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At least 19 records

High-pressure liquid chromatography: A brief introduction and its application in analyzing the degradation of a C-ether (Thio-ether) liquid lubricant

The general principles of classical liquid chromatography and high pressure liquid chromatography (HPLC) are reviewed, and their advantages and disadvantages are compared. Several chromatographic techniques are reviewed, and the analytical separation of a C-ether liquid lubricant by each technique is illustrated. A practical application of HPLC is then demonstrated by analyzing a degraded C-ether liquid lubricant from full scale, high temperature bearing tests.

Source record

Use of high pressure liquid chromatography in the study of liquid lubricant oxidation

The general principles of classical liquid chromatography and high-pressure liquid chromatography (HPLC) are reviewed, and their advantages and disadvantages are compared. Several chromatographic techniques are reviewed, and the analysis of a C-ether liquid lubricant by each technique is illustrated. An analysis by size exclusion chromatography of an ester lubricant, which had been degraded using a micro-oxidation apparatus, is illustrated to show how HPLC can be used in the study of high-temperature lubricant degradation.

Morales, W.

High-pressure liquid chromatography of aromatic amines

Analysis made on commercially available liquid chromatograph demonstrates high-pressure liquid chromatographic conditions for separation of approximately 50 aromatic amines ranging from simple aniline derivatives to complex multiring di- and tri-amines.

Young, P. R.

Research to Significantly Enhance Composite Survivability at 550 F in Oxidative Environments

Prairie View A&M University using the NASA FAR grant has embarked on several paths to accomplish the initial goals of: (1) synthesizing three ring aromatic diamines to be used as monomers in the synthesis of polyamide resins; and (2) study hydrothermal aging behaviors and glass transition changes of composites synthesized at NASA Glenn Research Center. In establishing the synthesis of the three ring aromatic diamine, it has become necessary to conduct preliminary synthesis to include the nitration of diphenylmethane. The concentration and temperature were altered to assess the effect of purity of isomeric product distribution in such electrophilic aromatic substitution reaction. Products were analyzed using H and C-NMR, Thin Layer Chromatography, High Pressure Liquid Chromatography and GC-Mass Spectrometry (in progress). Results indicate that by varying the concentration of the reaction, a mixture of products can be obtained. Other electrophilic aromatic substitution reactions are also in progress such as Friedel-Craft acylation reaction using diphenylmethane with 4-nitrobenzoyl chloride to afford other diamine products. Furthermore, PVAMU has nearly completed the hydrothermal studies to assess the oxidative stability of DSP443B and DSP442A panels formulated at NASA Glenn Research Center.

Byrd, Jim

Persistence of bone collagen cross-links in skeletons of the Nuraghi population living in Sardinia 1500-1200 B.C

Bone collagen has a specific molecular ultrastructure which can be proved by birefringence. This protein, forming the main organic component of bone tissue, is known to survive millennia in paleontological bones and teeth. Birefringence of bone collagen obtained from the skeletons of the Nuraghi population living in Sardinia c-ca 1500 years B.C. was found previously by the use of polarizing microscopy [1]. In this paper, using high pressure liquid chromatography (HPLC) techniques, we show the existence of bone collagen cross-links preserved in Nuraghi skeletons after more than 3000 years.

Non-NASA Center

Formation of RNA oligomers on montmorillonite: site of catalysis

Certain montmorillonites catalyze the self condensation of the 5'-phosphorimidazolide of nucleosides in pH 8 aqueous electrolyte solutions at ambient temperatures leading to formation of RNA oligomers. In order to establish the nature of the sites on montmorillonite responsible for this catalytic activity, oligomerization reactions were run with montmorillonites which had been selectively modified (I) at the edges by (a) fluoride treatment, (b) silylation, (c) metaphosphate treatment of the anion exchange sites (II) in the interlayer by (a) saturation with quaternary alkylammonium ions of increasing size, (b) aluminum polyoxo cations. High pressure liquid chromatography, HPLC, analysis of condensation products for their chain lengths and yields indicated that modification at the edges did not affect the catalytic activity to a significant extent, while blocking the interlayer strongly inhibited product formation.

NASA Discipline Exobiology

Alpha-A crystallin: quantitation of C-terminal modification during lens aging

Previous studies have demonstrated that the C-terminal region of alpha-A crystallin is susceptible to age-dependent, posttranslational modification. To quantitate the amount of modification, alpha-A crystallin was purified from total proteins of the aging bovine lens, then digested with lys-C endoproteinase. Reverse phase, high pressure liquid chromatography was used to resolve and quantitate the resulting peptides, to determine the amount of C-terminal peptide relative to peptides from other regions of the protein that have not been reported to undergo modification. The results indicate that relative to alpha-A crystallin from newborn lens, posttranslational modification has occurred in approximately 45-55% of the C-terminal region from mature lens. These results demonstrate extensive modification of the C-terminal region of alpha-A crystallin from the mature lens, indicating that during the aging process, posttranslational modifications in this region may make significant contributions to the aggregated state and/or molecular chaperone properties of the molecule.

NASA Discipline Cell Biology

Use of Fisher's Ratio assisted multivariate curve resolution- alternating least squares for discovery-based analysis using ultrahigh pressure liquid chromatography-high resolution mass spectrometry

Non-targeted analysis of complex chemical mixtures can be difficult considering the convoluted nature of the matrix and the potential unknown chemical differences between samples or classes of samples. Ultrahigh pressure liquid chromatography coupled to quadrupole time-of-flight mass spectrometry (UHPLC-QTOF) is an ideal technique to probe chemical differences for a wide variety of samples. While UHPLC-QTOF can discover minute chemical differences down to low part per billion (ppb) concentrations with a high degree of confidence, the application of high-resolution mass spectrometry can yield massive amounts of information (∼ 10 gb per sample) that cannot be analyzed manually. Therefore, the application of chemometric techniques is mandatory for the interrogation of complex samples. Fisher's ratio (FR) assisted multivariate curve resolution-alternating least squares (MCR-ALS) was used to the discover and identify the chemical differences between two classes of materials: 1) a pond water matrix and 2) the matrix spiked with a pharmaceutical standard mix containing 17 compounds. Thirteen of the seventeen spiked compounds were discovered using FR analysis, and then five were successfully deconvoluted using MCR-ALS wherein the number of curves chosen were automatically determined using singular value decomposition (SVD). In conclusion, the use of an automated FR assisted MCR-ALS will aid in discovering trace levels of chemical components without the need for the researcher to provide potentially biased input which will aid in non-targeted workflow.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH

Quantitative separation of tetralin hydroperoxide from its decomposition products by high performance liquid chromatography

A method for the separation and analysis of tetralin hydroperoxide and its decomposition products by high pressure liquid chromatography has been developed. Elution with a single, mixed solvent from a micron-Porasil column was employed. Constant response factors (internal standard method) over large concentration ranges and reproducible retention parameters are reported.

Worstell, J. H.

Application of cabin atmosphere monitors to rapid screening of breath samples for the early detection of disease states

Analysis of human breath is a nonintrusive method to monitor both endogenous and exogenous chemicals found in the body. Several technologies were investigated and developed which are applicable to monitoring some organic molecules important in both physiological and pathological states. Two methods were developed for enriching the organic molecules exhaled in the breath of humans. One device is based on a respiratory face mask fitted with a polyethylene foam wafer; while the other device is a cryogenic trap utilizing an organic solvent. Using laboratory workers as controls, two organic molecules which occurred in the enriched breath of all subjects were tentatively identified as lactic acid and contisol. Both of these substances occurred in breath in sufficient amounts that the conventional method of gas-liquid chromatography was adequate for detection and quantification. To detect and quantitate trace amounts of chemicals in breath, another type of technology was developed in which analysis was conducted using high pressure liquid chromatography and mass spectrometry.

Valentine, J. L.

High performance addition-type thermoplastics (ATTs) - Evidence for the formation of a Diels-Alder adduct in the reaction of an acetylene-terminated material and a bismaleimide

Recently, the concept and demonstration of a new versatile synthetic reaction for making a large number of high-performance addition-type thermoplastics (ATTs) were reported. The synthesis shows promise for providing polymers having an attractive combination of easy processability, good toughness, respectable high temperature mechanical performance, and excellent thermo-oxidative stability. The new chemistry involves the reaction of an acetylene-terminated material with a bismaleimide or benzoquinone. In order to clarify the reaction mechanism, model compound studies were undertaken in solutions as well as in the solid state. The reaction products were purified by flash chromatography and characterized by conventional analytical techniques including NMR, FT-IR, UV-visible, mass spectroscopy, and high pressure liquid chromatography. The results are presented of the model compound studies which strongly support the formation of a Diels-Alder adduct in the reaction of an acetylene-terminated compound and a bismaleimide or benzoquinone.

Pater, R. H.

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.

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.

Analysis of aromatic polyamine mixtures for formulation of LARC-160 resin

An investigation was conducted to identify a potential substitute for the aromatic polyamine mixture, Jeffamine AP-22, currently used to formulate LARC-160 polyimide precursor resin. Jeffamine AP-22 was characterized by high pressure liquid chromatography and mass spectrometry. Eleven different aromatic amines in the mixture were isolated and identified. Subsequent liquid chromatographic analysis of nine additional commercially available aromatic polyamine mixtures identified three candidates that are similar in composition to AP-22.

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.

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