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

  • Christopher Lee
  • Kevin Dazen
  • Kabindra Kafle
  • Andrew Moore
  • David K. Johnson
  • Sunkyu Park
  • Seong H. Kim
Chapter
Part of the Advances in Polymer Science book series (POLYMER, volume 271)

Abstract

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.

Keywords

X-ray diffraction Sum frequency generation spectroscopy Infrared spectroscopy Raman spectroscopy Nuclear magnetic resonance Crystallinity index Wood pulp 

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Copyright information

© Springer International Publishing Switzerland 2015

Authors and Affiliations

  • Christopher Lee
    • 1
  • Kevin Dazen
    • 1
  • Kabindra Kafle
    • 1
  • Andrew Moore
    • 2
  • David K. Johnson
    • 3
  • Sunkyu Park
    • 2
  • Seong H. Kim
    • 1
  1. 1.Department of Chemical Engineering and Materials Research InstitutePennsylvania State UniversityUniversity ParkUSA
  2. 2.Department of Forest BiomaterialsNorth Carolina State UniversityRaleighUSA
  3. 3.National Renewable Energy LaboratoryGoldenUSA

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