, differential scanning calorimetry, and mass spectroscopy. When the preparation of N-(4-ethynylphenyl)phthalimide was attempted by the thermal cyclodehydration of N-(4-ethynylphenyl)-2-carboxybenzamide, N-(4-acetylphenyl)phthalimide was obtained as the major component. This unusual hydration of an ethynyl group was investigated and a mechanism was proposed to explain it.

Hergenrother, P. M.↗

Characterization of initial cure reactions in propargyl and nadic end capped model compounds

Imide model compounds containing propargyl and nadic groups were studied to obtain a fundamental understanding of the reaction of these groups attached to imide oligomers. The initial cure reactions were examined by a variety of characterization techniques including high pressure liquid chromatography, infrared spectroscopy, thermal analyses, and mass spectroscopy. The initial step in the cure of propargyl end capped model compounds probably involved the formation of a new terminal acetylenic group. Configurational changes involving endo/exo isomerism was found in the nadimide model compounds. Nadimide compounds heated in air and in nitrogen appeared to cure by different mechanisms.

Young, P. R.↗

Gamma-irradiation of malic acid in aqueous solutions

The gamma-irradiation of malic acid in aqueous solutions was studied under initially oxygenated and oxygen-free conditions in an attempt to determine the possible interconversion of malic acid into other carboxylic acids, specifically those associated with Krebs cycle. The effect of dose on product formation of the system was investigated. Gas-liquid chromatography combined with mass spectrometry was used as the principal means of identification of the nonvolatile products. Thin layer chromatography and direct probe mass spectroscopy were also employed. The findings show that a variety of carboxylic acids are formed, with malonic and succinic acids in greatest abundance. These products have all been identified as being formed in the gamma-irradiation of acetic acid, suggesting a common intermediary. Since these molecules fit into a metabolic cycle, it is strongly suggestive that prebiotic pathways provided the basis for biological systems.

Negron-Mendoza, A.↗

Characterization of aging effects of LARC-160

Specimens of freshly prepared polyimide precursor resin LARC-160 and resin aged at room temperature up to 45 days were characterized by high-pressure liquid chromatography and several different thermal analyses. Graphite reinforced composites were then fabricated from fresh and aged resin and tested to determine if changes observed by these techniques were significant. It was found that resin aging resulted in greater flow during processing and poorer composite isothermal stability. However, aging did not affect the room-temperature flexural or short-beam-shear strengths of the composites.

Young, P. R.↗

Preparation and analysis of standardized waste samples for Controlled Ecological Life Support Systems (CELSS)

The preparation and analysis of standardized waste samples for controlled ecological life support systems (CELSS) are considered. Analysis of samples from wet oxidation experiments, the development of ion chromatographic techniques utilizing conventional high pressure liquid chromatography (HPLC) equipment, and an investigation of techniques for interfacing an ion chromatograph (IC) with an inductively coupled plasma optical emission spectrometer (ICPOES) are discussed.

Carden, J. L.↗

Template-directed synthesis of oligoguanylic acids - Metal ion catalysis

The effects of Zn(2+), Pb(2+) and other metal ions on the efficiency and stereo-selectivity of the template-directed oligomerization of guanosine 5'-phosphorimidazolide are investigated. Reactions were run in the presence of a polyC template in a 2,6-lutidine buffer, and products analyzed by high-performance liquid chromatography on an RPC-5 column. The presence of the Pb(2+) ion is found to lead to the formation of 2'-5' linked oligomers up to the 40-mer, while Zn(2+) favors the formation of predominantly 3'-5' linked oligomers up to the 35-mer. When amounts of uracil, cytidine or adenosine 5'-phosphorimidazole equal to those of the guanosine derivative are included in the reaction mixture, the incorrect base is incorporated into the oligomer about 10% of the time with a Pb(2+) catalyst, but less than 0.5% of the time with Zn(2+). The Sn(2+), Sb(3+) and Bi(3+) ions are also found to promote the formation of 2'-5' oligomers, although not as effectively as Pb(2+), while no metal ions other than Zn(2+) promote the formation of the 3'-5' oligomers. The results may be important for the understanding of the evolution of nucleic acid replication in the absence of enzymes.

Bridson, P. K.↗

Fire-Resistant Composites

Resin blend produces high-char-yield, low-smoke composites. Diglycidyl Ether of Bis-(4-Hydroxyphenyl)-Fluorene is prepared by reacting epichlorohydrin and sodium hydroxide with 9,9-bis(hydroxyphenyl) fluorene. End of reaction determined by gas or liquid chromatography, mass spectroscopy or infrared techniques. Used to manufacture printed circuit boards and panels for buildings, ships and aircraft.

Kourtides, D. A.↗

Polymer research at NASA Langley Research Center

Polymer synthesis programs involve the development of Novel thermoplastics, pseudothermoplastics, and thermosets. These systems are prepared to elucidate structure-property relationships involving thermal capabilities, toughness, processability and environmental stability. Easily processable polyimides, solvent-resistant polysulfones and polyphenylquinoxalines, and tougher high and intermediate temperature polymers were developed. Characterization efforts 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 was studied by rheology, mechanical behavior, separation techniques and spectroscopy. The degradative 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 were also studied.

Terry L. St. Clair↗

Mutagenic screening of diamine monomers

The effects of phenyl ring coupling moieties, of isomeric amine positions relative to the coupling groups, and of insertion of other coupling groups on the mutagenic response of a series of dianilines were investigated using the Ames Salmonella assay. Generally, S-9 metabolic activation from Aroclor-induced rat liver was required for mutagenic expression. The range of mutagenicity of steric isomers of several dianiline series was also investigated. No mutagenicity was found for purified samples of o,o' and m,p' isomers of methylene dianiline (MDA) and diaminobenzophenone, while varying degrees of mutagenicity were found for other isomers. The mutagenicity of "benzylogs" of MDA decreased as the degree of linear separation of the m,m' anilino groups by aromatic rings increased. Methylation and two-year storage increased mutagenic response in certain isomers of MDA. However, high performance liquid chromatography indicated there was no discernible change in m,p'-MDA samples aged under varied conditions over four months. Likewise, no change in mutagenicity was found.

Ross, W. D.↗

A carbon-13 and proton nuclear magnetic resonance study of some experimental referee broadened-specification /ERBS/ turbine fuels

Preliminary results of a nuclear magnetic resonance (NMR) spectroscopy study of alternative jet fuels are presented. A referee broadened-specification (ERBS) aviation turbine fuel, a mixture of 65 percent traditional kerosene with 35 percent hydrotreated catalytic gas oil (HCGO) containing 12.8 percent hydrogen, and fuels of lower hydrogen content created by blending the latter with a mixture of HCGO and xylene bottoms were studied. The various samples were examined by carbon-13 and proton NMR at high field strength, and the resulting spectra are shown. In the proton spectrum of the 12.8 percent hydrogen fuel, no prominent single species is seen while for the blending stock, many individual lines are apparent. The ERBS fuels were fractionated by high-performance liquid chromatography and the resulting fractions analyzed by NMR. The species found are identified.

Dalling, D. K.↗

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.↗

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.↗

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.↗