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Microstructure elucidation of historic silk (Bombyx mori) by nuclear magnetic resonance

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Abstract

1H NMR cryoporometry and solid-state 13C cross-polarization (CP) magic-angle spinning (MAS) NMR spectroscopy were used to characterize the microstructure of historic and fresh silk samples. Silk is a polymeric bicomponent material composed of fibroin and water located in micropores. According to the 1H NMR cryoporometry method, the intensity of the water resonance as a function of the temperature was used to obtain the pore size distribution, which was strongly asymmetric with a well-defined maximum at 1.1 nm. Compared with the fresh silk samples, the volume of pores around 1.1 nm decreased distinctly in the historic silk, and more pores larger than 2 nm emerged accordingly. In addition, these results correlated well with solid-state 13C CP/MAS NMR spectroscopy as the percentage of random coil in the historic silk sample was much less than that in the fresh silk samples. Therefore, it is suggested that the water-filled microvoids grow larger as the random coil conformation fades away in the degradation process.

We elucidate that compared with fresh silk, the water filled micropores within historic silk grow larger as the random coil conformation fade away in the degradation process

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Authors and Affiliations

  1. Department of History of Science and Scientific Archaeology, University of Science and Technology of China, Hefei, China

    Zhanyun Zhu, Decai Gong & Liu Liu

  2. Basic Research Center of Conservation Science, University of Science and Technology of China, Hefei, China

    Zhanyun Zhu, Decai Gong & Liu Liu

  3. Hefei National Laboratory for Physical Sciences at the Microscale, University of Science and Technology of China, Hefei, China

    Yusong Wang

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  1. Zhanyun Zhu
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  2. Decai Gong
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  3. Liu Liu
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  4. Yusong Wang
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Correspondence to Decai Gong.

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Zhu, Z., Gong, D., Liu, L. et al. Microstructure elucidation of historic silk (Bombyx mori) by nuclear magnetic resonance. Anal Bioanal Chem 406, 2709–2718 (2014). https://doi.org/10.1007/s00216-014-7660-8

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  • DOI: https://doi.org/10.1007/s00216-014-7660-8

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