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  • Polymer and Materials Science  (112.478)
  • Nuclear reactions  (4.460)
  • Gas chromatography
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  • 1
    Digitale Medien
    Digitale Medien
    Identification of rumanite (Romanian amber) as thermally altered succinite (Baltic amber) (2000)
    Springer
    Physics and chemistry of minerals 27 (2000), S. 665-678 
    Details
    ISSN: 1432-2021
    Schlagwort(e): Key words Amber ; Rumantite ; Succinite ; Pyrolysis ; Gas chromatography ; Mass spectrometry
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie , Geologie und Paläontologie , Physik
    Notizen: Abstract  Romanian amber (rumanite) has been considered to be a separate species of fossil resin for more than a century. While earlier investigators held it to be very similar to succinite (Baltic amber), modern scholars have assigned it a distinctly different botanical origin. We have found that almost all of the constituents of the ether-soluble fractions of 13 specimens of authentic rumanite identified by gas chromatography–mass spectrometry have previously been reported in the soluble fraction of succinite, including succinic acid and its monoterpene esters. Additionally and significantly, the soluble fraction of rumanite contains a number defunctionalized compounds that do not preexist in succinite, but that are produced by pyrolysis of whole succinite or of its insoluble polymeric fraction. Simultaneous methylation pyrolysis–gas chromatography–mass spectrometry of the polymeric fraction of seven of the rumanite specimens yielded further copious amounts of dimethyl succinate, a number of diterpene resin acid methyl esters, and additional defunctionalized compounds known to be pyrolysis products of succinite. The evidence shows conclusively that the botanical origin of rumanite is not distinct from that of succinite. Rather, rumanite is a succinite that has suffered partial thermal degradation in the course of the folding of the Oligocene Kliwa sandstone formation in which it is most commonly found.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/s002690000111
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  • 2
    Digitale Medien
    Digitale Medien
    Isolation and identification of odorants generated in wine during its oxidation: a gas chromatography–olfactometric study (2000)
    Springer
    European food research and technology 211 (2000), S. 105-110 
    Details
    ISSN: 1438-2385
    Schlagwort(e): Key words Wine ; Flavor ; Oxidation ; Aroma ; Gas chromatography ; olfactometry
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Werkstoffwissenschaften, Fertigungsverfahren, Fertigung
    Notizen: Abstract  The changes in the flavor profiles of several white wines undergoing oxidation were monitored through gas chromatography–olfactometry (GCO). The study showed that up to 19 odorants were generated during wine oxidation, and that several of the odorants originally present in the wine disappeared or decreased. An aroma extract dilution analysis revealed that 5 of these 19 odorants have maximum dilution factors, and that a second group of 7 may have some sensory significance as well. The isolation and identification of the different odorants was achieved via normal and reverse-phase high-performance liquid chromatography and high-resolution GCO. The impact odorants of oxidized wine were found to be 2, 4, 5-trimethyldioxolane, methional (methylthiopropanal), sotolon (4,5-dimethyl-3-hydroxy-2(5H)-furanone), eugenol (4-propenyl-2-methoxyphenol) and an unknown compound with mass spectrum similar to methylvanillate. Other odorants also formed during wine oxidation were 1-octen-3-ol, t-2-nonenal, furfural, benzaldehyde, 2-butoxyethanol, acetovanillone and a dioxolane isomer.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/s002179900128
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  • 3
    Digitale Medien
    Digitale Medien
    Determination of nitric oxide metabolites by means of the Griess assay and gas chromatography–mass spectrometry in the cavernous and systemic blood of healthy males and patients with erectile dysfunction during different functional conditions of the penis (2000)
    Springer
    Urological research 28 (2000), S. 364-369 
    Details
    ISSN: 1434-0879
    Schlagwort(e): Key words Nitric oxide metabolites ; Erectile dysfunction ; Griess reaction ; Gas chromatography ; Mass spectrometry
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract Recent research implicated that the relaxation of cavernous arterial and trabecular smooth muscle – the crucial event in penile erection – is initiated by the release of nitric oxide (NO) from nerve terminals within the cavernous tissue as well as from the endothelia that line the lacunar spaces and the intima of penile arteries. The present study was undertaken to determine whether plasma levels of the NO metabolites nitrate (NO− 3) and nitrite (NO− 2) in the systemic and cavernous blood of male subjects change during different penile conditions, and whether there is a difference in the NO− 3 and NO− 2 levels of normal males and patients with erectile dysfunction (ED). Twenty-four potent adult male volunteers and 15 patients with ED were exposed to visual and tactile erotic stimuli in order to elicit penile tumescence and, in the group of healthy volunteers, rigidity. Whole blood was aspirated from the corpus cavernosum and the cubital vein, and NO− 3 and NO− 2 levels were determined in plasma aliquots by means of the Griess reaction and a method combining gas chromatography and mass spectrometry (GC-MS). The mean systemic and cavernous plasma NO3 −/NO2 − level in blood samples obtained from the healthy volunteers was 25–31 μM when determined by means of the Griess reaction and 37–41 μM when measured by GC-MS. Both approaches revealed that NO3 −/NO2 − levels in the peripheral and cavernous blood do not change appreciably during developing erection, rigidity and detumescence. Moreover, no significant differences were found between NO3 −/NO2 − plasma levels in the systemic and cavernous blood samples taken from the normal subjects and patients during penile flaccidity, tumescence and detumescence. Our results may reflect the fact that NO metabolism in the corpora cavernosa in the phases of penile tumescence and rigidity may account for only a minor fraction of local levels of NO3 − and NO2 −, which may also derive from exogenous sources. Moreover, the basal levels of NO metabolites in the blood flushing the lacunar spaces of the cavernous body in the state of developing erection could conceal any release of NO that may occur within the penile tissue. Thus, we conclude that the quantification of NO metabolites by means of advanced detection methods, such as GC-MS, is of no use in the workup of ED.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/s002400000141
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  • 4
    Digitale Medien
    Digitale Medien
    Solution-Phase Synthesis of Mixed Amide Libraries by Simultaneous Addition of Functionalities (SPSAF) to a Diketopiperazine Tetracarboxylic Acid Scaffold Monitored by GC Analysis of Isobutyl Alcohol (2000)
    Weinheim : Wiley-Blackwell
    Liebigs Annalen 2000 (2000), S. 1669-1675 
    Details
    ISSN: 1434-193X
    Schlagwort(e): Combinatorial chemistry ; Amides ; Gas chromatography ; Chemistry ; General Chemistry
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A symmetric diketopiperazine scaffold 2 has been prepared in a very simple two-step procedure from L-aspartic acid dimethyl ester. This product (a tetracarboxylic acid equally protected at the two symmetric positions) has been employed as a template for the synthesis of mixed amide libraries in the solution phase using the SPSAF (simultaneous addition of functionalities) strategy. By judicious choice of the amines employed, it is possible to prepare parallel libraries containing hundreds of products using just a small number of different amines. We have also developed a simple method for monitoring the required conversion of the acid into amides based on an assay of the amount of iBuOH (determined by GC) formed during the coupling mediated by isobutyl chloroformate. We have observed that a conversion higher than 90% (iBuOH by GC) guarantees correct formation of the desired amides. This indirect method for assessing the conversion in a combinatorial reaction employing mixed reactants (SPSAF) can conveniently be used for the routine determination of libraries prepared in the solution phase. In a broader perspective, the present results contribute as a further step in the development of new and simple systems for monitoring the progress and evolution of combinatorial reactions
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 5
    Digitale Medien
    Digitale Medien
    Note on the Net Retention Volume in Chromatography with a Real Gas as a Carrier (2000)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 23 (2000), S. 119-126 
    Details
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; retention volume ; real gas carrier ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The problem of the calculation and interpretation of the net retention volume with a real gas as carrier is revisited. The properties of the carrier are described by a first order virial equation of state. The net retention volume of a solute is related to the mean flow rate of the carrier, therefore determination of the mean flow rate of a real gas carrier is reviewed. It is shown that the mean flow rate cannot be calculated from the mean column pressure. With a real gas carrier the local capacity factor depends on the local pressure of the real gas. The basic relationship between the net retention volume and the function describing this pressure dependence is also reviewed. Precise formulae as well as practical approximations are presented for the calculation of the mean flow rate, of the mean column pressure, and of a representative pressure related to the mean capacity factor.
    Zusätzliches Material: 3 Tab.
    Materialart: Digitale Medien
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  • 6
    Digitale Medien
    Digitale Medien
    Detection of adulteration of pumpkin seed oil by analysis of content and composition of specific Δ7-phytosterols (1999)
    Springer
    European food research and technology 209 (1999), S. 400-406 
    Details
    ISSN: 1438-2385
    Schlagwort(e): Key words Pumpkin seed oil ; Oil adulteration ; Δ7-Phytosterols ; Sample clean-up procedure ; Gas chromatography
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Werkstoffwissenschaften, Fertigungsverfahren, Fertigung
    Notizen: Abstract  A simple and accurate method for the determination of phytosterols by capillary gas chromatography was developed for the analysis of the seeds and oil of the pumpkin Cucurbita pepo L., the naked seed variety growing in the southern Styrian parts of Austria. After extraction of the oil and saponification, the remaining unsaponifiable material was isolated and purified using silica gel columns. For greater volatility, the sterols were derivatised to trimethylsilylethers, and gas chromatography was performed on a column of high polarity, allowing separation of the Δ5-sterols from the Δ7-sterols and thus yielding a typical chromatographical pattern. Quantification of the phytosterols using 5α-cholestan or cholesterol as internal standards led to a method of high accuracy. Comparison of the chromatographic pattern of the phytosterol fraction of pumpkin seed oil with those of other vegetable oil samples permitted the use of this method to detect adulteration of pumpkin seed oil.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/s002170050516
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  • 7
    Digitale Medien
    Digitale Medien
    Chemische Synthese und gaschromatographischer Nachweis von Alkylglucuroniden (1999)
    Springer
    Rechtsmedizin 9 (1999), S. 184-189 
    Details
    ISSN: 1434-5196
    Schlagwort(e): Key words Ethyl glucuronide ; Congeners of alcoholic beverages ; Alkyl glucuronide ; Gas chromatography ; Mass spectrometry ; Schlüsselwörter Ethylglucuronid ; Begleitstoffe ; Alkylglucuronid ; Gaschromatographie ; Massenspektrometrie
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin , Rechtswissenschaft
    Beschreibung / Inhaltsverzeichnis: Zusammenfassung Es wird die chemische Synthese von Alkylglucuroniden beschrieben, die nach Konsum von begleitstoffhaltigen Getränken als Metaboliten im Urin erscheinen. Von folgenden Alkoholen wurden die Glucuronide synthetisiert: Methanol, d5-Ethanol, Propanol, Isopropanol, Butanol, Isobutanol, R-(–)-2-Butanol, S-(+)-2-Butanol, Isopentanol, S-(–)-2-Methylbutanol. Die Retentionsindizes der Acetyl-, Pentafluorpropyl(PFP)- und Trimethylsilyl(TMS)-derivate werden mitgeteilt und der Einfluß der chemischen Struktur auf den RI-Wert diskutiert. Die Massenspektren der homologen Derivate erwiesen sich als sehr ähnlich, aber einige Fragmente sind spezifisch für die Kettenlänge der Alkylgruppe und können zur Identifizierung und Quantifizierung der Glucuronide in Urinproben herangezogen werden.
    Notizen: Abstract The chemical synthesis of alkyl glucuronides, which appear as metabolites in urine after the consumption of beverages containing congeners of ethanol, is described. Glucuronides of the following alcohols were synthesized: methanol, d5-ethanol, propanol, isopropanol, butanol, isobutanol, R-(–)-2-butanol, S-(+)-2-butanol, isopentanol and S-(–)-2-methylbutanol. The retention indices of acetyl, pentafluorpropyl (PFP) and trimethylsilyl (TMS) derivatives are given and discussed in relation to the chemical structures. Mass spectra of homologous derivatives were shown to be very similar but some fragments were specific for the chain length of the alkyl moiety and can be used for identification and a quantitative estimation of glucuronides in urine samples.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/s001940050106
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  • 8
    Digitale Medien
    Digitale Medien
    Peak capacity in packed capillary column solvating gas chromatography (1999)
    Springer
    Chromatographia 49 (1999), S. 333-337 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Supercritical fluid chromatography ; Gas chromatography ; Solvating gas chromatography ; Peak capacity
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary In this paper, a general peak capacity expression was evaluated using columns containing various packing materials under solvating gas chromatography (SGC) conditions. Differing from column efficiency, peak capacity can describe both separation capability and speed when introducing the dead time into the peak capacity expression. Various factors that influence peak capacity in SGC are described, including particle pore size, chemical surface modification, particle size, column length, temperature, and pressure.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467566
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  • 9
    Digitale Medien
    Digitale Medien
    The GC determination of cisplatin as platinum(II) from pharmaceutical preparations and blood sample of cancer patients (1999)
    Springer
    Chromatographia 49 (1999), S. 249-252 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Cisplatin determination ; Blood analysis
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A capillary gas chromatographic method is described for the determination of cisplatin based on the complexation of platinum(II) with bis(isovalerylacetone) ethylenediimine (H2IVA2en) and extraction in chloroform. The chromatography was carried out on a BP1 or a BP5 column with an FID. Copper(II), nickel (II) and palladium(II) separated completely and did not affect the determination of platinum(II). The method was applied of the determination of cisplatin in a pharmaceutical preparation and blood samples of cancer patients after infusion of cisplatin. The amounts of cisplatin in blood were found to be within 246–283 ng mL−1 with a C.V. of 2.35–4.26%.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467551
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  • 10
    Digitale Medien
    Digitale Medien
    Transition metal complex stationary phases for the CGC analysis of ethers, thioethers and ketones (1999)
    Springer
    Chromatographia 49 (1999), S. 273-280 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Complexation stationary phases ; Bonding metal complexes ; Capillary columns
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The use of polysiloxanes with cyano or thiol groups as stationary phases for complexation gas chromatography is discussed. The polymers were obtained via polycondensation followed by polymerisation of the corresponding dichloro- or dimethoxy-silanes. Both the phases were modified by bonding transition metal chlorides with were modified by bonding transition metal chlorides with cyano (CuCl2 or CoCl2) and thiol groups (NiCl2 or CoCl2). The phases were examined in order to determine their application to the analysis of ethers, thioethers and ketones. Due to the presence of lone electron pairs on oxygen or sulphur atoms, the compounds should be capable of specific interacting with the electron-withdrawing centre of the liquid stationary phases. A number of retention parameters (retention indices, molecular retention indices and specific retention volume) were determined, which allowed characterisation of specific interactions between the bonded metal and the compound analysed. The results also enabled assessment of the influence of the structure of the compounds on their retention. The measurements were also carried out for the phases with free SH and CN groups as reference phases. The work demonstrates that the phases obtained may be useful for effective separations.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467556
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  • 11
    Digitale Medien
    Digitale Medien
    Microwave assisted extraction and sonication of polychlorobiphenils from river sediments and risk assesment by toxic equivalency factors (1999)
    Springer
    Chromatographia 49 (1999), S. 21-27 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Microwave and ultrasonic extraction ; River sediment ; Dioxin-like polychlorobiphenyls ; Toxic equivalency factors
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Microwave extraction and ultrasonication of dioxin-like polychlorobiphenyls (PCBs) from sediment samples were investigated. After separation of dioxin-like PCBs from a sample matrix on an acidic-alkaline silica gel column, dioxin-like PCBs were determined by GC-ECD, using dual capillary columns. Recoveries of dioxin-like PCBs in river sediment samples exceeded 80% by both extraction techniques. Toxic equivalency factors and their use for the PCB congeners investigated were applied.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467182
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  • 12
    Digitale Medien
    Digitale Medien
    Solid phase microextraction of volatiles from water using open cap vials (1999)
    Springer
    Chromatographia 49 (1999), S. 513-519 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Solid phase microextraction ; Open cap vials ; Volatile compounds (BTEX) ; Water matrix
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The testing of open cap vials in headspace solid-phase microextraction combined with capillary gas chromatography is reported. The losses of volatile analytes from such vials were analyzed theoretically and investigated experimentally. The benzene, toluene, ethylbenzene, and xylene isomers spiked in water were used as model compounds. Extraction yields and precision obtained under optimized experimental conditions as exposure time, desorption time and temperature were compared applying vials with open caps or sealed with teflon lined septa.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467751
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  • 13
    Digitale Medien
    Digitale Medien
    Retention system, thermodynamic properties and structure correlations of environmental analytes (1999)
    Springer
    Chromatographia 49 (1999), S. 385-390 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Structure correlations ; Polycyclic aromatic hydrocarbons ; Polychlorinated biphenyls ; Polychlorinated pesticides
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A composite chromatographic retention index system has been developed for identifying polycyclic aromatic hydrocarbons, polychlorinated biphenyls and polychlorinated pesticides. When retention indices and thermodynamic data of polycyclic aromatic hydrocarbons on 5% phenylmethylsiloxane stationary phase were compared with those obtained on polydimethylsiloxane a correlation was found between retention and electronic properties. Determination and quantitation of individual contaminants in water and sediment samples from Lake Mecoacán were achieved by capillary gas chromatography with flame ionization and electrocapture detection.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467611
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  • 14
    Digitale Medien
    Digitale Medien
    Analysis of organic pollutants in sewage by supercritical fluid extraction (1999)
    Springer
    Chromatographia 49 (1999), S. 399-405 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Solid phase adsorption ; Supercritical fluid extraction ; Sewage ; Organic pollutants
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Analytical methods have been developed for the determination of organic pollutants of intermediate polarity in sewage. Water samples are first passed through a solid phase adsorption cartridge. The analytes are then extracted from the absorbent with supercritical CO2 into a small volume of trapping solvent. Finally, the extracts are analyzed directly by capillary gas chromatography and gas chromatography-mass spectrometer. The various parameters (pressure, temperature, type and concentration of modifiers, trapping solvent, flow rate and volume of supercritical fluid and equilibrium time) influencing the efficiency of extraction were studied. Extraction efficiencies for the test compounds are 〉70%, and relative standard deviations are 〈4.6% (n=3). The methods established were applied to the analysis of sewage at the Lanzhou Wastewater Treatment Plant, China. 66 organic pollutants were detected, of which 15 compounds appeared in the list of priority pollutants suggested by the US EPA.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467613
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  • 15
    Digitale Medien
    Digitale Medien
    Estimation of retention times of homologous series in temperature programmed gas chromatography (1999)
    Springer
    Chromatographia 49 (1999), S. 509-512 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Homologous series ; Retention times
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary It is shown how to estimate the retention times of homologous series members in linear temperature programmed gas chromatography with the aid of a spread-sheet. Both the ease of estimation and the accuracy of the estimation depend on whether the homologue is eluted during the rising portion of the temperature program or the hold time at the end, and also on whether the homologous series is eluted from one injection or a number of injections. When all members of the series elute in the one chromatographic run the percentage standard deviation of the predicted retention times from the experimental retention times is 0.1. When members of the series elute in different chromatographic runs, the percentage standard deviation of predicted times from experimental times is 0.6, compared with an experimental percentage standard deviation for replicates of 0.5.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467750
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  • 16
    Digitale Medien
    Digitale Medien
    Averaging the pressure and flow rate of the carrier gas in a gas chromatographic column (1999)
    Springer
    Chromatographia 49 (1999), S. 449-453 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Average column pressure ; Average column flow ; Specific retention volume ; Distribution coefficient
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A systematic derivation of corresponding equations shows that averaging the pressure and the flow rate of the mobile phase in a gas chromatographic column over the column length and over the time that an unretained component resides in the column, requires the use of three different compressibility correction factors,j 2 1 ,j 3 2 , andj 4 3 . When multiplied by the adjusted retention volume,V R-VM, the Martin and James mobile phase compressibility correction factorj 3 2 , only, produces the value of specific retention volume,V g T , which is connected unambiguously with the thermodynamic phase distribution coefficient,K, of the sorbate.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467622
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  • 17
    Digitale Medien
    Digitale Medien
    Conversions of carbon monoxide oxidation over Pt−Rh alloy catalysts calculated by a new gas chromatographic technique (1999)
    Springer
    Chromatographia 49 (1999), S. 285-292 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Reversed-flow gas chromatography ; Carbon monoxide oxidation ; Bimetallic Pt−Rh catalysts
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Catalytic fractional conversions of carbon monoxide to carbon dioxide over Pt−Rh alloy catalysts in the presence of excess oxygen, under steady-state or non steady-state conditions, as well as corresponding rate constants for the CO oxidation reaction were measured by using the reversed-flow gas chromatographic technique. From the variation of the conversions with temperature, maximum values of conversions were found, which depend on the catalysts nature (Pt content), while from the variation of the rate constants with temperature, activation energies for the CO oxidation reaction were determined, which also depend on the catalyst Pt content. The results suggest a synergism between Pt and Rh in the Pt−Rh bimetallic catalysts in accordance with previous works, showing that reversed-flow gas chromatography can be used with simplicity and accuracy for the kinetic study of the CO oxidation reaction, which is of technological importance for the control of air pollution.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467558
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  • 18
    Digitale Medien
    Digitale Medien
    A very thick film open-tubular trap for headspace capillary gas chromatography (1999)
    Springer
    Chromatographia 49 (1999), S. 321-326 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Headspace analysis ; Open-tubular trap ; Very thick film column
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary An open-tubular trap with a very thick film was studied for “full on-line” headspace capillary gas chromatography, and was used as an enrichment trap for headspace sampling. The preparation of the open-tubular column with up to an 80 μm thick film, by combining both static and dynamic coating, is described in detail. The break-through volume for the open-tubular trap of different film thickness, as the loading capacity for HS sampling, does not increase linearly in proportion to the film thickness. A study of the difference between a packed adsorbent trap and an open-tubular trap shows that HS capillary GC with open-tubular trap loses less of the retention capacity, has better resolution ability and higher recovery. By independently and rapidly heating the open-tubular trap, the GC peaks may have higher resolution. Examples of successful analyses, by the opentubular trap with “full on-line” HS capillary GC, include trace aromatic hydrocarbon (1 ppm-100 ppm) in polybutadiene-styrene rubber and trace alcohol and acrylic esters (10 ppm–1000 ppm) in polyacrylate hydrous emulsion.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467564
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  • 19
    Digitale Medien
    Digitale Medien
    Hydroxyproline interference during the gas chromatographic analysis of D/L aspartic acid in human dentine (1999)
    Springer
    International journal of legal medicine 112 (1999), S. 124-131 
    Details
    ISSN: 1437-1596
    Schlagwort(e): Key words Hydroxyproline ; D/L Aspartic acid ; N-TFA isopropyl ester derivatives ; Gas chromatography ; Collagen
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin , Rechtswissenschaft
    Notizen: Abstract The proportion of D- to L-enantiomers of aspartic acid in metabolically isolated proteins has been used by forensic scientists to estimate age at death. We have demonstrated the interference of a derivative of hydroxyproline (N-TFA isopropyl Hyp ester) with the N-TFA isopropyl L-Aspartic (Asp) acid ester during gas chromatography of amino acids. This has serious implications for the accurate quantification of the D- to L-Asp ratio extracted from collagenous proteins. Having demonstrated the potential for this co-elution in amino acid standards, acid-soluble dentine proteins and non-mineralised collagen, we argue that this problem can be overcome either by high resolution separation or by analysis of the (Hyp-poor) non-collagenous protein fraction.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/s004140050214
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  • 20
    Digitale Medien
    Digitale Medien
    Superior ECD Performance through Design and Application (1999)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 24-28 
    Details
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; ECD ; Micro-ECD ; GC detector ; organochlorine pesticides ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---A new ECD, the HP 6890 Series Micro-ECD, was designed to address inherent deficiencies in classical electron capture detectors (ECD), especially with respect to sensitivity, linearity, dynamic range, and ruggedness. Several novel technologies were incorporated in the totally new design and were refined through practical testing and user feedback. Validation of the micro-ECD performance was accomplished through side-by-side testing of the Micro-ECD with previous ECDs following US EPA Contract Laboratory Program methods for pesticides and PCBs. In addition, extensive interviews were conducted with early users of the Micro-ECD who also had experience with other designs running a variety of ECD methods. The design and resulting performance improvements are described.
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 21
    Digitale Medien
    Digitale Medien
    Rapid Method for the Determination of Thiabendazole and Imazalil Residues in Orange by Capillary Column Gas Chromatography (1999)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 303-304 
    Details
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; food analysis ; pesticide residues ; thiabendazole ; imazalil ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 22
    Digitale Medien
    Digitale Medien
    Pulsed Splitless Injection and the Extent of Matrix Effects in the Analysis of Pesticides (1999)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 395-402 
    Details
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; pulsed splitless injection ; pesticide residues ; matrix effects ; retention gap ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The applicability of pulsed splitless injection to the gas chromatographic analysis of pesticide residues in fruit and vegetables has been evaluated. 22 pesticides belonging to different chemical classes, including those known to be liable to matrix induced response enhancement, were selected for the study. The parameters of pressure pulse have been tested for optimum performance of injection. Application of the pressure pulse was found to decrease matrix effects during analyses of real samples. Further decline of matrix effects was obtained using higher sample injection volumes. The installation of a deactivated retention gap was necessary to obtain good peak shapes with injection volumes exceeding 1 μL of sample. Up to 4 μL was then injected without peak distortion and consequent loss of resolution. Using 4 μL pulsed splitless injection, matrix effects were almost completely eliminated even at very low concentration levels of analytes. The highest matrix effects observed for tested compounds at the lowest concentration level tested were in the range of 110-122%.
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 23
    Digitale Medien
    Digitale Medien
    Determination of Vapor Liquid Equilibrium from the Kovats Retention Index on Dimethylsilicone using the Wilson Mixing Model (1999)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 565-588 
    Details
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; Kovats retention index ; vapor pressure ; boiling point ; Wilson activity coefficient ; binary phase diagrams ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Non-ideal mixing in a dimethylsilicone stationary phase is modeled according to the Wilson activity coefficient. Pure liquid vapor pressures of alkylated compound series are calculated from capillary GLC retention with the functional group heat of solution in a polymer solvent. The new method uses the Kovats index, molar mass, and functional group to determine the bubble line of a compound. Boiling points at reduced and normal pressure are compared to literature values of 194 gasoline components. An unlike molecular pair interaction parameter is derived, using only bubble line data of the pure liquids. Binary phase diagrams are constructed and compared to vapor liquid equilibrium data.
    Zusätzliches Material: 22 Ill.
    Materialart: Digitale Medien
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  • 24
    Digitale Medien
    Digitale Medien
    Solid Phase Microextraction and GC-MIP-AED for the Speciation Analysis of Organomercury Compounds (1999)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 181-182 
    Details
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; microwave induced emission spectrometry ; speciation ; mercury ; SPME, headspace SPME ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: ---No abstract
    Zusätzliches Material: 1 Ill.
    Materialart: Digitale Medien
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  • 25
    Digitale Medien
    Digitale Medien
    Analysis of the Naturally Occurring Pesticide Rotenone by Capillary Gas Chromatography (1999)
    Weinheim : Wiley-Blackwell
    Journal of High Resolution Chromatography 22 (1999), S. 294-296 
    Details
    ISSN: 0935-6304
    Schlagwort(e): Gas chromatography ; capillary ; fused silica ; rotenone ; Chemistry ; Analytical Chemistry and Spectroscopy
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: No abstract
    Zusätzliches Material: 3 Ill.
    Materialart: Digitale Medien
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  • 26
    Digitale Medien
    Digitale Medien
    Characterisation of paint layers in Chinese archaelogical relics by pyrolysis-GC-MS (1999)
    Springer
    Chromatographia 49 (1999), S. 268-272 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Mass spectrometry ; Analytical pyrolysis ; Chinese art objects ; Mercury analysis
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A few samples of polychrome Chinese archaeological objects of art have undergone analytical pyrolysis coupled with GC-MS to evaluated the possibility of contemporary characterization of the pigments as well as the organic media used. The red pigment cinnabar (HgS) is easily media used. The red pigment cinnabar (HgS) is easily detected, whereas in the case of organic components positive results are only found where the matrices are resistant to archaeological environmental conditions.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467555
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  • 27
    Digitale Medien
    Digitale Medien
    [60] Fulleropyrrolidine functionalized polysiloxane as a stationary phase for capillary gas chromatography (1999)
    Springer
    Chromatographia 49 (1999), S. 293-298 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; [60] Fulleropyrrolidine polysiloxane ; High temperature stationary phase
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary In this paper, a new type of [60]fulleropyrrolidine functionalized polysiloxane in which the fullerene moieties were incorporated in the main polysiloxane chain was synthesized the first time and used as a stationary phase for capillary gas chromatography. It demonstrated high column efficiency (2600–2866 plates m−1, on a 250 μm diameter column, for naphthalenek=3.1–3.2, 120 °C), a wide operational temperature range (90–360 °C) and outstanding thermostability. It can be used at 360 °C with a baseline drift of 5∼8×10−15A. Benzene homologues, aromatic hydrocarbons, polar compounds such as alcohols, esters, ketones, anilines and phthalic diesters can be seperated well on this column.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467559
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  • 28
    Digitale Medien
    Digitale Medien
    Polybutadiene-coated zirconia packing materials in solvating gas chromatography using carbon dioxide as mobile phase (1999)
    Springer
    Chromatographia 49 (1999), S. 431-435 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Supercritical fluid chromatography ; Solvating gas chromatography ; Polybutadiene coated zirconia ; CO2 mobile phase
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary In this paper, practical considerations of column efficiency, separation speed, thermal stability, and column polarity of capillary columns packed with polybutadiene-coated zirconia were investigated under solvating gas chromatography (SGC) conditions using carbon dioxide as mobile phase. When compared with results obtained from conventional porous octadecyl obtained from conventional porous octadecyl bonded silica (ODS) particles, PBD-zirconia particles produced greater change in mobile phase linear velocity with pressure than conventional ODS particles under the same conditions. The maximum plate number per second (Nt) obtained with a 30 cm PBD-zirconia column was approximately 1.5 times higher than that obtained with an ODS column at 100 °C. Therefore, the PBD-zirconia phase is more suitable for fast separations than conventional ODS particles in SGC. Maximum plate numbers per meter of 76,900 and 63,300 were obtained using a 57 cm×250 μm i.d. fused silica capillary column packed with 3 μm PBD-zirconia at 50 °C and 100 °C, respectively. The PBD-zirconia phase was stable at temperatures up to 320 °C under SGC conditions using carbon dioxide as mobile phase. Polarizable aromatic compounds and low molecular weight ketones and aldehydes were eluted with symmetrical peaks from a 10 cm column packed with 3 μm PBD-zirconia. Zirconia phases with greater inertness are required for the analysis of more polar compounds by SGC.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467619
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  • 29
    Digitale Medien
    Digitale Medien
    Efficiency of direct solid-phase microextraction from water-comparison of different fibre types including a new C8-coating (1999)
    Springer
    Chromatographia 49 (1999), S. 686-690 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Solid-phase microextraction ; Fibre coating ; Volatile organic compounds ; Semi-volatile organic compounds
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The efficiency of direct solid-phase microextraction (SPME) was determined for 27 selected volatile and semivolatile organic compounds (BTEX, chloro- and bromobenzenes, chlorinated pesticides and PCBs). The fibres used were 7μm polydimethylsiloxane (PDMS), 30μm PDMS, 100μm PDMS, 65μm PDMS-divinylbenzene, 85μm polyacrylate, 65μm Carbowax-divinylbenzene, 75μm Carboxen-PDMS and a new 65μm C8 fibre. Extraction yields for these compounds were calculated under standardised conditions: 75μm Carboxen-PDMS was found to be the most efficient fibre for compounds with low boiling points. Although 65μm C8 can be used for extraction of all compounds studied, in no one case is it the most effective coating. 100μm PDMS and the more polar coatings can be used for a broad range of compounds, whereas application of 7μm and 30μm PDMS cannot be recommended. Inter-fibre comparison revealed significant differences between three different Carboxen-PDMS fibres. The results enable suitable coatings to be chosen for each of the 27 compounds and for substances with similar properties.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02466913
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  • 30
    Digitale Medien
    Digitale Medien
    Synergistic effect of mixed stationary phase in gas chromatography (1999)
    Springer
    Chromatographia 49 (1999), S. 567-571 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Mixed stationary phase ; Calixarenes ; Crown ethers ; Cyclodextrins
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Mixed stationary phases containing of 25,27-dibutoxy-5,11,17,23-tetra-tert-butyl-26,28-diundecenyloxy calix [4]arene (C[4]B)+ω-undecylomethyl-18-crown-6 polysiloxane (PSO-11-18-C-6) and C[4]B polysiloxane (PSO-C[4]B)+permethyl-β-cyclodextrin (PM-β-CD) were investigated in capillary gas chromatography. By comparing their selectivity for positional isomers with that of the corresponding individual pure stationary phases, synergistic effects were found.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467761
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  • 31
    Digitale Medien
    Digitale Medien
    Gas chromatographic determination of 2-chloro-1-[[4-[(2,6-dichlorophenoxy)methyl]phenyl]methoxy]-4-methoxybenzene (SCH 48973), a potent anti-picornaviral agent, in dog serum (1999)
    Springer
    Chromatographia 49 (1999), S. 575-578 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Electron capture detector ; Anti-picornaviral agent in dog serum ; Enteroviruses
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A gas chromatographic assay for the determination of SCH 48973, a potent broad spectrum anti-picornaviral agent, was developed and validated in dog serum. The method involved extraction with organic solvent followed by separation on a capillary column (DB-1) with quantitation by an electron-capture detector. The method was sensitive with a limit of quantitation of 10 ng mL−1. The linearity of the method was satisfactory as indicated by correlation coefficients of 〉0.999 and visual examination of the calibration curves. The method was precise with a coefficient of variation ranging from 2.3 to 13.2% and accurate with a bias ranging from −9.1 to 7.9%. Moreover, SCH 48973 was stable in dog serum after being subjected to three freeze-thaw cycles. The assay was shown to be sensitive, specific, accurate and precise, and reliable for use in pharmacokinetic or toxicokinetic studies.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467763
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  • 32
    Digitale Medien
    Digitale Medien
    Monitoring of nicotine in air using sorptive enrichment on polydimethylsiloxane and TD-CGC-NPD (1999)
    Springer
    Chromatographia 49 (1999), S. 520-524 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Sorptive preconcentration ; Air monitoring ; Nicotine ; Hospital air
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A novel method for the enrichment of nicotine from gaseous samples is presented. It is based on the sampling of 6 liters of air onto a cartridge packed with 100% polydimethylsiloxane (PDMS) particles. The analytes are dissolved (partitioned) into the PDMS phase which results in much better recoveries and reproducibilities compared to those obtained on common adsorbents. The PDMS tube is then placed in a thermal desorption (TD) unit connected to a CGC-NPD or CGC-MS system. The procedure was employed for routinely monitoring air in a hospital. Nicotine was typically found at levels ranging from 5 to 250 μg m−3 (ppb) depending on the location and number of smokers present. Additionally, the efficiency of nicotine filters was determined by sampling simultaneously at the filter in- and outlet and was found to be 46%.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467752
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  • 33
    Digitale Medien
    Digitale Medien
    Quantitative determination of carbohydrates in orange juice by gas chromatography (1998)
    Springer
    Zeitschrift für Lebensmittel-Untersuchung und -Forschung 206 (1998), S. 48-51 
    Details
    ISSN: 1431-4630
    Schlagwort(e): Key words Carbohydrates ; Myo-inositol ; Orange juice quality ; Gas chromatography
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Werkstoffwissenschaften, Fertigungsverfahren, Fertigung
    Notizen: Abstract  A gas chromatographic method using a capillary column is described for the quantitative analysis of fructose, glucose, sucrose and myo-inositol in orange juice. The method is evaluated for precision and recovery using phenyl-β-glucoside as an internal standard. The results support the suitability of the method. Carbohydrates (fructose, glucose, sucrose and myo-inositol) were determined in different kinds of orange juice. The determination of carbohydrate composition and ratios of the carbohydrate constituents provide a method to assess orange juice quality, especially the myo-inositol content and myo-inositol/fructose ratio. These new indices, which were found to be lower in samples made from concentrates, provide information on the quality and genuineness of orange juice.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/s002170050212
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  • 34
    Digitale Medien
    Digitale Medien
    Amounts of conjugated linoleic acid (CLA) in German foods and evaluation of daily intake (1998)
    Springer
    Zeitschrift für Lebensmittel-Untersuchung und -Forschung 206 (1998), S. 77-82 
    Details
    ISSN: 1431-4630
    Schlagwort(e): Key words Anticarcinogen ; CLA ; Conjugated linoleic acid ; Daily intake ; Foods ; Gas chromatography ; Lipids
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Werkstoffwissenschaften, Fertigungsverfahren, Fertigung
    Notizen: Abstract  The quantities of the biologically active isomer of conjugated linoleic acid (CLA) – C18:2 c9t11 – in 139 German foods were analysed by capillary gas chromatography (results are given as a % of all identified fatty acid methyl esters). The CLA content ranged from 0.40% (Gouda) to 1.70% (Jurassic cheese, Old Emmentaler) in dairy products, from 0.11% (rabbit) to 1.20% (lamb) in meat, and from 0.01% (pike-perch) to 0.09% (carp) in fish. CLA could be detected in neither vegetable fats or oils nor in margarines (CLA 〈0.01%). Crisps, chocolates, cakes and pastries, and other foods have only a negligible CLA content. The average estimated CLA intake in Germany was calculated to be 0.35g CLA/day for women and 0.43g CLA/day for men.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/s002170050218
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  • 35
    Digitale Medien
    Digitale Medien
    Comparison of gas chromatographic methods for analysis of butyric acid in milk fat and fats containing milk fat (1998)
    Springer
    Zeitschrift für Lebensmittel-Untersuchung und -Forschung 206 (1998), S. 213-216 
    Details
    ISSN: 1431-4630
    Schlagwort(e): Key words Milk fat ; Mixed fat ; Milk fat content ; Butyric acid ; Gas chromatography
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Werkstoffwissenschaften, Fertigungsverfahren, Fertigung
    Notizen: Abstract  The analysis of butyric acid (C4) is of importance for the determination of the proportion of milk fat in mixed fats. Three gas chromatographic methods were compared with regard to their precision for the measurement of C4, i.e. analysis of butyric acid methyl ester after trans-esterification of fat by sodium methylate (method A) or trimethyl sulphonium hydroxide (method B), as well as analysis of free butyric acid (method C), using an internal standard with each method. The examination of 30 milk fats which varied greatly in terms of their C4 content, using methods A, B and C, resulted in mean values of C4 of 3.42 g/100 g fat, 3.71 g/100 g fat and 3.06 g/100 g fat, respectively. The value determined using method B seemed too high, and this may have been due to the presence of co-eluting artefacts, whereas the value determined using method C was clearly too low, and can probably be attributed to losses during sample preparation. The standard deviation (SD) of 0.015 obtained from repeated analyses using method A was quite good. Results obtained using methods B and C had SDs of 0.029 and 0.074, respectively. Different levels of free fatty acids did not affect the results obtained using method A. When method A was checked by analysis of the reference fat, CRM 164, the C4 level determined was found to deviate from the certified C4 content of 3.49 (± 0.06) g/100 g fat by only 0.05 g C4/fat 100 g. Thus method A proved the most suitable for the determination of the proportion of milk fat in mixed fats by analysis of butyric acid.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/s002170050245
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  • 36
    Digitale Medien
    Digitale Medien
    The isoprostanes: Unique bioactive products of lipid peroxidation (1998)
    Springer
    Journal of biomedical science 5 (1998), S. 415-420 
    Details
    ISSN: 1423-0127
    Schlagwort(e): Isoprostanes ; Oxidative stress ; Lipid peroxidation ; Gas chromatography ; Mass spectrometry ; Human disease
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Biologie , Medizin
    Notizen: Abstract The development of a specific, reliable and noninvasive method for measuring oxidative stress in humans is essential for establishing the role of free radicals in human diseases. Currently, accurate techniques to assess oxidant injury in vivo are extremely limited although a number of approaches are being investigated. Of these, the measurement of specific products of nonenzymatic lipid peroxidation, the F2-isoprostanes (F2-IsoPs), appears to be a more accurate marker of oxidative stress in vivo in humans than other available methods. The purpose of this brief review is to acquaint the reader with the IsoPs from a biochemical perspective and to provide information regarding the utility of quantifying these compounds as indicators of oxidant stress.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02255929
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  • 37
    Digitale Medien
    Digitale Medien
    Changes in free monosaccharides during storage of some UHT milks: a preliminary study (1998)
    Springer
    Zeitschrift für Lebensmittel-Untersuchung und -Forschung 207 (1998), S. 180-181 
    Details
    ISSN: 1431-4630
    Schlagwort(e): Key words UHT milk ; Storage ; Monosaccharides ; Gas chromatography
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Werkstoffwissenschaften, Fertigungsverfahren, Fertigung
    Notizen: Abstract  Changes in the free monosaccharide fraction and non-casein nitrogen during the 3-month storage of five batches of commercial UHT milk were studied. Batches with high residual proteolytic activity showed a considerable increase in galactose, N–acetyl glucosamine and N–acetyl galactosamine levels during the storage period, whereas their glucose and myo-inositol contents remained unaltered. In batches with slight or negligible proteolytic activity no changes in the free monosaccharide fraction were observed.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/s002170050315
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  • 38
    Digitale Medien
    Digitale Medien
    Application of a new method for analysis of exhaled gas in critically ill patients (1998)
    Springer
    Intensive care medicine 24 (1998), S. 415-421 
    Details
    ISSN: 1432-1238
    Schlagwort(e): Key words Acetone ; Gas chromatography ; Isoprene ; Lipid peroxidation ; Microwave desorption ; N-pentane
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Medizin
    Notizen: Abstract Objective: Application of a new method for analysis of exhaled gas in critically ill patients. Design: Open study. Setting: Surgical intensive care unit of an university hospital. Patients: Thirty-seven consecutive, critically ill, mechanically ventilated patients. Interventions: None. Measurements and results: Chemical analysis of the patient's exhaled gas was based upon substance adsorption and concentration onto activated charcoal, microwave desorption and gas chromatographic separation. Patients with acute respiratory distress syndrome (ARDS) exhaled less isoprene than those without ARDS [9.8 (8.2–21.6) vs 21.8 (13.9–41.4) nmol/m2 per min [median (95 % confidence interval)], p = 0.04]. In patients who developed pulmonary infection, pentane elimination increased from 0.4 (0.0–5.4) to 2.7 (0.6–6.1, p = 0.05) nmol/m2 per min and isoprene elimination decreased from 5.2 (0–33) to 5.0 (0–17, p = 0.05) nmol/m2 per min, resulting in a significant increase in pentane/isoprene ratio from 0.1 (0–0.3) to 0.4 (0–15, p = 0.007) when compared to patients without pulmonary infection. Conclusions: The new method allows quantitative analysis of human gas samples with low substance concentrations and is well suited for clinical studies which involve the investigation of metabolic processes in the lung and the body.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/s001340050589
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  • 39
    Digitale Medien
    Digitale Medien
    Mixing in Stars and the Evolution of the 3He Abundance (1998)
    Springer
    Space science reviews 84 (1998), S. 199-206 
    Details
    ISSN: 1572-9672
    Schlagwort(e): Nuclear reactions ; Nucleosynthesis ; Abundances ; Stars:Evolution ; Interior ; Rotation
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Physik
    Notizen: Abstract We first recall the observational and theoretical facts that constitute the so-called 3He problem. We then review the chemical anomalies that could be related to the destruction of 3He in red giants stars. We show how a simple consistent mechanism can lead to the destruction of 3He in low mass stars and simultaneously account for the low 12C/13C ratios and low lithium abundances observed in giant stars of different populations. This process should both naturally account for the recent measurements of 3He/H in galactic HII regions and allow for high values of 3He observed in some planetary nebulae. We propose a simple statistical estimation of the fraction of stars that may be affected by this process.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1023/A:1005027519798
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  • 40
    Digitale Medien
    Digitale Medien
    Calix[4]arene derivatives as stationary phases for capillary gas chromatography (1998)
    Springer
    Chromatographia 47 (1998), S. 689-694 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Stationary phases ; Calix[4]arene derivatives
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Two new kinds of calix[4]arene derivatives, 5,11,17,23-tetra-tert-butyl-25,27-bis(isopropylcarbamoyl-methoxy)-26,28-diundecenyloxy calix[4]arene (C[4]A) and 25,27-dibutoxy-5,11,17,23-tetra-tert-butyl-26,28-diundecenyloxy calix[4]arene (C[4]B), have been synthesized for use as stationary phases in capillary gas chromatography with OV1701. These stationary phases demonstrate high column efficiencies, wide operating temperature ranges, good thermal stability and excellent selectivity for aromatic isomers, especially phenol compounds. Their inclusion properties are also discussed.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467455
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  • 41
    Digitale Medien
    Digitale Medien
    Quantitative analysis of residual synthetic polystyrene adsorbent in drugs by curie-point pyrolysis gas chromatography (1998)
    Springer
    Chromatographia 47 (1998), S. 203-208 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Pyrolysis GC ; Residual polystyrene ; Streptomycin ; Vitamin B1
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Residual synthetic adsorbent, cross-linked polystyrene, used in drug purification has been analyzed quantitatively by Curie-point pyrolysis gas chromatography. The peaks of intact polystyrene adsorbent in the pyrogram were used as key peaks for quantitative measurement of residues of the adsorbent in vitamin B1 and streptomycin sulfate. It was shown that them-ethylstyrene orp-ethylstyrene peaks in the pyrolyzates were suitable for determination of polystyrene adsorbent content. The levels of residual adsorbent in the drugs were found to be 〈0.1 %, the value stipulated by the International Conference on Harmonization (ICH). In quantitative evaluation of an adsorbent content of 0.1 % the precision was 3.6 % and 2.7 % for vitamin B1 and streptomycin sulfate, respectively.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02466582
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  • 42
    Digitale Medien
    Digitale Medien
    Development of gas chromatographic method for determination of cholesterol oxides in meat products (1998)
    Springer
    Chromatographia 47 (1998), S. 42-48 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Cholesterol oxides ; Cholesterol oxidation products (COPs) ; Meat products
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A method of extraction, purification and gas chromatographic analysis of five cholesterol oxidation products (COPs) (7β-hydroxycholesterol, 5α, 6α-epoxycholesterol, 25-hydroxycholesterol, 7-ketocholesterol and cholestane-3β, 5α, 6β-triol) has been developed. The method is aimed at the determination of COPs in meat and meat products, in particular dry sausages, where large differences in the content of cholesterol and its oxidation derivatives may occur. Linearity of response of trimethylsilyl ethers was defined. The minimum concentration tested was 2.5 μg g−1 in the injected solution. The main feature of the present work is the addition of a purification step of unsaponifiables by SPE on silica cartridges. Extraction recoveries of COP standard mixtures, performed with or without the SPE step, are evaluated. The introduction of the clean-up step results in high purity samples without further losses in the entire process.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02466784
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  • 43
    Digitale Medien
    Digitale Medien
    Direct solid-phase microextraction combined with gas and liquid chromatography for the determination of lidocaine in human urine (1998)
    Springer
    Chromatographia 47 (1998), S. 678-684 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Column liquid chromatography ; Solid-phase microextraction ; Local anaesthetic lidocaine ; Optimisation of extraction
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Solid-phase microextraction (SPME) has been combined with gas chromatography (GC) and liquid chromatography (LC) for the determination of lidocaine in human urine. A polydimethylsiloxane (PDMS) coated fibre was directly immersed into buffered urine. Extraction conditions such as time, pH, ionic strength, temperature, and agitation were optimised. The extracted lidocaine was thermally desorbed in a split/splitless injector for analysis with a GC-FID system or desorbed with liquid in a specially designed SPME-LC interface for analysis with an LC-UV system. After optimisation the method developed was evaluated and validated. Extraction yields of 22% were obtained in about 45 min. The reproducibility of the method is 〈5% (relative standard deviation). For five-times diluted urine, linear ranges were found from 5–1000 and 25–1000 ng·mL−1 for SPME-GC and SPME-LC, with detection limits of 5 ng·mL−1 for SPME-GC and 25 ng·mL−1 for SPME-LC. SPME can be used as a simple sample pretreatment method for the determination of lidocaine in urine by GC and LC.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467453
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  • 44
    Digitale Medien
    Digitale Medien
    Fast determination of VOCs in workplace air by solid-phase extraction and gas chromatography-mass spectrometry (1998)
    Springer
    Chromatographia 47 (1998), S. 57-62 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Solid-phase extraction ; Graphitized carbon black ; Volatile organic compounds ; Workplace air
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A fast, simple, and reliable method is presented for the determination of atmospheric semi-volatile organic pollutants at μg m−3 levels. The method has been used to monitor potentially carcinogenic toxic compounds to which workers are exposed in workplaces, and to measure the same compounds in outdoor air.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02466786
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  • 45
    Digitale Medien
    Digitale Medien
    Determination of safrole in differentAsarum species by headspace gas chromatography (1998)
    Springer
    Chromatographia 47 (1998), S. 685-688 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Headspace sampling ; Safrole ; Asarum species
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The development of a headspace GC method (HS-GC) to determine the safrole content in differentAsarum species from China and Europe, using eugenol as internal standard, is presented in this paper. The best results could be achieved by thermostating the samples at 100°C for 30.0 min, adding 10 μL of water to each sample. Optimum pressurisation and injection time showed to be 3.0 min and 12 s, respectively. GC separation was performed on an SE-54 column. The HS-GC results for safrole were in good agreement with those obtained by direct GC analysis of the dichloromethane (DCM) plant extracts. The investigated Asarum samples showed great deviations concerning the safrole content even within the sameAsarum species, e.g.Asarum himalaicum from Sichuan contained 0.0051% of this compound, the same species from the province of Hebei 0.53%.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467454
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  • 46
    Digitale Medien
    Digitale Medien
    Gas chromatographic analysis of phthalate esters in plastic toys (1998)
    Springer
    Chromatographia 47 (1998), S. 724-726 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Phthalate esters ; PVC ; Plastic toys
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A method for the analysis of 10 phthalate esters in plastic toys is described. The samples are soxhlet extracted in dichloromethane and phthalate esters in the extract are analysed by GC. Detection limits of dimethyl phthalate, diethyl phthalate, dibutyl phthalate, bis(2-ethylhexyl) phthalate, di-n-octyl phathalate, di-n-nonyl phthalate, benzyl butyl phthalate and benzyl octyl phthalate were approximately 5 ppm. The detection limits of diisononyl phthalate and diisodecyl phthalate, which are mixtures of several isomers, were approximately 200ppm. Analysis of 17 plastic toys revealed that only PVC-toys contained phthalate esters. Bis(2-ethylhexyl) phthalate, diisononyl phthalate and diisodecyl phthalate in concentrations up to 40% were present in the PVC-toys.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467461
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  • 47
    Digitale Medien
    Digitale Medien
    Analysis of cyanide in blood by headspace solid-phase microextraction (SPME) and capillary gas chromatography (1998)
    Springer
    Chromatographia 47 (1998), S. 209-214 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Solid-phase microextraction ; Headspace sampling ; Cyanide in blood
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Cyanide can be extracted from whole blood samples by headspace solid-phase microextraction (SPME) with a Carbowax/divinylbenzene-coated fiber. During heating a vial of a whole blood sample containing cyanide and acetonitrile as internal standard (IS) at 50°C in the presence of Na2SO4, a Carbowax/divinylbenzene-coated SPME fiber was exposed in the headspace of the vial for 45 min to allow adsorption of cyanide and IS. The fiber needle was then injected into a capillary gas chromatography (GC) instrument equipped with nitrogen-phosphorus detection. The headspace SPME-GC with a Supel-Q PLOT fused silica capillary column gave large peaks for cyanide and IS; almost no interfering peaks appeared. Recoveries of cyanide dnd IS from human whole blood were 3.02–4.06% and 0.21%, respectively. The calibration curve for cyanide added to human blood showed excellent linearity in the range of 0.04–4.0 μg mL−1; the detection limit was about 0.02 μg mL−1. The coefficients of intra-day and inter-day variation were not greater than 7.1 and 9.2%. Good correlation (r 2=0.999) was found between the present SPME-GC method and the conventional microdiffusion colorimetric method. Data on determination of cyanide in rat blood after intraperitoneal administration are also presented.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02466583
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  • 48
    Digitale Medien
    Digitale Medien
    Synergistic effects in mixed gas chromatographic stationary phases consisting of dibenzo-18-crown-6 and MPBHpB (1998)
    Springer
    Chromatographia 47 (1998), S. 575-578 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Mixed stationary phases ; Dibenzo-18-crown-6 ether ; MPBHpB ; Synergistic effects
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The synergistic effect is investigated in mixed gas chromatographic stationary phases containing dibenzo-18-crown-6 +MPBHpB [o-methyl-p-phenylene-bis-(p-heptoxy benzoate)], [o-methyl-p-phenylene-bis-(p-heptoxy benzoate)], with benzene/cyclohexane, cyclokexanes, phenols, alcohols and aniline derivatives as sample compounds pairs. Some of the separations reveal positive or negative synergistic effect. This effect depends on the temperature, the mixing ratio and the linear velocity of the carrier gas.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467498
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  • 49
    Digitale Medien
    Digitale Medien
    Sulfuric acid pretreatment for the simultaneous GC screening of organochlorine and organophosphorus pesticides in herbal essential oils (1998)
    Springer
    Chromatographia 47 (1998), S. 587-592 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Organochlorine and organophosphorus pesticides ; Herbal medicine ; Essential oils ; Sulfuric acid treatment
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A rapid and new clean-up method utilizing sulfuric acid treatment is demonstrated to identify and quantify the level of organochlorine (OC) and organophosphorus (OP) pesticide residue concentrations in herbal essential oils by gas chromatography (GC). Essential oils fortified with pesticides, that are extracted from herbs by steam distillation are partitioned with 65% acetonitrile/water(v/v) and treated with sulfuric acid at different reaction times and sulfuric acid concentrations. Optimal conditions, to avoid interference from essential oils in gas chromatographic analysis, is 17% (v/v) of a mixed phase ratio of sulfuric acid to organic solvent (hexane/ethyl ether=9∶1, v/v) and a reaction time of 30s. The response of the flame ionization detector (FID) is linear for all pesticides determined. Recovery of pesticides from fortified herbs studied are in the range of 75% to 111% (RSD, 4% to 11%) for OC, and 72% to 116% (RSD, 2% to 11%) for OP. Although sulfuric acid treatment destroys carbamate and some organophosphorus pesticides, this method has efficiently reduced matrix interference and provides a rapid, economical clean-up method with excellent linear data having low coefficients of variation for the GC analyses of BHC isomers, DDD, DDE, DDT, chlorothalonil, chloropyrifos, tetradifon, fenitrothion, malathion, and parathion in matrices of herbal essential oils.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467500
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  • 50
    Digitale Medien
    Digitale Medien
    Enantiomeric separation of unusual secondary aromatic amino acids (1998)
    Springer
    Chromatographia 48 (1998), S. 53-58 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Column liquid chromatography ; Gas chromatography ; Enantiomeric separation ; Chiral derivatization ; Unusual secondary aromatic amino acids
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary High-performance liquid chromatographic and gas chromatographic methods were developed for the separation of unusual secondary aromatic amino acids. Amino acids containing 1,2,3,4-tetrahydroisoquinoline, 1,2,3,4-tetrahydronorharmane-1-carboxylic acid and 1,2,3,4-tetrahydro-3-carboxy-2-carboline moieties were synthetized in racemic or chiral forms. The high-performance liquid chromatography was carried out either on a teicoplanin-containing chiral stationary phase or on an achiral C18 column. In the latter case the diastereomers of the amino acids formed by precolumn derivatization with the chiral reagents 2,3,4,6-tetra-O-acetyl-β-D-glucopyranosyl isothiocyanate or 1-fluoro-2,4-dinitrophenyl-5-L-alanine amide were separated. The gas chromatographic analyses were based on separation on a Chirasil-L-Val column.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467516
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  • 51
    Digitale Medien
    Digitale Medien
    Urinary steroid analysis of women with effluvium (1998)
    Springer
    Chromatographia 48 (1998), S. 86-88 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Solid phase extraction ; Methoxime-silyl derivate ; Urinary steroids ; Women with effluvium
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Urinary steroid metabolites were measured by capillary gas chromatography in 25 women (aged 33.3±12.0 years) with effluvium and 16 control healthy laboratory workers women (aged 34.6±8.4 years). There was significant elevation in the level of a number of steroids and steroid metabolites. The elevation of most steroid metabolites refers to the increased steroid secretion of the adrenal and the high cortisol metabolites levels may be do to stress in some of the patients with effluvium.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467522
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  • 52
    Digitale Medien
    Digitale Medien
    Capillary gas chromatography of urinary steroids of terbutaline-treated asthmatic children (1998)
    Springer
    Chromatographia 48 (1998), S. 163-165 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Solid-phase extraction ; Urinary steroids ; Terbutaline treatment ; Asthmatic children
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Steroid metabolites have been measured by capillary gas chromatography in the urine of 38 children aged 3–6 years. The children comprised three groups: those with asthma being treated with Terbutaline (13), children with asthma but not undergoing treatment (17), and control children in hospital but free from endocrine diseases (8). There were significant (P〈0.05) differences between the amounts of steroids excreted by the different groups of children. Terbutaline therapy led to elevated levels of tetrahydrocortisone, androstenediol, 11-ketopregnanetriol and a reduced ratio of androgen to cortisol metabolites compared with those for untreated asthmatic children. We assume that Terbutaline does not have a steroid-like mechanism of action but acts by modification of the activity of several adrenocortical enzymes. We suggest a hypothesis whereby the antiasthmatic effect of Terbutaline could not only be a connected with its well-known mechanism of action, but it might be explained as a result of the modification of the production of certain glucocorticoids and androgen hormones.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467536
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  • 53
    Digitale Medien
    Digitale Medien
    Characterisation of GC stationary phases in multilinear retention model (1998)
    Springer
    Chromatographia 48 (1998), S. 728-738 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Stationary phases ; Prototypical phases ; Retention model ; Retention value ; Dipolarity
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Stationary phases are characterised in a multilinear retention model by retention data of a set of selected prototypical substances. Prototypical stationary phases confirm the application of prototypical substances in the retention model. For comparison, 27 stationary phases are characterized with solute descriptors of the solvation model. New adjusted substance factors are calculated for 33 selected compounds for a new characterization of GC stationary phases in the extended retention model with retention values, calculated from retention indices and b-values of the n-alkane equation. Substance dipolarityD N-factors are separated from πN, the adjusted dipolarity-polarisability. New substance factors give satisfying correlation results and new explanatory factors as phase descriptors for 27 stationary phases.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467640
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  • 54
    Digitale Medien
    Digitale Medien
    Precision of milk fat quantitation in mixed fats by analysis of butyric acid (1998)
    Springer
    Chromatographia 48 (1998), S. 758-762 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Butyric acid ; Milk fat content ; Mixed fats
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Quantitation of the milk fat content in mixed fats is of interest in food analysis. It can be achieved by calculation from the butyric acid (C4) content in the mixed fat and a mean C4 content for pure milk fats. Alternatively, instead of applying a C4 mean value, the C4 content in the actual milk fat can be used if this reference sample is available. A recently improved analytical method based on gas chromatography of butyric acid methyl ester using an internal standard has been applied to determine the milk fat content in mixtures with beef tallow, lard, soybean oil, olive oil, sunflower oil, palm kernel oil and palm oil ranging from 1 to 90% milk fat content. Within the whole range of mixtures, mean absolute deviations between the determined and the actual milk fat content were below 0.5% and the maximum absolute deviation was not more than 1.0% when using the reference sample. The overall mean absolute deviation was 0.04% for milk fat contents of 1 to 10% and 0.28% for milk fat contents of 10 to 90%.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467644
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  • 55
    Digitale Medien
    Digitale Medien
    Determination of acids in Brazilian sugar cane spirits and other alcoholic beverages by HRGC-SPE (1998)
    Springer
    Chromatographia 48 (1998), S. 751-757 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Solid phase extraction ; Brazilian sugar cane spirit ; Lower fatty acids
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A gas chromatographic method for the analysis of seventeen acids in a water/ethanol matrix is described. The diluted samples were first concentrated by solid phase extraction. Nonanoic acid was the internal standard. A good separation profile was obtained for all compounds, including the isomers: n and iso-butyric acids, n and isovaleric acids and n and iso-caproic acids. The method is fast, sensitive (20–30 μg L−1) and has a good reproducibility (4–7 %). The recovery was in the range of 94%–116% for the medium chain acids (C7-C16). This method allowed the identification of fourteen acids in caninhas and other spirits. The total acid content and the profile of the exportation type caninhas are similar to the ones obtained for several international beverages.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467643
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  • 56
    Digitale Medien
    Digitale Medien
    Charge-transfer interactions between nucleophilic compounds and chromatographic packings containing chemically bonded Cu(II) complexes (1998)
    Springer
    Chromatographia 48 (1998), S. 284-292 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Metal complexes ; Chemically bonded phases ; Thermodynamic parameters ; Specific interactions
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary Results are presented of studies of packings containing copper (II) acetylacetonate (acac), hexafluoroacetylacetonate (hfac), and chloride, chemically bonded via β-dik-etonate groups. The retention parameters retention factor (k) specific retention volume (V g), and molecular retention index (M e) were measured and used to calculate the thermodynamic parameters free energy of adsorption (ΔG a) heat of adsorption (−ΔH a), and entropy of adsorption (ΔS a). These parameters enable, characterization of specific interactions between aromatic and cyclic hydrocarbons, ethers and thioethers and metal complexes chemically bonded, to a silica surface.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467684
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  • 57
    Digitale Medien
    Digitale Medien
    Data correlation in on-line solid-phase extraction-gas chromatography-atomic emission/mass spectrometric detection of unknown microcontaminants (1998)
    Springer
    Chromatographia 48 (1998), S. 273-283 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Atomic emission and MS detection ; Solid-phase extraction ; Aqueous samples
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A procedure is described for the (non-target) screening of hetero-atom-containing compounds in tap and waste water by correlating data obtained by gas chromatography (GC) using atomic emission (AED) and mass selective (MS) detection. Solid-phase extraction (SPE) was coupled on-line to both GC systems to enable the determination of microcontaminants at the 0.02–1 μg L−1 level in 7–50 mL of aqueous sample. The screening was limited to compounds present in at least one heteroatom-selective GC-AED trace above a predetermined concentration level. These compounds were identified by their partial formulae (AED) and the corresponding mass spectra, which were obtained from the GC-MS chromatogram via the retention index concept. The potential of the approach was demonstrated by the identification of target compounds as well as all unknowns present in tap and waste water above the predetermined threshold of 0.05 μg L−1 (tap water) or 0.5 μg L−1 (waste water).
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467683
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  • 58
    Digitale Medien
    Digitale Medien
    Gas chromatographic determination of major sterols in edible oils and fats using solid-phase extraction in sample preparation (1998)
    Springer
    Chromatographia 48 (1998), S. 745-750 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Solid-phase extraction ; Rapeseed oil ; Sterols
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary A capillary gas chromatographic method is described for the determination of major plant sterols and cholesterol in edible oils and fats. In the sample preparation procedure reversed-phase, solid-phase extraction with C18 adsorbent was used to extract the unsaponifiable matter and for sample cleanup after saponification. Sterols were quantitated as their trimethylsilylether derivatives using an internal standard method (betulin). The method was validated by recovery tests and analysis of two reference materials representing vegetable oil mixture and milk fat matrices. Average recoveries of spiked cholesterol and cholesterol acetate in rapeseed oil were 103±4% (n=12) and 101±3% (n=10), respectively. The sterol values determined in the reference materials were found to be in a good agreement with their given certified or indicative values. Applied to edible oils and fats, plant sterols and cholesterol at levels〉20 mg kg−1 could be accuratively quantitated.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467642
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  • 59
    Digitale Medien
    Digitale Medien
    Crown ether capped cyclodextrin used as stationary phase for capillary gas chromatography (1998)
    Springer
    Chromatographia 48 (1998), S. 817-822 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Crown ether capped cyclodextrin ; Chiral separations ; Isomer separations
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The solution of a new synthesized compound, mono-6-(1'-benzo-aza-15-crown-5)-2, 3, 6- permethyl-β-cyclodextrin, in the moderately polar polysiloxane OV-1701 was coated onto fused silica capillary column. The chromatographic characteristics including column efficiency, polarity and selectivity were studied. Excellent selectivity for the separation of enantiomers and positional isomers was obtained. The results show that the combined effect between the special caves of β-cyclodextrin and crown ether plays a significant role in the separation.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467654
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  • 60
    Digitale Medien
    Digitale Medien
    Gas chromatography with UV-vis molecular absorption spectrometry detection: Data acquisition and treatment when using a diode-array spectrophotometer (1998)
    Springer
    Chromatographia 48 (1998), S. 535-541 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; UV-Vis detection ; Gas phase absorption spectrometry ; Alcohols
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary This article describes a theoretical/practical study of the parameters which affect the chromatograms obtained when using a molecular diode-array spectrometer as the detector in gas chromatography. The objective is to offer some rules which permit the identification of the optimum signal/noise relation. To achieve this, we study the effect of the different parameters which affect the noise and how to reduce their impact, as well as alternatives for increasing the signal. All the options tested can be applied by correctly programming the spectrometer with BASIC programs, within reach of any use who has even a small understanding of programming. Finally, we consider the effect that the selection of the acquisition conditions may have on the chromatographic resolution. All the studies are carried out using a mixture of alcohols and phenols.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02466646
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  • 61
    Digitale Medien
    Digitale Medien
    Synthesis of a new liquid crystal, 4-[(4-chlorobenzyl)oxy]-4′-cyanoazobenzene and its use as stationary phase in gas-chromatography (1998)
    Springer
    Chromatographia 48 (1998), S. 427-430 
    Details
    ISSN: 1612-1112
    Schlagwort(e): Gas chromatography ; Liquid crystal stationary phase ; Packed columns
    Quelle: Springer Online Journal Archives 1860-2000
    Thema: Chemie und Pharmazie
    Notizen: Summary The separation ofm-, p-, o- xylenes andm-, p- ethyltoluenes was studied on a packed column with 2,5% of 4-[(4-chlorobenzyl)oxy]-4′-cyanoazobenzene (CBOCA) on Chromosorb W HP 100–120 mesh. The synthesis and study of the mesomorphic behaviour of CBOCA are presented. Temperature range for the separation ofm-, p-, o- xylenes (in this order of elution) is 125–85°C, at cooling. The best separation was achieved at about 90°C. The separation temperature domain ofm-ethyltoluene fromp- ethyltoluene is 160–85°C.
    Materialart: Digitale Medien
    URL: http://dx.doi.org/10.1007/BF02467715
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  • 62
    Digitale Medien
    Digitale Medien
    Synthesis, homopolymerization, and block copolymerization of N-ethyl-2-ethynyl-pyridinium trifluoromethanesulfonate with styrene and butadiene (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 703-712 
    Details
    ISSN: 0887-624X
    Schlagwort(e): synthesis ; homopolymerization ; block copolymerization ; N-ethyl-2-ethyl-pyridinium ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A novel acetylenic monomer 2-N-ethyl pyridinium trifluoromethane sulfonate (2EPyEtTf) was synthesized and polymerized. Diblock copolymers of 2EPyEtTf with styrene and with butadiene were prepared. Initiation of the polymerization by living anionic polystyryl--Li+ and polybutadienyl--Li+ (Scheme 1) resulted in polystyrene-block-poly(N-ethyl-2-ethynylpyridinium trifluoromethanesulfonate) (PS57PA8), and polybutadiene -block-poly(N-ethyl-2-ethynylpyridinium trifluoromethanesulfonate) (PB30PA8). These amphiphilic block molecules contain rigid, conjugated, and strongly hydrophilic polyacetylene chain fragments attached to hydrophobic polystyrene or flexible polybutadiene chain fragments. The structure of these copolymers was studied by FTIR, UV-visible, and NMR spectroscopy. GPC and viscometry were also used to obtain information on the molecular mass and the molecular mass distribution. Thermal behavior was investigated by means of TGA and DSC. Both block copolymers were shown to form stable monolayers at the air-water interface. The positively charged rigid polyacetylene portion of the copolymer is believed to be partially submerged, while the more flexible hydrophobic chains are forced out of the water. Multilayers of PB30PA8 deposited using the Langmuir-Blodgett technique were found to be less uniform than in the case of the previously reported polystyrene-block-poly(2EPyMeTf) (PS12PA4) copolymer (Balogh et al., Macromolecules, 29, 1996). Polycation-polyanion self-assembly deposition was also investigated, using polystyrenesulfonate (PSS) as polyanion. While PS57PA8/PSS layer-by-layer deposition was not uniform, it was found that PB30PA8/PSS gave homogenous and stable films on hydrophilic glass substrates. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 703-712, 1998
    Zusätzliches Material: 8 Ill.
    Materialart: Digitale Medien
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  • 63
    Digitale Medien
    Digitale Medien
    Kinetics of the photoinitiated inverse microemulsion polymerization of 2-methacryloyl oxyethyl trimethyl ammonium chloride (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 737-748 
    Details
    ISSN: 0887-624X
    Schlagwort(e): inverse microemulsion polymerization ; MADQUAT ; nucleation ; photopolymerization ; molecular weights ; flocculants ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The polymerization of inverse microemulsions of 2-methacryloyl oxyethyl trimethyl ammonium chloride stabilized by a blend of nonionic emulsifiers (a sorbitan sesquioleate and a sorbitan monooleate) and initiated by UV light in the presence of Azobis(isobutyronitrile) (AIBN) was investigated. The effect of initiator concentration, light intensity, emulsifier concentration, and dispersed phase weight fraction on the polymerization rate (Rp), number of polymer particles (Np), and polymer molecular weight (Mw) was studied. The application of this process to tubular reactors is discussed. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 737-748, 1998
    Zusätzliches Material: 15 Ill.
    Materialart: Digitale Medien
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  • 64
    Digitale Medien
    Digitale Medien
    Molecular weight distribution of crosslinked polymers produced in emulsion (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1127-1156 
    Details
    ISSN: 0887-624X
    Schlagwort(e): emulsion polymerization ; crosslinking and long-chain branching ; molecular weight distribution ; compartmentalization ; gel formation ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A kinetic model for evaluating the chain length distribution of a branched polymer produced in emulsion was developed. Chain branching occurring through any intermolecular mechanism is considered, namely, crosslinking, chain transfer to polymer and propagation to terminal double bond. The model accounts for active chain compartmentalization and, when coupled to a model able to describe the evolution of the polymerization system, allows evaluation of the cumulative properties of the produced polymer both in the pregel and postgel phases. The numerical difficulties related to the description of a rather wide polymer chain population and of gel formation are overcome by using the ‘numerical fractionation’ technique. A parametric analysis of both instantaneous and cumulative properties is reported and discussed, with special attention to the role of radical compartmentalization in determining the molecular weight properties of a polymer produced in emulsion. Significant differences with the molecular weights computed using models developed for homogeneous (non compartmentalized) systems have been found. A comparison with the predictions of Flory's statistical theory is also reported in terms of gel point and gel weight fraction. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1127-1156, 1998
    Zusätzliches Material: 12 Ill.
    Materialart: Digitale Medien
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  • 65
    Digitale Medien
    Digitale Medien
    Cationic copolymerization of cyclic ketene acetals: The effect of substituents on reactivity (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 861-871 
    Details
    ISSN: 0887-624X
    Schlagwort(e): 2-methylene-1,3-dioxane ; 4-methyl-2-methylene-1,3-dioxane ; 4,4,6-trimethyl-2-methylene-1,3-dioxane ; 2-methylene-1,3-dioxolane ; 4-methyl-2-methylene-1,3-dioxolane ; 4,5-dimethyl-2-methylene-1,3-dioxolane ; cationic copolymerization ; reactivity ratio ; relative reactivity ; ring-retained polymerization ; cyclic ketene acetals ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Cationic copolymerizations of 4-methyl-2-methylene-1,3-dioxane, 2 (M1), with 2-methylene-1,3-dioxane, 1 (M2); of 4,4,6-trimethyl-2-methylene-1,3-dioxane, 3 (M1), with 2-methylene-1,3-dioxane, 1 (M2); of 4-methyl-2-methylene-1,3-dioxolane, 5 (M1), with 2-methylene-1,3-dioxolane, 4 (M2); and of 4,5-dimethyl-2-methylene-1,3-dioxolane, 6 (M1), with 2-methylene-1,3-dioxolane, 4 (M2) were conducted. The reactivity ratios for these four types of copolymerizations were r1 = 1.73 and r2 = 0.846; r1 = 2.26 and r2 = 0.310; r1 = 1.28 and r2 = 0.825; r1 = 2.23 and r2 = 0.515, respectively. The relative reactivities of these monomers towards cationic polymerization are: 3 〉 2 〉 1; and 6 〉 5 〉 4. With both five- and six-membered ring cyclic ketene acetals, the reactivity increased with increasing methyl substitution on the ring. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 861-871, 1998
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 66
    Digitale Medien
    Digitale Medien
    Enzymatic activity of trypsin adsorbed on temperature-sensitive composite polymer particles (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 883-888 
    Details
    ISSN: 0887-624X
    Schlagwort(e): temperature sensitive ; particle ; emulsion polymerization ; morphology ; adsorption ; enzyme ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Two kinds of temperature-sensitive composite polymer particles were prepared by seeded emulsion copolymerizations of (dimethylamino)ethyl methacrylate and ethylene glycol dimethacrylate with 0.14 μm-sized polystyrene and 0.26 μm-sized poly(methylmethacrylate) seed particles. To evaluate the usefulness as a carrier for biomolecules, the enzymatic activities of trypsin adsorbed on these two composite polymer particles were measured at temperatures above and below each lower critical solution temperature (LCST). In both cases, adsorbed trypsin retained its enzymatic activity during repeated adsorption/desorption measurements. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 883-888, 1998
    Zusätzliches Material: 7 Ill.
    Materialart: Digitale Medien
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  • 67
    Digitale Medien
    Digitale Medien
    Synthesis of (1→6)-2,5-anhydro-D-glucitol through cyclopolymerization of 3,4-di-O-allyl-1,2 : 5,6-dianhydro-D-mannitol and optical resolution ability of its derivative in HPLC (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 901-909 
    Details
    ISSN: 0887-624X
    Schlagwort(e): (1→6)-2,5-anhydro-D-glucitol ; HPLC ; optical resolution ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The cyclopolymerization of 3,4-di-O-allyl-1,2 : 5,6-dianhydro-D-mannitol (1) was carried out using BF3·OEt2 and t-BuOK. The polymer obtained by the polymerization with BF3·OEt2 mainly consisted of (1→6)-bonded 3,4-di-O-allyl-2,5-anhydro-D-glucitol as the five-membered constitutional repeating unit, though it contained a small amount of other cyclic repeating units. On the other hand, during the polymerization using t-BuOK, the stereoregular polymer (1→6)-linked 3,4-di-O-allyl-2,5-anhydro-D-glucitol (2) was synthesized via a regio- and stereoselective mechanism. Cleavage of the allyl ether linkage in polymer 2 occurred to produce the polymer consisting of only 2,5-anhydro-D-glucitol units, i.e., (1→6)-2,5-anhydro-D-glucitol (3). Chromatographic enantioseparation of chloroquine and tröger base has been performed on (3,5-dimethylphenyl)carbamate and 4-methylbenzoate derivatives of 3 as a chiral stationary phase for high-performance liquid chromatography. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 901-909, 1998
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 68
    Digitale Medien
    Digitale Medien
    Model structures of thermoplastic polyesters having regularly alternated aromatic and fluorinated segments (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 939-947 
    Details
    ISSN: 0887-624X
    Schlagwort(e): fluorine ; perfluoropolyether ; polyester ; segmented ; thermoplastic ; interfacial synthesis ; thermal transitions ; dynamic-mechanical properties ; chemical resistance ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Linear segmented polyesters containing soft perfluoropolyether (PFPE) and hard aromatic segments are obtained by an interfacial polycondensation reaction of an acyl chloride-ended fluorinated prepolymer with various aromatic diphenols in the presence of phase transfer catalysts (PTC) as accelerators. Experimental conditions for reaching high molecular weights are discussed. The calorimetric analysis (DSC) of all the polyesters synthesized shows a typical biphasic morphology, where a very low Tg (〈 -110°C) corresponding to the segregated PFPE moiety, is always accompanied by another Tg or a higher melting temperature, depending on the nature of the hard phase. Dynamic-mechanical analysis (DMA) has been carried out confirming the DSC results and suggesting diversified mechanical behaviors at the various temperatures in line with the amorphous or semicrystalline nature of the polymer. Chemical resistance was finally tested by dipping in several solvents and chemicals. The new polyesters show high contact angles, a moderate swelling in many organic solvents and excellent stability in aggressive hydrolytic environments. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 939-947, 1998
    Zusätzliches Material: 6 Ill.
    Materialart: Digitale Medien
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  • 69
    Digitale Medien
    Digitale Medien
    Thermosensitive lactitol-based polyether polyol (LPEP) hydrogels (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 979-984 
    Details
    ISSN: 0887-624X
    Schlagwort(e): lactitol ; hydrogel ; polyether polyol ; PEO and PPO linkage ; swelling degree ; thermosensitivity ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A series of new thermosensitive polymer hydrogels were prepared by reacting acylated poly(ethylene glycol) bis(carboxymethyl) ether (PEGBCOCl) with lactitol-based polyether polyols (LPEP). The polyether polyols were generated from propoxylation of lactitol and have molecular weights ranging from 1337 to 4055 g/mol. The hydrogels absorb water up to 1000% of their dry weight and expel free water at temperatures at and above 30°C. The wide ranging swelling behavior and excellent thermosensitivity depend closely on the degree of crosslinking and the propylene oxide lengths in the polyols. Differential scanning calorimetry of the hydrogels showed two endotherms associated with the phase transitions of PO and EO segments in the hydrogel structures. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 979-984, 1998
    Zusätzliches Material: 4 Ill.
    Materialart: Digitale Medien
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  • 70
    Digitale Medien
    Digitale Medien
    Kinetic and microstructure studies of poly(ethylene-co-p-methylstyrene) copolymers prepared by metallocene catalysts with constrained ligand geometry (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1017-1029 
    Details
    ISSN: 0887-624X
    Schlagwort(e): Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: This paper discusses the poly(ethylene-co-p-methylstyrene) copolymers prepared by metallocene catalysts, such as Et(Ind)2ZrCl2 and [C5Me4(SiMe2NtBu)]-TiCl2, with constrained ligand geometry. The copolymerization reaction was examined by comonomer reactivity (reactivity ratio and comonomer conversion versus time), copolymer microstructure (DSC and 13C-NMR analyses) and the comparisons between p-methylstyrene and other styrene-derivatives (styrene, o-methylstyrene and m-methylstyrene). The combined experimental results clearly show that p-methylstyrene performs distinctively better than styrene and its derivatives, due to the cationic coordination mechanism and spatially opened catalytic site in metallocene catalysts with constrained ligand geometry. A broad composition range of random poly(ethylene-co-p-methylstyrene)copolymers were prepared with narrow molecular weight and composition distributions. With the increase of p-methylstyrene concentration, poly(ethylene-co-p-ethylstyrene)copolymer shows systematical decrease of melting point and crystallinity and increase of glass transition temperature. At above 10 mol % of p-methylstyrene, the crystallinity of copolymer almost completely disappears. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1017-1029, 1998
    Zusätzliches Material: 8 Ill.
    Materialart: Digitale Medien
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  • 71
    Digitale Medien
    Digitale Medien
    Synthesis and spinning of a thermotropic liquid crystal copolyester containing a semirigid cycloaliphatic spacer (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1473-1480 
    Details
    ISSN: 0887-624X
    Schlagwort(e): thermotropic polymers ; liquid crystalline polymers ; semirigid spacers ; melt spinning ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A thermotropic, liquid crystalline copolyester, based on 2-chlorohydroquinone, 1,4-cyclohexanedimethanol and terephthaloyl chloride, has been synthesized and melt spun. The cyclohexanedimethylene moiety acts as a semirigid spacer, introducing flexibility while preserving the thermotropic nature of the polymer. Melt-spun fibers were observed to have a high degree of molecular alignment owing to the nematic nature of the melt. Both polymer and fiber properties have been characterized. Characterization techniques used to this end include elemental analysis, hot-stage polarized light microscopy, scanning electron microscopy, dilute solution viscometry, Fourier transform infrared spectroscopy, nuclear magnetic resonance, differential scanning calorimetry, and thermogravimetric analysis. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1473-1480, 1998
    Zusätzliches Material: 9 Ill.
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  • 72
    Digitale Medien
    Digitale Medien
    Synthesis and properties of copolymers from 2-hydroxyethyl methacrylate-linked nonsteroidal antiinflammatory agents with methacrylic acid (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1481-1490 
    Details
    ISSN: 0887-624X
    Schlagwort(e): ibuprofen ; ketoprofen ; naproxen ; copolymer reactivity ; thermal stability ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Three nonsteroidal antiinflammatory drugs, 2-(4-isobutylphenyl)-propionic acid (ibuprofen), 2-(3-benzoylphenyl)-propionic acid (ketoprofen), and 2-(6-methoxy-2-naphthyl)-propionic acid (naproxen), were covalently linked with 2-hydroxyethyl methacrylate (HEMA). The drug-linked HEMA (M1) (ibuprofen-linked HEMA abbreviated as HI; ketoprofen-linked HEMA as HK, and naproxen-linked HEMA as HN), were respectively copolymerized with methacrylic acid (M2), MA, to obtain macromolecular prodrugs. The compositions of the copolymers were determined by means of a 1H-NMR spectroscopy and monomer reactivity ratios were estimated using the Kelen-Tüdös linear differential equation. The reactivity ratios are: r1 = 0.101 ± 0.012, r2 = 1.071 ± 0.065 for HI-MA; r1 = 0.344 ± 0.066, r2 = 0.966 ± 0.032 for HN-MA, and r1 = 0.650 ± 0.182, r2 = 1.032 ± 0.106 for HK-MA, respectively. The monomer reactivity toward to MA radical estimated from 1/r2 values is almost same for all three monomers (1/r2 ∼ 1). The glass transition temperatures of three drug-linked homopolymers go hand in hand with the steric hindrance of three drugs, i.e., ketoprofen 〉 naproxen ≫ ibuprofen calculated the minimum energy by computer molecular modeling. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1481-1490, 1998
    Zusätzliches Material: 8 Ill.
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  • 73
    Digitale Medien
    Digitale Medien
    Liquid chromatography of macromolecules at the critical adsorption point. II. Role of column packing: Bare silica gel (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1363-1371 
    Details
    ISSN: 0887-624X
    Schlagwort(e): liquid chromatography ; column packing ; bare silica gel ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Liquid chromatography of macromolecules at the critical adsorption point (LC CAP) presents a potentially very powerful method for molecular characterization of complex polymers. However, LC CAP applicability is limited due to various experimental problems. The pore sizes and surface chemistry of the column packings belong to the most important weak points of the method. The LC CAP behavior of poly(methyl methacrylate)s was investigated using bare silica gels of 6, 12, and 100 nm pore sizes and with various amounts of surface silanols. Tetrahydrofuran as the adsorption suppressing liquid and toluene as the adsorption promoting liquid were mixed to form the “nearly critical” eluents. Both pore size and surface chemistry of silica were found to strongly influence the retentive characteristics of the system in the critical adsorption area. Macromolecules that were large enough to be excluded from the packing pores hardly followed the LC CAP rules: their retention volumes changed irregularly with the polymer molar mass and their recovery dropped sharply. The narrow pore silica gel-packed column governed the elution patterns of the whole column set composed of silica gels with different pore sizes. This makes the conventional LC CAP characterization of common polymers with broader molar mass distribution impractical and even not feasible. A hybrid column system was proposed containing narrow pore nonadsorptive column added in series to the meso- and macroporous LC CAP silica gels. This narrow pore column would allow separation of gas, impurities, and system peaks from the polymer peaks. The possible successive changes of the surface of silica gel, e.g., due to formation of silanols by hydrolysis or due to irreversible adsorption of some admixtures from the sample or eluent may make the LC CAP irrepeatable. Pronounced peak broadening was observed in the critical adsorption area and this effect increased strongly with the polymer molar mass. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1363-1371, 1998
    Zusätzliches Material: 7 Ill.
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  • 74
    Digitale Medien
    Digitale Medien
    New polymer syntheses. XCVII. Hyperbranched LC-polyesters based on β-(4-hydroxyphenyl)propionic acid and 4-hydroxybenzoic acid (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1397-1405 
    Details
    ISSN: 0887-624X
    Schlagwort(e): hyperbranched polyesters ; nematic phase ; phloritic acid ; vectra ; melt rheology ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Two classes of liquid crystalline hyperbranched copolyesters were prepared by the copolycondensation of silylated 3,5-bis(acetoxy)benzoic acid with mixtures of mesogenic difunctional monomers. The first class of LC-copolyesters was obtained from 1 : 1 mixtures (molar ratio) of silylated β-(4-acetoxyphenyl)propionic acid and silylated 4-acetoxybenzoic acid (poly(HPPA/HBA)). The second class of LC-copolyesters was obtained by additional copolycondensation of silylated 6-acetoxy-2-naphthoic acid. The hyperbranched copolyesters of this ternary system poly(HPPA/HBA/HNA) proved to be less crystalline in contrast to the binary system. In both classes of LC-copolyesters the degree of branching was varied via the feed ratio of 3,5-dihydroxybenzoic acid. A minimum segment length of 6 difunctional monomer units between the branching points is required to establish a nematic phase. However, a greater segment length is needed to obtain a homogeneous LC-phase. The poly(HPPA/HBA) copolyesters were also characterized by melt rheology. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1397-1405, 1998
    Zusätzliches Material: 8 Ill.
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  • 75
    Digitale Medien
    Digitale Medien
    Polymerization of acrylates by atom transfer radical polymerization. Homopolymerization of 2-hydroxyethyl acrylate (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1417-1424 
    Details
    ISSN: 0887-624X
    Schlagwort(e): 2-hydroxyethyl acrylate ; poly(2-hydroxyethyl acrylate) ; atom transfer radical polymerization (ATRP) ; controlled free radical polymerization ; MALDI-MS ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The application of atom transfer radical polymerization (ATRP) to the homopolymerization of 2-hydroxyethyl acrylate, a functional monomer, is reported. The polymerizations exhibit first-order kinetics, and molecular weights increase linearly with conversion. Polydispersities remain low throughout the polymerization (Mw/Mn ≈ 1.2). Reactions were conducted in bulk and in 1 : 1 (by volume) aqueous solution; the latter demonstrates the resilience of ATRP to protic media. Analysis of poly(2-hydroxyethyl acrylate) by MALDI-MS and 1H-NMR shows Mn,exp to be much closer to Mn,th than those observed by SEC using polystyrene standards. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1417-1424, 1998
    Zusätzliches Material: 4 Ill.
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  • 76
    Digitale Medien
    Digitale Medien
    Unbridged bivalent lanthanidocenes for isotactic and stereomultiblock polymerization of methyl methacrylate (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1599-1606 
    Details
    ISSN: 0887-624X
    Schlagwort(e): bivalent organolanthanides ; polymerization ; methyl methacrylate ; stereomultiblock polymer ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Bivalent organolanthanides with unbridged substituted indenyl or fluorenyl ligands (1-SiMe3Ind)2YTHF (I), (9-SiMe3Flu)2YTHF (II), were found to efficiently catalyze the stereoregular polymerization of methyl methacrylate. The microstructure of resultant polymers was shown to be dependent of a conformation that the ligands adopt at the polymerization temperature. The formation of isotactic rich PMMAs from complex II was proposed to be associated with the fluctuation of the 9-trimethylsilylfluorenyls around a C2 symmetric twisted-conformation. The formation of the multi(syndioPMMA-block-iso-PMMA) polymers from the mixture of rac- and meso-isomers of I was rationalized on the basis of competing conjugate addition and inversion of the metallocene conformation. Surprisingly, both rac- and meso-isomers of I were found to operate with similar activity and stereospecifity, although the stereospecific operation of the meso-form was not completely understandable. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1599-1606, 1998
    Zusätzliches Material: 1 Ill.
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  • 77
    Digitale Medien
    Digitale Medien
    Novel hydrogen-transfer polymerization of vinyl monomer derived from p-toluenesulfonyl isocyanate and acrylamide (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1491-1494 
    Details
    ISSN: 0887-624X
    Schlagwort(e): sulfonyl isocyanate ; acrylamide ; hydrogen-transfer polymerization ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: No abstract.
    Zusätzliches Material: 1 Ill.
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  • 78
    Digitale Medien
    Digitale Medien
    p-Nitrophenol permeability and temperature characteristics of an acryloyl-L-proline methyl ester-based porous gel membrane (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1495-1500 
    Details
    ISSN: 0887-624X
    Schlagwort(e): acryloyl-L-proline methyl ester (A-ProOMe) ; methacryloyl-L-proline methyl ester (MA-ProOMe) ; porous gel membranes ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Thermoresponsive porous gel membranes were synthesized by a simultaneously occurring process consisting of radiation-induced polymerization and crosslinking in aqueous solutions at various concentrations of acryloyl-L-proline methyl ester(A-ProOMe) without a crosslinker. Permeation of p-nitrophenol (PNP) through a thermoresponsive porous gel membrane obtained at a monomer concentration of 80% (w/w) drastically reduced around 14°C, the lower critical solution temperature (LCST) of linear poly(A-ProOMe) in water, from 0.60 × 10-3 cm/min at 10°C to no permeation at 18°C, accompanied by changes in both size and shape of pores associated with gel shrinkage. Moreover, it was found that porous gel membranes with a porosity of approximately 60% had a greater PNP permeability constant through porous gel membranes with mutually connected pores obtained at a monomer concentration of 50% (w/w) than individually supported pores obtained at a monomer concentration of 70% (w/w). © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1495-1500, 1998
    Zusätzliches Material: 9 Ill.
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  • 79
    Digitale Medien
    Digitale Medien
    Polymerization under a magnetic field. VI. Triplet dye-sensitized photopolymerization of acrylamide and methyl methacrylate (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1509-1513 
    Details
    ISSN: 0887-624X
    Schlagwort(e): methylene blue ; dye-sensitized photopolymerization ; magnetic field ; triplet state ; acrylamide ; methyl methacrylate ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Methylene blue sensitized photopolymerization of acrylamide (AM) and methyl methacrylate (MMA) using triethanolamine or the sodium salt of EDTA as a reducing agent has been investigated under the influence of a magnetic field (0-7.3 kG). There was no effect of the magnetic field (MF) on the polymerization of AM and MMA in aqueous medium. However, in the water-methanol mixture (1 : 1) the yield of polymer decreases and the molecular weight increases in both cases under MF. This has been explained on the basis of the triplet mechanism. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1509-1513, 1998
    Zusätzliches Material: 5 Tab.
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  • 80
    Digitale Medien
    Digitale Medien
    Porous monodisperse poly(divinylbenzene) microspheres by precipitation polymerization (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1543-1551 
    Details
    ISSN: 0887-624X
    Schlagwort(e): polymer microspheres ; monodisperse ; crosslinked ; porosity ; porogen ; precipitation polymerization ; divinylbenzene ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The precipitation polymerization of commercial divinylbenzene in acetonitrile containing up to 40 vol. % toluene or other cosolvents is shown to produce novel porous monodisperse poly(divinylbenzene) microspheres. These microspheres have diameters between 4 and 7 μm, total pore volumes of up to 0.52 cm3/g, and surface areas of up to 800 m2/g. As no surfactant nor stabilizer was used in the preparation of these particles, their surfaces are free of any such residues. The particles were slurry-packed into stainless steel columns for size exclusion chromatography evaluation, and the results show an exclusion limit at molecular weights of 500 g/mol. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1543-1551, 1998
    Zusätzliches Material: 6 Ill.
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  • 81
    Digitale Medien
    Digitale Medien
    (Diisopropylamido) bis (methylcyclopentadienyl) lanthanides as single-component initiators for polymerization of methyl methacrylate (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1593-1597 
    Details
    ISSN: 0887-624X
    Schlagwort(e): MMA ; polymerization ; (diisopropylamido)bis(methylcyclopentadienyl)lanthanides ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: It was first found that (diisopropylamido)bis(methylcyclopentadienyl)lanthanides (MeC5H4)2LnN(i-Pr)2(THF) (Ln = Yb (1), Er (2), Y (3)) exhibit extremely high catalytic activity in the polymerization of methyl methacrylate. The reactions can be carried out over a quite broad range of polymerization temperatures from -78 to 40°C. The catalytic activity of the complexes increases with an increase of ionic radii of the metal elements, i.e. Y 〉 Er 〉 Yb. The results of GPC (gel permeation chromatography) indicate that the number-average molecular weights (Mn) of polymers obtained exceed 100 × 103 and the molecular weight distribution (Mw/Mn) becomes broad with the increase of temperature. Furthermore highly syndiotactic PMMA (87.7%) can be obtained by lowering the reaction temperature to -78°C. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1593-1597, 1998
    Zusätzliches Material: 1 Ill.
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  • 82
    Digitale Medien
    Digitale Medien
    Preparation and properties of poly(styrene-co-maleic anhydride)/silica hybrid materials by the in situ sol-gel process (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1607-1613 
    Details
    ISSN: 0887-624X
    Schlagwort(e): sol-gel ; hybrid material ; poly(styrene-co-maleic anhydride) ; tetraethoxysilane ; (3-aminopropyl)triethoxysilane ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Poly(styrene-co-maleic anhydride)/silica hybrid material has been successfully prepared from styrene-maleic anhydride copolymer and tetraethoxysilane (TEOS) in the presence of a coupling agent (3-aminopropyl)triethoxysilane (APTES) by an in situ sol-gel process. It was observed that the gel time of sol-gel solution was dramatically influenced by the amount of APTES. The hybrid material exhibits optical transparency almost as good as both silica gel and the copolymer. The covalent bonds between organic and inorganic phases were introduced by the aminolysis reaction of the amino group with maleic anhydride units of copolymer to form a copolymer bearing trimethoxysilyl groups, which undergo hydrolytic polycondensation with TEOS. The differential scanning calorimetry (DSC) showed that the glass transition temperature of the hybrid materials increases with increasing of SiO2 composition. Photographs of scanning electron microscopy (SEM) and atomic force microscopy (AFM) inferred that the size of the inorganic particles in the hybrid materials was less than 20 nm. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1607-1613, 1998
    Zusätzliches Material: 8 Ill.
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  • 83
    Digitale Medien
    Digitale Medien
    Influence of plasma treatment on the molar mass of poly(ethylene terephthalate) investigated by different chromatographic and spectroscopic methods (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1639-1648 
    Details
    ISSN: 0887-624X
    Schlagwort(e): poly(ethylene terephthalate) (PET) ; plasma ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The influence of different types of low and atmospheric pressure plasma on poly(ethylene terephthalate) (PET) has been studied in terms of changes in molar mass and molar mass distribution. Apart from a variation of plasma gases (oxygen, helium) different types of plasma (microwave, radio frequency, corona discharge) were used for the plasma surface modification. The changes in molar mass and types of functional end groups of lower molar mass products were investigated by means of matrix-assisted laser desorption/ionization time of flight mass spectrometry (MALDI-TOFMS), whereas the high-molar mass fraction was analyzed by means of size-exclusion chromatography (SEC). The formation of crosslinked products during exposure to a helium plasma, which emits preponderately energy-rich and intense ultraviolet radiation, was proved by means of thermal field-flow fractionation (ThFFF). This method combined with a multiangle laser light scattering (MALLS) detector allows detection of weakly crosslinked polymers and microgels. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1639-1648, 1998
    Zusätzliches Material: 9 Ill.
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  • 84
    Digitale Medien
    Digitale Medien
    Synthesis and properties of poly(ether imide)s derived from 2,6-bis(3,4-dicarboxyphenoxy)naphthalene dianhydride and aromatic diamines (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1657-1665 
    Details
    ISSN: 0887-624X
    Schlagwort(e): 2,6-bis(3,4-dicarboxyphenoxy)naphthalene dianhydride ; poly(ether imide)s ; thermal behavior ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A new naphthalene unit-containing bis(ether anhydride), 2,6-bis(3,4-dicarboxyphenoxy)naphthalene dianhydride, was synthesized in three steps starting from the nucleophilic nitrodisplacement reaction of 2,6-dihydroxynaphthalene and 4-nitrophthalonitrile in N,N-dimethylformamide (DMF) solution in the presence of potassium carbonate, followed by alkaline hydrolysis of the intermediate bis(ether dinitrile) and subsequent dehydration of the resulting bis(ether diacid). High-molar-mass aromatic poly(ether imide)s were prepared using a conventional two-step polymerization process from the bis(ether anhydride) and various aromatic diamines. The intermediate poly(ether amic acid)s had inherent viscosities of 0.65-2.03 dL/g. The films of poly(ether imide)s derived from two rigid diamines, i.e. p-phenylenediamine and benzidine, crystallized during the thermal imidization process. The other poly(ether imide)s belonged to amorphous materials and could be fabricated into transparent, flexible, and tough films. These aromatic poly(ether imide) films had yield strengths of 104-131 MPa, tensile strengths of 102-153 MPa, elongation to break of 8-87%, and initial moduli of 1.6-3.2 GPa. The glass transition temperatures (Tg's) of poly(ether imide)s were recorded in the range of 220-277°C depending on the nature of the diamine moiety. All polymers were stable up to 500°C, with 10% weight loss being recorded above 550°C in both air and nitrogen atmospheres. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1657-1665, 1998
    Zusätzliches Material: 2 Ill.
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  • 85
    Digitale Medien
    Digitale Medien
    A simple method for the anionic polymerization of α-carbonyl acids in water (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1683-1683 
    Details
    ISSN: 0887-624X
    Schlagwort(e): Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Zusätzliches Material: 1 Ill.
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  • 86
    Digitale Medien
    Digitale Medien
    Novel aromatic polyhydrazides and poly(amide-hydrazide)s based on “multiring” flexible dicarboxylic acids (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1847-1854 
    Details
    ISSN: 0887-624X
    Schlagwort(e): polyhydrazides ; poly-1,3,4-oxadiazoles ; thermal behavior ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Two flexible dicarboxylic acid monomers, 4,4′-[isopropylidenebis(1,4-phenylene)dioxy]dibenzoic acid (1) and 4,4′-[hexafluoroisopropylidenebis(1,4-phenylene)-dioxy]dibenzoic acid (3), were synthesized from readily available compounds in two steps in high yields. High molecular-weight polyhydrazides and poly(amide-hydra-zide)s were directly prepared from dicarboxylic acids 1 and 3 with terephthalic dihydrazide (5), isophthalic dihydrazide (6), and p-aminobenzhydrazide (7) by the phosphorylation reaction by means of diphenyl phosphite (DPP) and pyridine in N-methyl-2-pyrrolidone (NMP)/LiCl, or prepared from the diacyl chlorides of 1 and 3 with the hydrazide monomers 5-7 by the low-temperature solution polycondensation in NMP/LiCl. Less favorable results were obtained when using triphenyl phosphite (TPP) instead of DPP in the direct polycondensation reactions. Except for those derived from terephthalic dihydrazide, the resulting polyhydrazides and poly(amide-hydrazide)s could be cast into colorless, flexible, and tough films with good tensile strengths. All the hydrazide polymers and copolymers are amorphous in nature and are readily soluble in various polar solvents such as NMP and dimethyl sulfoxide (DMSO). Their Tgs were recorded in the range of 162-198°C and could be thermally cyclodehydrated into the corresponding polyoxadiazoles and poly(amide-oxadiazole)s approximately in the region of 300-380°C, as evidenced by the DSC thermograms. The oxadiazole polymers and copolymers showed a dramatically decreased solubility and higher Tg when compared to their respective hydrazide prepolymers. They exhibited Tgs of 190-216°C and were stable up to 450°C in air or nitrogen. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1847-1854, 1998
    Zusätzliches Material: 4 Ill.
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  • 87
    Digitale Medien
    Digitale Medien
    Novel polyisobutylene/poly(dimethylsiloxane) bicomponent networks. I. Synthesis and characterization (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1891-1899 
    Details
    ISSN: 0887-624X
    Schlagwort(e): polyisobutylene ; poly(dimethylsiloxane) ; hydrosilation ; bicomponent networks ; molecular weight between crosslinks ; network functionality ; sol fraction ; extractables ; model networks ; end-linking ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The synthesis of novel polyisobutylene (PIB)/poly(dimethylsiloxane) (PDMS) bicomponent networks is described. The synthesis strategy (see Figure 1) was to prepare well-defined and -characterized allyl-tritelechelic polyisobutylenes [φ(PIB - C - C=C)3] and SiH-ditelechelic poly(dimethylsiloxanes) (HSi-PDMS-SiH) and then crosslink these moieties by hydrosilation. The φ(PIB - C - C=C)3 was prepared by living isobutylene polymerization followed by end-quenching with allyltrimethylsilane, whereas the HSi-PDMS-SiH was obtained by equilibrium polymerization of octamethylcyclotetrasiloxane and tetramethyldisiloxane. The detailed structures of the starting polymers were characterized by GPC and 1H-NMR spectroscopy. A series of PIB/PDMS bicomponent networks of varying compositions and average molecular weights between crosslinks (Mc) of ∼ 20,000 g/mol were assembled. Optimum crosslinking conditions were defined in terms of H2PtCl6 catalyst concentration, nature of solvent, time, temperature, and stoichiometry of ∼ CH2CH=CH2/∼SiH groups, allowing for the convenient synthesis of well-defined model bicomponent networks. Swelling studies and elemental analysis confirm the correctness of the synthetic strategy. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1891-1899, 1998
    Zusätzliches Material: 6 Ill.
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  • 88
    Digitale Medien
    Digitale Medien
    Novel polyisobutylene/poly(dimethylsiloxane) bicomponent networks. II. Network structure and property characterization (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1901-1910 
    Details
    ISSN: 0887-624X
    Schlagwort(e): polyisobutylene ; poly(dimethylsiloxane) ; bicomponent networks ; network structure ; molecular weight between crosslinks ; network properties ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The first part of this series concerned the synthesis of novel polyisobutylene (PIB)/poly(dimethylsiloxane) (PDMS) bicomponent networks; the present paper concerns the structure and property characterization of a series of bicomponent networks of varying compositions (PIB wt %/PDMS wt % = 92/8, 70/30, 50/50, 35/65) having average molecular weights between crosslinks (Mc) of ˜ 20,000 g/mol. According to network structure analysis by uniaxial equilibrium stress-strain measurements, the experimental Mc's are in excellent agreement with theoretical values. Hydrosilation end-linking efficiency was quantitated by the amount of sol and functional group analysis by 1H-NMR spectroscopy. NMR evidence indicates double-bond isomerization during hydrosilation. Network compositions by elemental analysis together with the low sol fractions indicate efficient crosslinking. These data suggest highly efficient network formation and well-defined bicomponent network structures. While PIB and PDMS showed Tg's at -72 and -124°C, respectively, the bicomponent network did not exhibit clearly discernible phase transitions. The heat stability of bicomponent networks increased slightly with increasing PDMS content showing initial (10%) degradation temperatures at ˜ 380°C in nitrogen and ˜ 320°C in air. Tensile strengths and elongations were dependent on composition and varied in the 0.6-3.8 MPa and 600-1100% ranges, respectively. The swelling behavior was not much affected by composition. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1901-1910, 1998
    Zusätzliches Material: 8 Ill.
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  • 89
    Digitale Medien
    Digitale Medien
    Copolymerization of carbon monoxide and norbornene derivatives with ester groups by palladium catalyst (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1785-1790 
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    ISSN: 0887-624X
    Schlagwort(e): carbon monoxide ; norbornene ester ; glass transition temperature ; palladium catalyst ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: In this article we will discuss the synthesis of the new copolymers of norbornene derivatives with an ester group and carbon monoxide, using Pd(CH3CN)4(BF4)2 as a catalyst and 2,2′-bipyridine as a ligand in nitromethane/methanol at 60°C. Elementary analysis, infrared spectra, and NMR spectra indicated that copolymers contain ketone, ester, and bicyclic structures. Methanol functions as the coinitiator and chain transfer agent in copolymerization. A decrease in the molar ratio of [CH3OH]/[Pd] caused an increase in molecular weight and a decrease in yield of the copolymer. The number-average molecular weight of copolymers (Mn) ranged from 3800 to 5300, and the glass transition temperature (Tg) ranged from -32 to 117°C. Thermal analysis revealed that both T10%d and Tmaxd exceeded 180 and 230°C, respectively. Linear long-chain substituents such as n-C11H23C(O)—O—CH2— drastically reduced Tg to a value of -32°C. In general, copolymers having a longer linear side-chain substituents of ester on norbornene have a more desirable solubility. Moreover, X-ray diffraction demonstrated that the degree of crystallinity decreases with an increasing length of side chain substituents. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1785-1790, 1998
    Zusätzliches Material: 2 Ill.
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  • 90
    Digitale Medien
    Digitale Medien
    LC-polyimides XXXIV. Noncrystalline thermotropic copoly(ester-imide)s based on PET (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1813-1820 
    Details
    ISSN: 0887-624X
    Schlagwort(e): poly(ester-imide)s ; poly(ethylene terephthalate) ; transesterification, nematic phase ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Four series of copoly(ester-imide)s (co-PEIs) were prepared by transesterification of poly(ethylene terephthalate), PET, with N-(4-carboxyphenyl)trimellitimide and an acetylated diphenol. Methylhydroquinone, tert. butylhydroquinone, phenylhydroquinone, and 2,7-dihydroxynaphthalene were used as diphenols. The chemical structures of these co-PEIs were characterized by chemical analyses, 1H-, and 13C-NMR spectra. A low degree of crystallinity was observed when the PET content was above 85% mol %. Between 60 and 80 mol % PET all co-PEIs are biphasic, whereas below 60 mol % the co-PEIs form a homogeneous nematic melt and below the glass transition temperature (Tg) a nematic glass. The Tgs vary continously with the molar composition but the mechanical properties drop sharply when the nematic phase changes to an isotropic one. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1813-1820, 1998
    Zusätzliches Material: 7 Ill.
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  • 91
    Digitale Medien
    Digitale Medien
    Morphology and grafting of oxazoline-functional polymer particles with various carboxylic acids (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1821-1827 
    Details
    ISSN: 0887-624X
    Schlagwort(e): morphology ; grafting ; oxazoline-functionalized polymer particles ; carbolic acids ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Oxazoline-functionalized, crosslinked PMMA-particles, prepared by free radical nonaqueous dispersion polymerization, were grafted with n-decanoic acid and carboxylic acid-terminated polystyrene. Oxazoline groups, separated by an alkylspacer from the PMMA backbone, showed enhanced mobility with respect to the backbone, as evaluated by solid-state NMR spectroscopy using a dipolar filter. As a function of molecular mass of the carboxylic acid, the oxazoline conversion varied from 70 mol % for n-decanoic acid to 1% for monocarboxylate-terminated polystyrene CT-PS with Mn: 15,900 g/mol. Morphological studies, performed by TEM, showed that reaction with acid terminated polystyrene results exclusively in interfacial grafting at the particle surface. At low grafting levels a raspberry-like morphology was obtained, whereas grafting levels exceeding 14 wt % CT-PS resulted in core-shell morphology. Core-shell morphology was also verified by static light scattering using toluene solvent, which is isorefractive to the PMMA core. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1821-1827, 1998
    Zusätzliches Material: 6 Ill.
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  • 92
    Digitale Medien
    Digitale Medien
    Aminolysis kinetics of model and polymer-bound anhydride moieties in low- and high-viscosity media (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 1573-1582 
    Details
    ISSN: 0887-624X
    Schlagwort(e): amic acid ; secondary amine ; maleic anhydride ; melt reaction kinetics ; model compounds ; polymer-bound functional groups ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: This study examines the legitimacy of using the reaction kinetics of low molecular weight model compounds in solution to predict the chemical kinetics of polymer-bound species in a homogeneous melt. The reaction under study takes place between an aliphatic secondary amine, diisooctadecylamine (DiOA), and a 5-membered anhydride ring, saturated maleic anhydride (MA), forming an amic acid product. The MA species was present as a pendant graft on either a model compound, dodecane-g-(maleic anhydride) (dodecane-g-MA), or a polymer chain, linear low-density polyethylene-g-(maleic anhydride) (LLDPE-g-MA). Pseudo-second-order kinetics of the anhydride consumption are followed by infrared spectroscopy, either in situ in dodecane solution or by scanning frozen film samples taken from a linear low-density polyethylene melt. It was found that the LLDPE-g-MA/DiOA system reacted at a slightly slower rate than the dodecane-g-MA/DiOA system in the low-viscosity solution at 140°C. In the melt, the dodecane-g-MA/DiOA system experienced a small decrease in the overall reaction rate compared to the same reaction carried out in dodecane. However, the LLDPE-g-MA/DiOA system underwent a 65% decrease in the observed second-order rate constant on going from a solution to the melt. To explain these phenomena, the effects of diffusion, miscibility, and chain entanglements in the melt are examined here. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 1573-1582, 1998
    Zusätzliches Material: 3 Ill.
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  • 93
    Digitale Medien
    Digitale Medien
    New polymer syntheses. XC. A-B-A triblock copolymers with hyperbranched polyester A-blocks (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 31-38 
    Details
    ISSN: 0887-624X
    Schlagwort(e): triblock copolymers ; polycondensations ; telechelic character ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Telechelic oligo(ether-ketone)s containing two trimethylsiloxy end groups and one methyl group per repeating unit were prepared by polycondensation of 4-fluoro-2′-methyl-4′-(trimethylsiloxy)benzophenone. The telechelic character was achieved by cocondensation of a small amount of silylated bisphenol-P. The end groups of the silylated oligo(ether-ketone)s were acetylated by means of acetyl chloride. On the basis of 1H-NMR end group analyses two samples of α,ω-bis(acetoxy) oligo(ether-ketone)s with DP = 14 and DP ∼ 28 were obtained. These oligo(ether-ketone)s and a 70 or 140 fold molar amount of silylated 3,5-bis(acetoxy)benzoic acid were polycondensed at 270°C in bulk. The resulting A-B-A triblock copolymers were fractionated by dissolution in tetrahydrofuran. In three out of four experiments a small fraction of precipitated material rich in oligo(ether-ketone) was isolated. The purified triblock copolymers were characterized by inherent viscosities and NMR spectra. For those samples containing the long oligo(ether-ketone) block a low degree of crystallinity was observed after annealing. Four additional polycondensations were conducted with an initial reaction temperature of 290°C. In this way a completely soluble and amorphous triblock copolymer was obtained. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 31-38, 1998
    Zusätzliches Material: 8 Ill.
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  • 94
    Digitale Medien
    Digitale Medien
    Liquid crystalline epoxy resins by polyaddition of diglycidyl ether of 4,4′-dihydroxybiphenyl and difunctional aromatic compounds (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 21-29 
    Details
    ISSN: 0887-624X
    Schlagwort(e): liquid crystalline polymers ; epoxy resins ; thermotropic ; polymer chain extension ; catalytic polyaddition ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: This work is a continuation of the authors' earlier investigations of liquid crystalline epoxy resins prepared from diglycidyl ether of 4,4′-dihydroxybiphenyl (DGE-DHBP), which was used as a mesogenic agent, and aliphatic dicarboxylic compounds, which were used as flexible spacers. In this paper, the synthesis and characterization of liquid crystalline epoxy resins, prepared from DGE-DHBP and difunctional aromatic compounds are described. Three series of liquid crystalline epoxy resins were prepared by chain extension of DGE-DHBP with isomeric hydroxybenzoic and benzenedicarboxylic acids as well as diphenols. An isophthalic-terminated polyether was applied to decrease the temperature of phase transitions. The syntheses were carried out by catalytic polyaddition in the melt. Triphenylphosphine was applied as the catalyst. The resulting epoxy resins were investigated by DSC, polarizing microscope as well as by X-ray and IR spectroscopy. The phase transition temperatures and the type of mesophase of the resulting products depend on the character of the functional groups in the chain extender and on the position of the functional groups in the aromatic ring. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 21-29, 1998
    Zusätzliches Material: 4 Ill.
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  • 95
    Digitale Medien
    Digitale Medien
    Preparation and properties of new soluble aromatic polyimides from 2,2′-bis(3,4-dicarboxyphenoxy)biphenyl dianhydride and aromatic diamines (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 2021-2027 
    Details
    ISSN: 0887-624X
    Schlagwort(e): 2,2′-bis(3,4-dicarboxyphenoxy)biphenyl dianhydride ; aromatic polyimides ; solubility ; thermal behavior ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A new aromatic tetracarboxylic dianhydride having a crank and twisted noncoplannar structure, 2,2′-bis(3,4-dicarboxyphenoxy)biphenyl dianhydride, was synthesized by the reaction of 4-nitrophthalonitrile with biphenyl-2,2′-diol, followed by hydrolysis and cyclodehydration. The biphenyl-2,2′-diyl-containing aromatic polyimides having inherent viscosities up to 0.66 dL/g were obtained by the conventional two-step procedure starting from the dianhydride monomer and various aromatic diamines. Most of the polyimides were readily soluble in amide-type solvents such as N,N-dimethylacetamide and N-methyl-2-pyrrolidone. The aromatic polyimides had glass transition temperatures in the range of 205-242°C, and began to lose weight around 415°C, with 10% weight loss being recorded at about 500°C in air. © 1998 John Wiley & Sons, Inc. J. Polym. Sci. A Polym. Chem. 36: 2021-2027, 1998
    Zusätzliches Material: 2 Ill.
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  • 96
    Digitale Medien
    Digitale Medien
    Studies of lipase-catalyzed polyesterification of an unactivated diacid/diol system (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 2069-2079 
    Details
    ISSN: 0887-624X
    Schlagwort(e): Candida antarctica lipase ; Novozym 435® ; polyester ; enzymatic polymerization ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Preliminary enzymatic polymerization studies in the simple stoichiometric adipic acid/butane-1,4-diol system using lipase B from Candida antarctica, immobilized as Novozym 435®, suggest that in solvent-free conditions a step-growth mechanism operates involving the sequential addition of an AB synthon by esterification mode only. Conversely, in toluene as solvent there is a change to the more facile transesterification mode in line with the conventional polyesterification procedure, pointing to a change in specificity of the lipase. Evidence is drawn from qualitative studies using a series of synthetic intermediates, enabling authentication of product mixtures together with an indication of the comparative reactivity of species along the proposed reaction pathway. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 2069-2080, 1998
    Zusätzliches Material: 5 Ill.
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  • 97
    Digitale Medien
    Digitale Medien
    Mechanical properties of blends of PAMAM dendrimers with poly(vinyl chloride) and poly(vinyl acetate) (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 2111-2117 
    Details
    ISSN: 0887-624X
    Schlagwort(e): dendritic polymer ; blends ; coatings ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: Hybrid blends of poly(amidoamine) PAMAM dendrimers with two linear high polymers, poly(vinyl chloride), PVC, and poly(vinyl acetate), PVAc, are reported. The interaction between the blend components was studied using dynamic mechanical analysis, xenon nuclear magnetic resonance (NMR) spectroscopy, and tensile property measurements. The data suggest a much higher degree of interaction between components of PVAc-containing blends compared to those containing PVC. © 1998 John Wiley & Sons, Inc. J Polym Sci A: Polym Chem 36: 2111-2117, 1998
    Zusätzliches Material: 4 Ill.
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  • 98
    Digitale Medien
    Digitale Medien
    Side chain liquid crystal polyurethanes with azobenzene mesogenic moieties: Influence of spacer length on hydrogen bonding at different temperatures (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 2135-2146 
    Details
    ISSN: 0887-624X
    Schlagwort(e): SCLC polyurethanes ; azobenzene mesogenic group ; alkyl spacer ; bilayer smectic phases ; hydrogen bonding ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: A series of side chain liquid crystal polyurethanes (CnCNPs), in which the spacer length was varied from 2 to 12 methylene units, were synthesized by the addition polymerization of α-[bis(2-hydroxyethyl)amino]-ω-(4-cyanoazobenzene-4′-oxy)alkanes (CnCN-diols) with hexamethylene diisocyanate. The liquid crystalline properties of CnCNPs were characterized by means of differential scanning calorimetry, polarizing optical microscopy, and X-ray diffraction. Polyurethanes with spacer length 4 or higher exhibited mesomophic properties. C4CNP and C5CNP exhibited an enantiotropic nematic mesophase, while C6-C12CNPs exhibited enantiotropic bilayer smectic mesophases. CnCNPs have a high tendency to crystallize; crystallization is kinetically controlled. Polyurethane's backbone crystallization is closely related to hydrogen bonding. To establish the role of hydrogen bonding in mesophase formation as well as crystallization, Fourier transform infrared spectroscopy studies of CnCNPs were carried out at different temperatures focusing on H-bonds between the N—H and C=O groups of the urethane backbone. With increasing temperature, C=O and N—H stretching bands were evenly shifted to higher wavenumbers, with two exceptions (C4CNP and C5CNP) discussed in detail in the text. © 1998 John Wiley & Sons, Inc. J. Polym. Sci. A Polym. Chem. 36: 2135-2146, 1998
    Zusätzliches Material: 11 Ill.
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  • 99
    Digitale Medien
    Digitale Medien
    Initiation mechanisms in free radical polymerization: Competitive reaction of cyanoisopropyl radicals with styrene and acrylonitrile (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 2169-2176 
    Details
    ISSN: 0887-624X
    Schlagwort(e): free radical ; initiation ; styrene ; acrylonitrile ; copolymerization ; nitroxide trapping ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: The competitive reactions of cyanoisopropyl radicals with the mixed monomers styrene and acrylonitrile have been investigated using the nitroxide radical trapping technique. When the trap concentration is kept low, second, third, and even fourth generation (in terms of successive monomer addition) carbon radicals have been observed as trapped products. The ratio of rate constants for the addition of styrene and acrylonitrile to cyanoisopropyl radicals is 2.7 at 75°C and 5.3 at 105°C. These values are compared with the ratios for reactions of these two monomers with a number of other radicals and discussed in terms of the polarities of the radicals and monomers. © 1998 John Wiley & Sons, Inc. J. Polym. Sci. A Polym. Chem. 36: 2169-2176, 1998
    Zusätzliches Material: 1 Ill.
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  • 100
    Digitale Medien
    Digitale Medien
    Synthesis and characterization of new poly(amide-imide)s from 1,4-bis(4-trimellitimidophenoxy)-2-tert-butylbenzene with various diamines (1998)
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part A: Polymer Chemistry 36 (1998), S. 2301-2307 
    Details
    ISSN: 0887-624X
    Schlagwort(e): 1,4-bis(4-trimellitimidophenoxy)-2-tert-butylbenzene (BTTB) ; direct polycondensation ; poly(amide-imide)s ; Chemistry ; Polymer and Materials Science
    Quelle: Wiley InterScience Backfile Collection 1832-2000
    Thema: Chemie und Pharmazie
    Notizen: New poly(amide-imide)s were prepared from a diimide-dicarboxylic acid, 1,4-bis(4-trimellitimidophenoxy)-2-tert-butylbenzene (BTTB), with various diamines by the direct polycondensation in N-methyl-2-pyrrolidinone (NMP) using triphenyl phosphite and pyridine as condensing agents. The new diimide-dicarboxylic acid BTTB containing an ether linkage and tert-butyl substituent was synthesized by the condensation reaction of 1,4-bis(4-aminophenoxy)-2-tert-butylbenzene with trimellitic anhydride. All the polymers were obtained in quantitative yields with inherent viscosities of 0.62-1.06 dL g-1. The polymers were amorphous, and most of them were readily soluble in aprotic polar solvents such as NMP, N,N-dimethylacetamide (DMAc), and N,N-dimethylformamide (DMF), as well as in less polar solvents such as dimethyl sulfoxide (DMSO), m-cresol, pyridine, and γ-butyrolactone, and also even in tetrahydrofuran. The glass transition temperatures of the polymers were determined by DSC method, and they were in the range of 238-279°C. These polymers were stable up to 408-449°C in air and 451-483°C in nitrogen and lose 10% weight in the range of 479-525°C in air and 480-528°C in nitrogen atmosphere. The polymer films had a tensile strength range of 71-115 MPa, an elongation at break range of 4-14%, and a tensile modulus range of 2.3-3.1 GPa. © 1998 John Wiley & Sons, Inc. J. Polym. Sci. A Polym. Chem. 36: 2301-2307, 1998
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