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Mixture Used (mixture + used)
Selected AbstractsMolecular mass ranges of coal tar pitch fractions by mass spectrometry and size-exclusion chromatographyRAPID COMMUNICATIONS IN MASS SPECTROMETRY, Issue 13 2009F. Karaca A coal tar pitch was fractionated by solvent solubility into heptane-solubles, heptane-insoluble/toluene-solubles (asphaltenes), and toluene-insolubles (preasphaltenes). The aim of the work was to compare the mass ranges of the different fractions by several different techniques. Thermogravimetric analysis, size-exclusion chromatography (SEC) and UV-fluorescence spectroscopy showed distinct differences between the three fractions in terms of volatility, molecular size ranges and the aromatic chromophore sizes present. The mass spectrometric methods used were gas chromatography/mass spectrometry (GC/MS), pyrolysis/GC/MS, electrospray ionization Fourier transform ion cyclotron resonance mass spectrometry (ESI-FTICRMS) and laser desorption time-of-flight mass spectrometry (LD-TOFMS). The first three techniques gave good mass spectra only for the heptane-soluble fraction. Only LDMS gave signals from the toluene-insolubles, indicating that the molecules were too involatile for GC and too complex to pyrolyze into small molecules during pyrolysis/GC/MS. ESI-FTICRMS gave no signal for toluene-insolubles probably because the fraction was insoluble in the methanol or acetonitrile, water and formic acid mixture used as solvent to the ESI source. LDMS was able to generate ions from each of the fractions. Fractionation of complex samples is necessary to separate smaller molecules to allow the use of higher laser fluences for the larger molecules and suppress the formation of ionized molecular clusters. The upper mass limit of the pitch was determined as between 5000 and 10,000,u. The pitch asphaltenes showed a peak of maximum intensity in the LDMS spectra at around m/z 400, in broad agreement with the estimate from SEC. The mass ranges of the toluene-insoluble fraction found by LDMS and SEC (400,10,000,u with maximum intensity around 2000,u by LDMS and 100,9320,u with maximum intensity around 740,u by SEC) are higher than those for the asphaltene fraction (200,4000,u with maximum intensity around 400,u by LDMS and 100,2680,u with maximum intensity around 286,u by SEC) and greater than values considered appropriate for petroleum asphaltenes (300,1200,u with maximum intensity near 700,u). Copyright © 2009 John Wiley & Sons, Ltd. [source] A comparative geochemical study of bituminous boat remains from H3, As-Sabiyah (Kuwait), and RJ-2, Ra's al-Jinz (Oman)ARABIAN ARCHAEOLOGY AND EPIGRAPHY, Issue 1 2005Jacques Connan This paper presents a geochemical analysis of fragments of bituminous amalgam from H3, As-Sabiyah (Kuwait), and RJ-2, Ra's al-Jinz (Oman). The fragments bear barnacles on one side and reed impressions on the other, and are thought to have been part of the coating of reed-bundle boats. The material from H3 dates to between 5300,4900 BC, while that of RJ-2 dates to 2500,2100 BC. Samples from both sites were geochemically compared to archaeological and ethnographic material from Kosak Shamali (northern Syria, c.5000,4400 BC), RH-5 (Oman, 4400,3500 BC) and Baghdad (central Iraq, 1900 AD). The composition of the bituminous amalgams was studied in detail. Rock-Eval Pyrolysis gave a measure of Total Organic Carbon in the samples, and allowed an initial comparison of the data sets using various parameters. Examination of the proportions of soluble and insoluble organic matter allowed an assessment of the quantity of vegetal matter added to the bitumen to make the bituminous amalgam. The composition of the Ra's al-Jinz material was studied using X-Ray Diffraction analysis and thin-section petrography, in order to assess the proportions of various minerals in the bituminous amalgams. It was concluded that the recipe for the bituminous mixture used to coat reed-bundle and wooden boats did not differ significantly from that commonly used to make ,mortar' for architectural purposes in Mesopotamia. Traces of animal fats or fish oils were not found in the analysed Ra's al-Jinz material, in contrast to previous hypotheses regarding the composition of the mixture. Comparison of the gross composition of extractable organic matter (the constituents of pure bitumen, soluble in chloroform or dichloromethane) showed the progressive effects of weathering on the samples. The isotopic composition of the bituminous material from H3 and the other sites was then compared to that of bitumen seeps and crude oils from Mesopotamia, Iran and Oman. The most significant result is that the material from As-Sabiyah originated in Kuwait, at a surface seep at Burgan, while the material from Ra's al-Jinz had a source in northern Mesopotamia. [source] Analysis of neuroactive amino acids from microdialysate samples by fluorescence detection using a modification of the 6-aminoquinolyl- N -hydroxysuccinimidyl carbamate methodBIOMEDICAL CHROMATOGRAPHY, Issue 10 2005M. Teresa Oreiro-García Abstract A sensitive and rapid reversed-phase high-performance liquid chromatographic method using pre-column derivatization with 6-aminoquinolyl- N -hydroxysuccinimidyl carbamate (AQC) and fluorescence detection is reported. By directly derivatizing microdialysate samples with AQC, an automatic and rapid simultaneous measurement of aspartate, serine, glutamate, glycine and histidine was developed. Excellent linearity (r2 , 0.998) was achieved for the standard mixture used for the validation experiments. Within-day and between-day precision was less than 6.2%, and the accuracy ranged from 95 to 105.2% in standards. This method is suitable for single run analysis of a high number of small volume microdialysate samples from rat hippocampus. Amino acids from microdialysate samples were quantified with RSD for reproducibility below 2%, and at approximately 0.1% for retention time. Copyright © 2005 John Wiley & Sons, Ltd. [source] AN ESTEROLYTIC ACTIVITY FROM A WILD EDIBLE MUSHROOM, LYCOPERDON PERLATUMJOURNAL OF FOOD BIOCHEMISTRY, Issue 4 2009AHMET COLAK ABSTRACT Lycoperdon perlatum Pers. (Lycoperdaceae, Agaricales, Agaricomycetidae, Agaricomycetes, Basidiomycota, Fungi) was evaluated for its esterolytic potential. Native electrophoresis of the crude extracts showed four bands having Rf values of 0.34, 0.39, 0.52 and 0.59. The esterase showed the highest activity toward a short-chain substrate, p -nitrophenyl acetate. Optimum reaction conditions for L. perlatum crude extract were attained at pH 8.0 and 40C. Esterolytic activity of enzyme extract was stimulated in the presence of Mn2+, Fe2+, Ca2+ and Zn2+ in the reaction mixture. The enzyme activity was stimulated by incubation at pH 6.0 but retained 77% of its original activity at its optimum pH after 24 h. Thermal inactivation was displayed after incubation for 20 min at various temperatures above 30C. At 1 mM final concentration, 2-mercaptoethanol, dithiothreitol, ethylenediamine tetraacetic acid and p -methylphenyl sulfonylfluoride inhibited the esterolytic reaction. These results support that the crude L. perlatum extract possesses an esterolytic activity having properties similar to other esterases. PRACTICAL APPLICATIONS Esterases catalyzing the cleavage and formation of ester bonds are known ,/,-hydrolases (EC 3.1.1.X). Esterases are used for the synthesis of flavor esters for the food industry, modification of triglycerides for fat and oil industry and resolution of racemic mixtures used for the synthesis of fine chemicals for the pharmaceutical industry. Therefore, the search for new enzyme sources is important for the development of new enzymes and applications. [source] Preparation and characterization of poly(butylene terephthalate)/poly(ethylene terephthalate) copolymers via solid-state and melt polymerizationJOURNAL OF POLYMER SCIENCE (IN TWO SECTIONS), Issue 5 2007M. A. G. Jansen Abstract To increase the Tg in combination with a retained crystallization rate, bis(2-hydroxyethyl)terephthalate (BHET) was incorporated into poly(butylene terephthalate) (PBT) via solid-state copolymerization (SSP). The incorporated BHET fraction depends on the miscibility of BHET in the amorphous phase of PBT prior to SSP. DSC measurements showed that BHET is only partially miscible. During SSP, the miscible BHET fraction reacts via transesterification reactions with the mobile amorphous PBT segments. The immiscible BHET fraction reacts by self-condensation, resulting in the formation of poly(ethylene terephthalate) (PET) homopolymer. 1H-NMR sequence distribution analysis showed that self-condensation of BHET proceeded faster than the transesterification with PBT. SAXS measurements showed an increase in the long period with increasing fraction BHET present in the mixtures used for SSP followed by a decrease due to the formation of small PET crystals. DSC confirmed the presence of separate PET crystals. Furthermore, the incorporation of BHET via SSP resulted in PBT-PET copolymers with an increased Tg compared to PBT. However, these copolymers showed a poorer crystallization behavior. The modified copolymer chain segments are apparently fully miscible with the unmodified PBT chains in the molten state. Consequently, the crystal growth process is retarded resulting in a decreased crystallization rate and crystallinity. © 2007 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem 45: 882,899, 2007. [source] Mammals, agri-environment schemes and set-aside , what are the putative benefits?MAMMAL REVIEW, Issue 4 2007D. W. MACDONALD ABSTRACT 1The impacts of agricultural intensification on farmland wildlife have been the subject of increasing concern, particularly over the last two decades. Population declines have occurred for a number of mammalian species, sometimes drastically so, and changes in farming practice are believed to be significant contributory factors. 2The major policy instruments for delivering environmental benefits on farmland are agri-environment schemes. These encourage farmers to adopt more environmentally sensitive farming practices to promote farmland biodiversity. Additionally, compulsory set-aside, which reduces agricultural surplus, could also have positive impacts on wildlife. In this paper we consider some of the putative benefits of agri-environment schemes and set-aside for mammals. 3We review how establishment and management options within agri-environment schemes and set-aside might affect habitat resources for mammals. For example, conservation headlands increase plant and invertebrate resources within the crop edge for mammals such as wood mice. Grassy field margins can support communities of smaller mammals, and hedgerows may act as important commuting and hunting routes. Their potential will depend on factors such as seed mixtures used, timing and severity of cutting, and length of time they have been in place. 4At a farm level, habitat heterogeneity may be increased through organic agriculture, which is supported by some agri-environment schemes. Studies suggest significant benefits to mammals, including wood mice and bats. However, it is increasingly recognized that effective conservation of farmland mammals must seek solutions at the landscape scale, addressing such issues as habitat connectivity between farms. One approach may be the better targeting of scheme agreements. 5We suggest that agri-environment schemes and set-aside can contribute to the conservation of mammals on farmland. Recent policy changes are likely to have further positive impacts on farmland wildlife but appropriate mammal monitoring programmes must be developed rigorously to assess their effects. [source] | ||||||||||