43,034 research outputs found

    CHLOROBENZENE AS A DIFFERENTIATING SOLVENT FOR THE OSCILLOMETRIC TITRATION OF WEAK ORGANIC BASES

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    Literature review of physical and chemical pretreatment processes for lignocellulosic biomass

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    Different pretreatment technologies published in public literature are described in terms of the mechanisms involved, advantages and disadvantages, and economic assessment. Pretreatment technologies for lignocellulosic biomass include biological, mechanical, chemical methods and various combinations thereof. The choice of the optimum pretreatment process depends very much on the objective of the biomass pretreatment, its economic assessment and environmental impact. Only a small number of pretreatment methods has been reported as being potentially cost-effective thus far. These include steam explosion, liquid hot water, concentrated acid hydrolysis and dilute acid pretreatments

    Atmospheric pressure gas chromatography-time-of-flight-mass spectrometry (APGC-ToF-MS) for the determination of regulated and emerging contaminants in aqueous samples after stir bar sorptive extraction (SBSE)

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    This work presents the development, optimization and validation of a multi-residue method for the simultaneous determination of 102 contaminants, including fragrances, UV filters, repellents, endocrine disruptors, biocides, polycyclic aromatic hydrocarbons (PAHs), polychlorinated biphenyls (PCBs), and several types of pesticides in aqueous matrices. Water samples were processed using stir bar sorptive extraction (SBSE) after the optimization of several parameters: agitation time, ionic strength, presence of organic modifiers, pH, and volume of the derivatizing agent. Target compounds were extracted from the bars by liquid desorption (LD). Separation, identification and quantification of analytes were carried out by gas chromatography (GC) coupled to time-of-flight (ToF-MS) mass spectrometry. A new ionization source, atmospheric pressure gas chromatography (APGC), was tested. The optimized protocol showed acceptable recovery percentages (50–100%) and limits of detection below 1 ng L−1 for most of the compounds. Occurrence of 21 out of 102 analytes was confirmed in several environmental aquatic matrices, including seawater, sewage effluent, river water and groundwater. Non-target compounds such as organophosphorus flame retardants were also identified in real samples by accurate mass measurement of their molecular ions using GC-APGC–ToF-MS. To the best of our knowledge, this is the first time that this technique has been applied for the analysis of contaminants in aquatic systems. By employing lower energy than the more widely used electron impact ionization (EI), AGPC provides significant advantages over EI for those substances very susceptible to high fragmentation (e.g., fragrances, pyrethroids)

    ECUT: Energy Conversion and utilization Technologies program biocatalysis research activity. Generation of chemical intermediates by catalytic oxidative decarboxylation of dilute organic acids

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    A rhodium-based catalyst was prepared and preliminary experiments were completed where the catalyst appeared to decarboxylate dilute acids at concentrations of 1 to 10 vol%. Electron spin resonance spectroscoy was used to characterize the catalyst as a first step leading toward modeling and optimization of rhodium catalysts. Also, a hybrid chemical/biological process for the production of hydrocarbons has been assessed. These types of catalysts could greatly increase energy efficiency of this process

    Monomers for thermosetting and toughening epoxy resins

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    Eight glycidyl amines were prepared by alkylating the parent amine with epichlorohydrin to form chlorohydrin, followed by cyclization with aqueous NaOH. Three of these compounds contained propargyl groups with postcuring studies. A procedure for quantitatively estimating the epoxy content of these glycidyl amines was employed for purity determination. Two diamond carbonates and several model propargly compounds were prepared. The synthesis of three new diamines, two which contain propargyloxy groups, and another with a sec-butyl group is in progress. These materials are at the dinitro stage ready for the final hydrogenation step. Four aromatic diamines were synthesized for mutagenic testing purposes. One of these compounds rapidly decomposes on exposure to air

    The CAMP-binding Ectoprotein from Saccharomyces cereuisiae Is Membrane-anchored by Glycosyl-Phosphatidylinositol

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    Saccharomyces cerevisiae contains an amphiphilic CAMP-binding glycoprotein at the outer face of the plasma membrane (M, = 54,000). It is converted to a hydrophilic form byt reatment withg lycosyl-phosphatidylinositol- specific phospholipases C and D (GPIPLC/ D), suggesting membrane anchorage by a covalently bound glycolipid. Determination of the constituents of the purified anchor by gas-liquid chromatography and amino acid analysis reveals the presence of glycerol, myo-inositol, glucosamine, galactose, mannose, ethanolamine, and asparagine (as the carboxylterminal amino acido f the Pronase-digested proteitno which the anchor is attached). Complementary results are obtained by metabolic labeling, indicating that fatty acids and phosphorus are additional anchor constituents. The phosphoruiss resistant to alkalinep hosphatase, whereas approximately half is lost from the protein after treatment with GPI-PLD or nitroaucisd , and all is removed by aqueous HF indicating the presence of two phosphodiester bonds. Inhibition of Nglycosylation by tunicamycin or removal of proteinbound glycan chains by N-glycanase or Pronase does not abolish radiolabeling of the anchor structure by any of the above compounds. Analysis of the products obtained after sequential enzymic and chemical degradation of the anchor agrees with the arrangemoefn t constitutents in GPIs from higher eucaryotes. Evidence for anchorage of the yeast CAMP-binding protein by a GPI anchoris strengthened additionallyb y the reactivity of the GPI-PLC-cleaved anchor with antibodies directed against the cross-reacting determinoaf nttr ypanosomal variant surface glycoproteins

    Extraction Methods and an Investigation of Drosophila Lipids

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    In earlier work (8) we extracted lipids from dried, macerated Drosophila melanogaster with ether, but later, working with larger quantities of undried flies, we found that most of the phospholipids were autolyzed. Kates' studies (2) led him to suggest n-propanol or isopropanol for lipid extraction (isopropanol was his later choice (6, 7)). Attempting to meet the requirements discussed above, we developed a new and relatively simple method of extraction employing n-propanol (9), or chloroformmethanol (2:1). The latter proved to be a more useful solvent. The method will be described in detail below, with results of an examination of Drosophila lipids

    Determination of Pharmaceuticals in Coastal Systems Using Solid Phase Extraction (SPE) Followed by Ultra Performance Liquid Chromatography – tandem Mass Spectrometry (UPLC-MS/MS)

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    This paper describes the optimization and validation of an analytical method for the determination of 83 pharmaceutically active compounds (PhACs) in aqueous samples using solid-phase extraction (SPE) followed by ultra performance liquid chromatography-triple quadrupole mass spectrometry (UPLC-QqQ-MS/MS). First, several experiments were conducted to optimize different SPE extraction parameters such as pH, elution solvents, and Na2EDTA addition. Extraction recovery percentages were between 17 and 146%, being higher than 70% for 47 target analytes. The effect of salinity in the extraction efficiency proved to be negligible ( 90%), and the precision of the method, calculated as the relative standard deviation (RSD) of replicate extractions and analyses, was less than 20%. The optimized method was successfully applied to the analysis of real water samples in estuarine and coastal systems from SW Spain (Cadiz Bay and Huelva Estuary). 49 out of 83 target compounds were found in 75% of samples. Ibuprofen, atenolol, gemfibrozil and caffeine were the most commonly detected substances, reaching concentrations up to 195 ng L-1

    Designing optimal mixtures using generalized disjunctive programming: Hull relaxations

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    A general modeling framework for mixture design problems, which integrates Generalized Disjunctive Programming (GDP) into the Computer-Aided Mixture/blend Design (CAMbD) framework, was recently proposed (S. Jonuzaj, P.T. Akula, P.-M. Kleniati, C.S. Adjiman, 2016. AIChE Journal 62, 1616–1633). In this paper we derive Hull Relaxations (HR) of GDP mixture design problems as an alternative to the big-M (BM) approach presented in this earlier work. We show that in restricted mixture design problems, where the number of components is fixed and their identities and compositions are optimized, BM and HR formulations are identical. For general mixture design problems, where the optimal number of mixture components is also determined, a generic approach is employed to enable the derivation and solution of the HR formulation for problems involving functions that are not defined at zero (e.g., logarithms). The design methodology is applied successfully to two solvent design case studies: the maximization of the solubility of a drug and the separation of acetic acid from water in a liquid-liquid extraction process. Promising solvent mixtures are identified in both case studies. The HR and BM approaches are found to be effective for the formulation and solution of mixture design problems, especially via the general design problem
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