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Cellulose

, Volume 23, Issue 2, pp 1073–1086 | Cite as

Comparison of sample crystallinity determination methods by X-ray diffraction for challenging cellulose I materials

  • Patrik Ahvenainen
  • Inkeri Kontro
  • Kirsi Svedström
Original Paper

Abstract

Cellulose crystallinity assessment is important for optimizing the yield of cellulose products, such as bioethanol. X-ray diffraction is often used for this purpose for its perceived robustness and availability. In this work, the five most common analysis methods (the Segal peak height method and those based on peak fitting and/or amorphous standards) are critically reviewed and compared to two-dimensional Rietveld refinement. A larger (\(n=16\)) and more varied collection of samples than previous studies have presented is used. In particular, samples (\(n=6\)) with low crystallinity and small crystallite sizes are included. A good linear correlation (\(r^{2} \ge 0.90\)) between the five most common methods suggests that they agree on large-scale crystallinity differences between samples. For small crystallinity differences, however, correlation was not seen for samples that were from distinct sample sets. The least-squares fitting using an amorphous standard shows the smallest crystallite size dependence and this method combined with perpendicular transmission geometry also yielded values closest to independently obtained cellulose crystallinity values. On the other hand, these values are too low according to the Rietveld refinement. All analysis methods have weaknesses that should be considered when assessing differences in sample crystallinity.

Keywords

Cellulose Crystallinity X-ray diffraction  Wide-angle X-ray scattering 

Notes

Acknowledgments

P.A. has received funding from the Finnish National Doctoral Program in Nanoscience. We would like to thank Dr. Seppo Andersson and Dr. Paavo Penttilä for providing some of the used X-ray diffraction data, and Dr. Carlos Eduardo Driemeier for giving access to the CRAFS package source code. We would also like to thank professor Ritva Serimaa for fruitful discussions on cellulose crystallinity and for motivating us to carry out this study.

Compliance with ethical standards

Conflicts of interest

The authors declare that they have no conflict of interest.

Supplementary material

10570_2016_881_MOESM1_ESM.pdf (129 kb)
Supplementary material 1 (pdf 128 KB)
10570_2016_881_MOESM2_ESM.zip (9 kb)
Supplementary material 2 (zip 9 KB)

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Copyright information

© Springer Science+Business Media Dordrecht 2016

Authors and Affiliations

  1. 1.Department of PhysicsUniversity of HelsinkiHelsinkiFinland

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