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  • 1
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 129 (1985), S. 95-101 
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Die Spin-Gitter(T1)- und Spin-Spin(T2)-Relaxationen der Protonen in isotaktischen Polypropylenfilmen verschiedener thermischer Vorgeschichte und nach Behandlung mit Tetrachlorethylen wurden mit gepulster NMR gemessen. Bei der aus der Schmelze abgeschreckten Probe wächst T1l (die längere T1) und sinkt T2a (die längste T2) mit steigender Temperatur der Wärmevorbehandlung. Mit steigender Temperatur nimmt die Massenfraktion der mobilen Region (Fa) ab und die Massenfraktion der starren Region (Fc) zu. Das fast lineare Wachstum von T1l mit steigendem Fc zeigt, daß vor allem die Rückbildung der mobilen amorphen Region für die Änderung von T1l verantwortlich ist.Bei der getemperten Probe wächst T1l ebenfalls mit steigender Temperatur der Wärmevorbehandlung, obwohl eine leichte Abnahme von T1l bei niederen Temperaturen beobachtet wird. Die starke Abnahme von T2a bei Erhöhung der Temperatur der Wärmevorbehandlung gibt Anlaß zu der Annahme, daß bei der getemperten Probe eine vergleichsweise selektive Extraktion stattfindet.
    Notes: Proton spin-lattice (T1) and spin-spin (T2) relaxation times of isotactic polypropylene films with different thermal histories, treated with tetrachloroethylene, were measured with pulsed NMR. For the melt-quenched sample T11 (the longer T1) increases and T2a (the longest T2) decreases with increasing treatment temperature. The mass fraction of mobile region (Fa) decreases and the mass fraction of rigid region (Fc) increases with increasing treatment temperature. T11 increases almost linearly with increasing Fc, indicating that the removal of the mobile amorphous region is mainly responsible for the change in T11.For the annealed sample T11 also increases with increasing treatment temperature, although a slight decrease in T11 for the low treatment temperature is observed. There is a large decrease in T2a when the treatment temperature is raised, suggesting that a comparatively selective extraction occurs for the annealed sample.
    Additional Material: 4 Ill.
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  • 2
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 113 (1983), S. 31-42 
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Ein isotaktischer Polypropylenfilm wurde mit Cyclohexan, Toluol, 1-Chlornaphthalin und Glyzerin behandelt. Die Änderung der Morphologie wurde durch Messung des Gewichtsverlusts, der Dichte, des Molekulargewichts, der Spin-Gitter- und der Spin-Spin-Relaxationszeiten bestimmt. Es gibt einen relativ engen Temperaturbereich, in dem eine starke Zunahme des Gewichtsverlusts beobachtet wird, die von der Art des Lösungsmittels abhängt. Die Dichteänderung hängt für alle Lösungsmittel linear von der Behandlungsdauer ab. Das Molekulargewicht steigt ebenfalls mit steigendem Gewichtsverlust. Die Zunahme von T1 mit steigender Temperatur ist beachtlich. T2 des amorphen Bereichs (T2a) steigt ebenfalls, wenn die Temperatur erhöht wird, es wird jedoch eine gewisse Abnahme von T2a an den mit Toluol und Cyclohexan bei höherer Temperatur behandelten Proben gefunden. Der Anteil des starren Bereichs (Tc) steigt an und der des mobilen Bereichs sinkt ab mit zunehmender Lösungsextraktion. Der Wert für Tc ist recht verschieden von dem kristallinen Anteil, der aus der Dichte am Beginn der Behandlung berechnet wird, gefolgt von einer allmählichen Annäherung an den Wert, der aus der Dichte errechnet wird, wobei jedoch bei den mit Cyclohexan behandelten Proben ein etwas anderes Verhalten gefunden wurde.
    Notes: An isotactic polypropylene film was treated with cyclohexane, toluene, 1-chloronaphthalene, and glycerin. The morphological changes were characterized by measurements of weight loss, density, molecular weight, and spin-lattice and spin-spin relaxation times. There is a relatively narrow temperature range at which a sharp increase in weight loss occurs corresponding to the kind of the solvent. The change in density occurs almost linearly with treatment time for all solvents. Molecular weight also increases as the weight loss is increased. There is a considerable increase in T1 with increasing treatment temperature. T2 of the amorphous region, T2a, also increases as the treatment temperature is increased, but some decrease in T2a is found in the samples treated with toluene and cyclohexane at higher temperatures. The fraction of the rigid region, Fc, increases and that of the mobile one, Fa, decreases with proceeding solvent extraction. The value of Fc is considerably different from the crystallinity calculated from the density in the early stage of the treatment followed by the gradual approach to the value calculated from the density, although some different behaviour was found with the samples treated with cyclohexane.
    Additional Material: 7 Ill.
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  • 3
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Die Stuktu von bei hoher Temperatur mit Tetrachlorethylen behandelten Filmen aus isotaktischem Polypropylen wurde durch die Bestimmung von Protonen-Spin-Gitter- (T1) und Spin-Spin-Relaxationszeiten (T2), Gewichsverlust, Kristallinität, Molmasse, Schmelztemperatur und Schmelzwärme charakterisiert. Zwei Arten von Proben, eine abgeschreck, eine getempert, wurden verwendet. Durch die Lösungsmittelbehandlung bei hoher Temperatur trat insbesondere bei der abgeschreckten Probe ein erheblicher Gewichtsverlust und ein Anstieg des Molekulargewichts und der Kristallinität auf. Diese morphologischen Veränderungen führten zu einer Verschiebung des T1-Minimums zu höheren Temperaturen und zu einer Abnahme von T2a. Die Wirkungen des Lösungsmittels auf die getemperte Probe waren qualitativ gleichartig, aber relativ schwach.
    Notes: The structural properties of isotactic polypropylene films treated with tetrachloroethylene at high temperatures were characterized by proton spin-lattice T1 and spin-spin T2 relaxation times, loss in weight, crystallinity, molecular weight, and melting temperature, and heat of fusion. Two kinds of samples, a quenched and an annealed sample, were employed. There are a considerable loss in weight and large increases in crystallinity and in molecular weight when treated the sample at high temperatures especially in the quenched one. These morphological changes result in a shift of T1 minimum to high temperatures and a decrease in T2a. The effects of the solvent on the annealed sample are qualitatively the same for the quenched one but are relatively mild.
    Additional Material: 12 Ill.
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  • 4
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Angewandte Makromolekulare Chemie 175 (1990), S. 29-38 
    ISSN: 0003-3146
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Description / Table of Contents: Die Temperatur des T1-Minimums für die Segmentbewegung in Polypropylen, das einen hohen ataktischen Anteil besitzt, ist niedriger als die in isotaktischem Polypropylen. Ein kurzes T1, T1s, tritt bei beiden Materialien auf. Bei Temperaturerhöhung nimmt T2a (T2 der beweglichen amorphen Bezirke) stark und T2m (T2 der dazwischen liegenden Bezirke) leicht zu, während sich T2c (T2 der steifen kristallinen Bezirke) kaum ändert. T2a in Polypropylen mit hohem ataktischem Anteil ist länger als in isotaktischem Polypropylen.Der Massenbruch der kristallinen Bezirke, Fc, nimmt bei Temperaturerhöhung ab und der der amorphen Bezirke, Fa, zu. Die Relaxationsgeschwindigkeit, 1/ (T1min), steigt linear mit Zunahme des amorphen Anteils an, außer bei der mit siedendem n-Heptan extrahierten Probe. Mit Zunahme der Peaktemperatur von tan δ fällt T2a nahezu linear ab, während die Temperatur des T1-Minimums zunimmt.
    Notes: The temperature of the T1 minimum for the segmental motion in polypropylene containing a lot of atactic fraction is lower than that in isotactic polypropylene. A short T1, T1s, appears for both materials. As the temperature is raised, there is a large increase in T2a (T2 of the mobile amorphous regions), and a mild increase in T2m (T2 of the intermediate regions), while there is no substantial change in T2c (T2 of the rigid crystalline regions). T2a in polypropylene containing a lot of atactic fraction is longer than that in isotactic polypropylene.The mass fraction of crystalline regions, Fc, decreases and that of the amorphous regions, Fa, increases as the temperature is raised. There is a linear increase in the relaxation rate, 1/(T1min), as the amorphous fraction is increased, except for the sample extracted with boiling n-heptane. With increase of the peak temperature of tanδ, T2a decreases nearly linearly, while the temperature of the T1 minimum increases.
    Additional Material: 7 Ill.
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  • 5
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 99 (1966), S. 3215-3217 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Notes: Ausgehend von α-Furyllithium werden Derivate des Furan-thiols-(2) (8) und -selenols-(2) (9) dargestellt. Freies 8 und 9 sind nur in alkalisch-wäßrigem Medium stabil.
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  • 6
    Electronic Resource
    Electronic Resource
    Weinheim : Wiley-Blackwell
    Berichte der deutschen chemischen Gesellschaft 99 (1966), S. 3932-3933 
    ISSN: 0009-2940
    Keywords: Chemistry ; Inorganic Chemistry
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Type of Medium: Electronic Resource
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  • 7
    Electronic Resource
    Electronic Resource
    Basel : Wiley-Blackwell
    Die Makromolekulare Chemie, Rapid Communications 12 (1991), S. 307-312 
    ISSN: 0173-2803
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Additional Material: 5 Ill.
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  • 8
    Electronic Resource
    Electronic Resource
    New York : Wiley-Blackwell
    Journal of Polymer Science: Polymer Letters Edition 15 (1977), S. 349-362 
    ISSN: 0360-6384
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology
    Additional Material: 12 Ill.
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  • 9
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Spin-lattice relaxation time T1 and spin-spin relaxation time T2 were measured at 40°C on the isotactic polypropylene films of varying preparations and thermal history. T1 increases with increasing crystallinity and two T1's appear for the samples annealed at elevated temperatures (〉120°C). These variations in T1 are well interpreted in terms of the spin diffusion and decoupling of the mobile protons with immobile ones. A free induction decay following a 90° pulse is the superposition of three different decay curves, one of which is exponential and other two are nonexponential. There is an increase in T2a with increasing crystallinity, which is indicative of the enhancement of the chain mobility in the amorphous region. There are differences between the crystallinity calculated from density and the fraction of crystalline region, Fc, obtained by the NMR method, which can be explained by the existence of the microparacrystals and the stress imposed on the amorphous chains on rapid cooling. On the other hand, there is a gradual lowering in T1 and a considerable increase in T2a as an atactic fraction is increased. The increase in atactic fraction also results in a decrease in the amount of the isotactic amorphous chains in the amorphous region.
    Additional Material: 9 Ill.
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  • 10
    ISSN: 0021-8995
    Keywords: Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Mechanical Engineering, Materials Science, Production Engineering, Mining and Metallurgy, Traffic Engineering, Precision Mechanics , Physics
    Notes: Proton spin-lattice, T1, and spin-spin, T2, relaxation times of uniaxially stretched polypropylene film were measured at 40°C using a wide line pulse spectrometer operating at 19.8 MHz. T1l, the longer T1, increases almost linearly with increasing stretching ratio, and T2a, T2 of the amorphous region, decreases gradually as the stretching ratio is increased. These results can be interpreted in terms of the increased constraints to molecular motion in the amorphous region. The fraction of the rigid protons in the sample, Fc, increases with increasing stretching ratio, while the crystallinity calculated from the density, Xd, does not change largely. The difference between Fc and Xd, therefore, increases as the stretching ratio is increased. This indicates that the physical structure of the highly stretched sample is far from the ideal two-phase model. The influence of the stretching temperature was also investigated. There are only slight increases in T1l and in Fc for the samples stretched in a temperature range from 80°C to 150°C, whereas the considerable increase in T2a occurs. The most notable change introduced at a high temperature stretching is the increase in the chain mobility in the amorphous region.
    Additional Material: 7 Ill.
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