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  • 1
    Electronic Resource
    Electronic Resource
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 33 (1995), S. 1995-2001 
    ISSN: 0887-6266
    Keywords: tussah silk fibroin ; methanol treatment ; molecular conformation ; crystallization ; Raman spectroscopy analysis ; Chemistry ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: Structural changes of tussah (Antheraea pernyi) silk fibroin films treated with different water-methanol solutions at 20°C were studied as a function of methanol concentration and immersion time. X-ray diffraction measurements showed that the α-helix structure, typical of untreated tussah films, did not change for short immersion times (2 min), regardless of methanol concentration. However, crystallization to β-sheet structure was observed following immersion of tussah films for 30 min in methanol solutions ranging from 20 to 60% (v/v). IR spectra of tussah films untreated and methanol treated for 2 min exhibited strong absorption bands at 1265, 892, and 622 cm-1, typical of the α-helix conformation. The intensity of the bands assigned to the β-sheet conformation (1245, 965, and 698 cm-1) increased for the sample treated with 40% methanol for 30 min. Raman spectra of tussah films with α-helix molecular conformation exhibited strong bands at 1657 (amide I), 1263 (amide III), 1106, 908, 530, and 376 cm-1. Following α → β conformational transition, amide I and III bands shifted to 1668, and to 1241, 1230 cm-1, respectively. The band at 1106 cm-1 disappeared and new bands appeared at 1095 and 1073 cm-1, whereas the intensity of the bands at 530 and 376 cm-1 decreased significantly. ©1995 John Wiley & Sons, Inc.
    Additional Material: 5 Ill.
    Type of Medium: Electronic Resource
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  • 2
    Electronic Resource
    Electronic Resource
    Bognor Regis [u.a.] : Wiley-Blackwell
    Journal of Polymer Science Part B: Polymer Physics 36 (1998), S. 2717-2724 
    ISSN: 0887-6266
    Keywords: tussah silk ; fibroin ; methanol treatment ; α-helix structure ; β-sheet structure ; dynamic mechanical analysis ; thermomechanical analysis ; Physics ; Polymer and Materials Science
    Source: Wiley InterScience Backfile Collection 1832-2000
    Topics: Chemistry and Pharmacology , Physics
    Notes: The thermal response of tussah (Antheraea pernyi) silk fibroin films treated with different water-methanol solutions at 20°C was studied by means of dynamic mechanical (DMA) and thermomechanical (TMA) analyses as a function of methanol concentration and treatment time. The DMA curves of α-helix films (treated with ≥80% v/v methanol for 2 min and 100% methanol for 30 min) showed the sharp fall of storage modulus at about 190°C, and the loss peak in the range 207-213°C. The TMA curves were characterized by a thermal shrinkage at 209-211°C, immediately followed by an abrupt extension leading to film failure. Both storage and loss modulus curves significantly shifted upwards for β-sheet films, obtained by treatment with ≤60% methanol for 30 min. The loss peak exhibited a maximum at 236°C. Accordingly, the TMA shrinkage at above 200°C disappeared. The films broke beyond 330°C, failure being preceded by a broad contraction step. Intermediate DMA and TMA patterns were observed for the other solvent-treated films. The loss peak shifted to higher temperature (219-220°C), and a minor loss modulus component appeared at about 230°C. This coincided with the onset of a plateau region in the storage modulus curve. The TMA extension-contraction events in the range 200-300°C weakened, and the samples displayed a final broad contraction (peak temperature 326-338°C) before breaking. The DMA and TMA response of these films was attributed to partial annealing by solvent treatment, which resulted in the formation of nuclei of β-sheet crystallization within the film matrix. The increased thermal stability was probably due to the small β-sheet crystals formed, which acted as high-strength junctions between adjacent random coil and α-helix domains. © 1998 John Wiley & Sons, Inc. J Polym Sci B: Polym Phys 36: 2717-2724, 1998
    Additional Material: 7 Ill.
    Type of Medium: Electronic Resource
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