Correlations of Apparent Cellulose Crystallinity Determined by XRD, NMR, IR, Raman, and SFG Methods

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• 关键词：X ; ray diffraction ; Sum frequency generation spectroscopy ; Infrared spectroscopy ; Raman spectroscopy ; Nuclear magnetic resonance ; Crystallinity index ; Wood pulp
• 刊名：Advances in Polymer Science
• 出版年：2016
• 出版时间：2016
• 年：2016
• 卷：271
• 期：1
• 页码：115-131
• 全文大小：480 KB
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• 作者单位：Christopher Lee (20)
  Kevin Dazen (20)
  Kabindra Kafle (20)
  Andrew Moore (21)
  David K. Johnson (22)
  Sunkyu Park (21)
  Seong H. Kim (20)
  
  20. Department of Chemical Engineering and Materials Research Institute, Pennsylvania State University, University Park, PA, 16802, USA
  21. Department of Forest Biomaterials, North Carolina State University, Raleigh, NC, 27695, USA
  22. National Renewable Energy Laboratory, 15013 Denver West Parkway, Golden, CO, 80401, USA
  
• 丛书名：Cellulose Chemistry and Properties: Fibers, Nanocelluloses and Advanced Materials
• ISBN：978-3-319-26015-0
• 刊物类别：Chemistry and Materials Science
• 刊物主题：Chemistry
  Polymer Sciences
  
• 出版者：Springer Berlin / Heidelberg
• ISSN：1436-5030

文摘

Although the cellulose crystallinity index (CI) is used widely, its limitations have not been adequately described. In this study, the CI values of a set of reference samples were determined from X-ray diffraction (XRD), nuclear magnetic resonance (NMR), and infrared (IR), Raman, and vibrational sum frequency generation (SFG) spectroscopies. The intensities of certain crystalline peaks in IR, Raman, and SFG spectra positively correlated with the amount of crystalline cellulose in the sample, but the correlation with XRD was nonlinear as a result of fundamental differences in detection sensitivity to crystalline cellulose and improper baseline corrections for amorphous contributions. It is demonstrated that the intensity and shape of the XRD signal is affected by both the amount of crystalline cellulose and crystal size, which makes XRD analysis complicated. It is clear that the methods investigated show the same qualitative trends for samples, but the absolute CI values differ depending on the determination method. This clearly indicates that the CI, as estimated by different methods, is not an absolute value and that for a given set of samples the CI values can be compared only as a qualitative measure.