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Search indexed NASA NTRS and DOE OSTI research on propulsion, heat transfer, battery materials and energy systems. Follow report and document links to the original sources.

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At least 181 records · Page 10
All sourcesNASA NTRSDOE OSTI
DOE OSTI2021

Synthesis and Advanced Characterization of Polymer–Protein Core–Shell Nanoparticles

Enzyme immobilization techniques are widely researched due to their wide range of applications. Polymer–protein core–shell nanoparticles (CSNPs) have emerged as a promising technique for enzyme/protein immobilization via a self-assembly process. Based on the desired application, different sizes and distribution of the polymer–protein CSNPs may be required. This work systematically studies the assembly process of poly(4-vinyl pyridine) and bovine serum albumin CSNPs. Average particle size was controlled by varying the concentrations of each reagent. Particle size and size distributions were monitored by dynamic light scattering, ultra-small-angle X-ray scattering, small-angle X-ray scattering and transmission electron microscopy. Results showed a wide range of CSNPs could be assembled ranging from an average radius as small as 52.3 nm, to particles above 1 µm by adjusting reagent concentrations. In situ X-ray scattering techniques monitored particle assembly as a function of time showing the initial particle growth followed by a decrease in particle size as they reach equilibrium. The results outline a general strategy that can be applied to other CSNP systems to better control particle size and distribution for various applications.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
DOE OSTI2023

Triphenylborane in Metal-Free Catalysis

The development and application of new organoboron reagents as Lewis acids in synthesis and metal-free catalysis have dramatically expanded over the past 20 years. In this context, we will show the recent uses of the simple and relatively weak Lewis acid BPh 3 —discovered 100 years ago—as a metal-free catalyst for various organic transformations. The first part will highlight catalytic applications in polymer synthesis such as the copolymerization of epoxides with CO 2 , isocyanate, and organic anhydrides to various polycarbonate copolymers and controlled diblock copolymers as well as alternating polyurethanes. This is followed by a discussion of BPh 3 as a Lewis acid component in the frustrated Lewis pair (FLP) mediated cleavage of hydrogen and hydrogenation catalysis. In addition, BPh 3 -catalyzed reductive N-methylations and C-methylations with CO 2 and silane to value-added organic products will be covered as well along with BPh 3 -catalyzed cycloadditions and insertion reactions. Collectively, this mini-review showcases the underexplored potential of commercially available BPh3 in metal-free catalysis.

Lewis acid↗
DOE OSTI2022

Dihydrooxazine Byproduct of a McMurry–Melton Reaction en Route to a Synthetic Bacteriochlorin

A synthetic route to gem-dimethyl-substituted bacteriochlorins—models of native bacteriochlorophylls—relies on the formation of a dihydrodipyrrin precursor via a series of established reactions: van Leusen pyrrole formation, Vilsmeier formylation, Henry reaction, borohydride reduction, Michael addition, and McMurry–Melton pyrroline formation. The latter is the least known of the series. Here, the McMurry–Melton reaction of a 2-(6-oxo-2-nitrohexyl)pyrrole in the presence of TiCl3 and an ammonium acetate buffer formed the expected Δ1-pyrroline, as well as an unexpected polar, cyclic byproduct (a 5,6-dihydro-4H-1,2-oxazin-6-ol), each attached to the 2-methylpyrrole unit. Both species were characterized by single-crystal X-ray diffraction. The McMurry–Melton reaction is a type of intercepted Nef reaction (the transformation of a nitroalkyl motif into a carbonyl group), where both the Δ1-pyrroline and the dihydrooxazine derive from the reaction of the nitrogen derived from the nitro group upon complete or partial reductive deoxygenation, respectively, with the γ-keto group. The report also considers competing Nef and McMurry–Melton reactions, the nature of available TiCl3 reagents, and the use of ammonium acetate for buffering the TiCl3/HCl reagent.

Tran, Vy-Phuong↗
DOE OSTI2024

Online characterization of primary and secondary emissions of particulate matter and acidic molecules from a modern fleet of city buses

The potential impact of transitioning from conventional fossil fuel to a non-fossil-fuel vehicle fleet was investigated by measuring primary emissions via extractive sampling of bus plumes and assessing secondary mass formation using the Gothenburg Potential Aerosol Mass (Go:PAM) reactor from 76 in-use transit buses. Online chemical characterization of gaseous and particulate emissions from these buses was conducted using chemical ionization mass spectrometry (CIMS) with acetate as the reagent ion, coupled with the Filter Inlet for Gases and AEROsols (FIGAERO). Acetate reagent ion chemistry selectively ionizes acidic compounds, including organic and inorganic acids, as well as nitrated and sulfated organics. A significant reduction (48 %–98 %) in fresh particle emissions was observed in buses utilizing compressed natural gas (CNG), biodiesels like rapeseed methyl ester (RME) and hydrotreated vegetable oil (HVO), and hybrid-electric HVO (HVO HEV ) compared to diesel (DSL). However, secondary particle formation from photooxidation of emissions was substantial across all the fuel types. The median ratio of particle mass emission factors of aged to fresh emissions increased in the following order: DSL buses at 4.0, HVO buses at 6.7, HVO HEV buses at 10.5, RME buses at 10.8, and CNG buses at 84. Of the compounds that can be identified by CIMS, fresh gaseous emissions from all Euro V/EEV (Enhanced Environmentally friendly Vehicle) buses, regardless of fuel type, were dominated by nitrogen-containing compounds such as nitrous acid (HONO), nitric acid (HNO 3 ), and isocyanic acid (HNCO), alongside small monoacids (C 1 –C 3 ). Notably, the emission of nitrogen-containing compounds was lower in Euro VI buses equipped with more advanced emission control technologies. Secondary gaseous organic acids correlated strongly with gaseous HNO 3 signals (R 2 =0.85–0.99) in Go:PAM, but their moderate to weak correlations with post-photooxidation secondary particle mass suggest that they are not reliable tracers of secondary organic aerosol formation from bus exhaust. Our study highlights that non-regulated compounds and secondary pollutant formation, not currently addressed in legislation, are crucial considerations in the evaluation of environmental impacts of future fuel and engine technology shifts.

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CH↗
NASA NTRS1972

Development of self extinguishing Durette and/or Nomex fabric

A treatment was developed for Nomex or Durette fabric which renders it self-extinguishing in a 70% oxygen, 30% nitrogen atmosphere at 5 psia. The treatment does not degrade the physical and textile properties of the fabric excessively and does not outgas or have an objectional odor. The treatment is permanent and does not lose its fire protecting qualities after laundering. The treatment utilizes a mixture of formaldehyde, phosphorous acid, and tri-methyl phosphate in methanol. The cloth to be treated is held in a boiling solution of the above reagents for 24 hours, removed, air dried, and then heated to 120 C in a circulating air oven for 90 minutes. The treatment turns Nomex a pale yellow but does not have an appreciable effect on drape or hand. One inch wide strips of treated cloth failed in tension at 192 lbs, while untreated controls broke at 215 lbs. To remove any excess reagents, the cloth is processed in a home laundry through one wash and dry cycle without the use of any detergents. The thermal shrinkage of the treated material is 23% compared to a control of 40% for unwashed Stern Nomex HT 90-40.

Source record↗
NASA NTRS1972

An investigation of the preparation of high molecular weight perfluorocarbon polyethers

High molecular weight perfluorocarbon polyether gums were obtained by photolysis of perfluorodienes and discyl fluorides containing a perfluorocarbon polyether backbond. The materials obtained are represented by chemical formulas. A method was developed whereby reactive acyl fluoride and trifluorovinyl end groups are converted into inert structures. In order to investigate the possible preparation of difunctional molecules which may be useful in polymer synthesis, the reactions of hexafluoropropene oxide (HFPO) with Grignard and organolithium reagents have been studied. Reactions of various nucleophilic reagents with HFPO were also investigated.

Watts, R. O.↗
NASA NTRS1975

Water system virus detection

A monitoring system developed to test the capability of a water recovery system to reject the passage of viruses into the recovered water is described. A nonpathogenic marker virus, bacteriophage F2, is fed into the process stream before the recovery unit and the reclaimed water is assayed for its presence. Detection of the marker virus consists of two major components, concentration and isolation of the marker virus, and detection of the marker virus. The concentration system involves adsorption of virus to cellulose acetate filters in the presence of trivalent cations and low pH with subsequent desorption of the virus using volumes of high pH buffer. The detection of the virus is performed by a passive immune agglutination test utilizing specially prepared polystyrene particles. An engineering preliminary design was performed as a parallel effort to the laboratory development of the marker virus test system. Engineering schematics and drawings of a fully functional laboratory prototype capable of zero-G operation are presented. The instrument consists of reagent pump/metering system, reagent storage containers, a filter concentrator, an incubation/detector system, and an electronic readout and control system.

Fraser, A. S.↗
NASA NTRS1975

Development of a chemiluminescent and bioluminescent system for the detection of bacteria in wastewater effluent

Automated chemiluminescent and bioluminescent sensors were developed for continuous monitoring of microbial levels in wastewater effluent. Development of the chemiluminescent system included optimization of reagent concentrations as well as two new techniques which will allow for increased sensitivity and specificity. The optimal reagent concentrations are 0.0025 M luminol and 0.0125 M sodium perborate in 0.75N sodium hydroxide before addition of sample. The methods developed to increase specificity include (1) extraction of porphyrins from bacteria collected in a filter using 0.1N NaOH - 50 percent Ethanol, and (2) use of the specific reaction rate characteristics for the different luminol catalysts. Since reaction times are different for each catalyst, the reaction can be made specific for bacteria by measuring only the light emission from the particular reaction time zone specific for bacteria. Developments of the bioluminescent firefly luciferase system were in the area of flow system design.

Thomas, R. R.↗
NASA NTRS1975

Automated single-slide staining device

An automatic single-slide Gram staining device is described. A timer-actuated solenoid controls the dispensing of gentian violet, Gram iodine solution, decolorizer, and 1% aqueous safranin in proper sequence and for the time required for optimum staining. The amount of stain or reagent delivered is controlled by means of stopcocks below each solenoid. Used stains and reagents can be flushed automatically or manually. Smears Gram stained automatically are equal in quality to those prepared manually. The time to complete one Gram cycle is 4.80 min.

Wilkins, J. R.↗
NASA NTRS1976

Functional colloidal particles for immunoresearch

The paper deals with the development of a new class of immunological reagents consisting of antibodies covalently bonded to polymeric microspheres to serve as convenient markers for detection of cell surface antigens by scanning electron and light microscopy. Attention is focused on the design and synthesis of spherical particles containing hydroxyl and carboxyl groups on their surface in a wide range of sizes (30-340 nm diam) by emulsion copolymerization, the preparation of spherical particles ranging from 300 nm to 3 microns and containing a variety of functional groups by means of ionizing radiation, and the experimental conditions for the covalent bonding of fluorescent molecules and antibodies to the spheres by means of the cyanogen bromide, carbodiimide and glutaraldehyde methods. These reagents are used to locate antigens on red blood cells, on mouse and human lymphocytes, and on the surface of photoreceptors. They offer a number of advantages and applications for the study of cell surfaces for immunodiagnosis.

Yen, S. P. S.↗
NASA NTRS1978

Measurement of total organic concentration in water

Instrument for determining total organic concentration in water uses no corrosive reagents or gases. Instead continuous ultraviolet photolysis process converts organic compounds to carbon dioxide (CO2). CO2 electrode is used to measure CO2 content. Only reagent necessary is oxygen, generated in situ by electrolyzing some water. In addition to application in aerospace industry, system has potential uses in pollution monitoring and in laboratory analyses.

Winkler, E.↗
NASA NTRS1979

Overview of methods for extraterrestrial materials processing

A brief survey of processing systems suitable for conversion of lunar soil fractions to refined industrial feedstocks are given. Description of a 'baseline' process using hydrochemical or metallurgical separation of compounds of major and minor elements using HF acid leaching as the initial step is presented. Rough engineering parameters including power and heat rejection requirements, potential loss of earth supplied reagents during recycling, and mass: output ratios of equipment, reagent inventory, and associated power and radiator facilities are described. Minimal practical scales for such systems and manpower requirements are discussed.

Waldron, R. D.↗
NASA NTRS1980

Silicon halide-alkali metal flames as a source of solar grade silicon

The feasibility of using continuous high-temperature reactions of alkali metals and silicon halides to produce silicon in large quantities and of suitable purity for use in the production of photovoltaic solar cells was demonstrated. Low pressure experiments were performed demonstrating the production of free silicon and providing experience with the construction of reactant vapor generators. Further experiments at higher reagent flow rates were performed in a low temperature flow tube configuration with co-axial injection of reagents and relatively pure silicon was produced. A high temperature graphite flow tube was built and continuous separation of Si from NaCl was demonstrated. A larger scaled well stirred reactor was built. Experiments were performed to investigate the compatability of graphite based reactor materials of construction with sodium. At 1100 to 1200 K none of these materials were found to be suitable. At 1700 K the graphites performed well with little damage except to coatings of pyrolytic graphite and silicon carbide which were damaged.

Olson, D. B.↗
NASA NTRS1976

Research in acetylene containing monomers

The preparation of precursor bisbenzils with pendant acetylene linkages for use in the synthesis of new aromatic poly (phenyl quinoxalines) was investigated. Attempts to condense para, para prime-dibromo benzil and potassium acetylide in liquid ammonia and in toluene, to prepare 4-phenyl acetyl phenyl ether, 4-(paraacetylphenyl) acetyl phenyl ether, 4-phenyl acetyl-4 primeacetyl phenyl acetyl phenyl ether, the reaction of 4-phenyl acetyl phenyl ether with Villsmeier reagent to prepare 4-(beta-chloro cinnamaldehyde) phenyl ether, the reaction of 4-(para-acetyl phenyl) acetyl phenyl ether with Villsmeier reagent, and the oxidation of bibenzil to prepare benzil are described. The reactions of phenyl acetylene with oxidizing agent, of phenyl acetylene with bromine, of 1,1,2,2-tetrabromo ethyl benzene with zinc and with oxidizing agent are described.

Ogliaruso, M. A.↗
NASA NTRS1982

Method of neutralizing the corrosive surface of amine-cured epoxy resins

The corrosive alkaline surface layer of an epoxy resin product formed by the curing of the epoxy with an aliphatic amine is eliminated by first applying a non-solvent to remove most or all of the free unreacted amine and then applying a layer of a chemical reagent to neutralize the unused amine or amine functional groups by forming a substituted urea. The surface then may be rinsed with acetone and then with alcohol. The non-solvent may be an alcohol. The neutralizing chemical reagent is a mono-isocyanate or a mono-isothiocyanate. Preferred is an aromatic mono-isocyanate such as phenyl isocyanate, nitrophenyl isocyanate and naplthyl isocyanate.

Lee, S. Y.↗
NASA NTRS1986

Tropospheric HO2 determination by FAGE

The detection efficiency is greatest at low pressures, where the subsequent removal of the HO product by the NO reagent (via HO + NO + M yields HONO + M) is relatively slow. Moreover, nozzle expansion of the air from ambient to low pressures produces a turbulent zone that assists in mixing the reagent with the sample. If the HO product is observed by laser-excited fluorescence, then the other advantages of low-pressure detection by FAGE (Fluorescence Assay with Gas Expansion) also apply. The FAGE instrumental response was calibrated to external HO2 by observing NO decay in the photolysis of HO-CH2O mixtures and by choosing conditions in which HO2 + NO is the only significant NO destruction path. HO2 was determined in urban air.

Obrien, R. J.↗
NASA NTRS1988

Deuterium exchange during acid-demineralisation

Isotopic analyses of residues prepared by demineralization of the Murchison meteorite using D-labelled reagents provide evidence for measurable exchange of H-isotopes between residue and reagents. Precise quantification of this effect is precluded by substantial inhomogeneity of the meteoritic organic matter. A conservative estimate of the degree of exchange is 3-5 percent of the H pyrolyzable as H2O. This could affect the shape of the curve defining D release as a function of temperature, but does not change conclusions previously drawn concerning the nature of the bulk D enrichment of insoluble organic matter in meteorites.

Kerridge, John F.↗
NASA NTRS1990

Prepenetrant Etchant For Incology(R) 903 Weld Overlays

Etching solution developed for use prior to type-IVc penetrant inspection of Incology(R) 903 weld overlays. Formulated as follows: 80 g ferric chloride hexahydrate, 300 mL reagent-grade hydrochloric acid, 25 mL food- or reagent-grade phosphoric acid, and 100 mL ethylene glycol. Gives more reasonable range of etching time and reduces probability of overetching and resulting damage. Stored indefinitely.

O'Tousa, Joseph E.↗