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

Content Provider	Springer Nature Link
Author	Ahvenainen, Patrik Kontro, Inkeri Svedström, Kirsi
Copyright Year	2016
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.
Starting Page	1073
Ending Page	1086
Page Count	14
File Format	PDF
ISSN	09690239
Journal	Cellulose
Volume Number	23
Issue Number	2
e-ISSN	1572882X
Language	English
Publisher	Springer Netherlands
Publisher Date	2016-02-17
Publisher Place	Dordrecht
Access Restriction	One Nation One Subscription (ONOS)
Subject Keyword	Cellulose Crystallinity X-ray diffraction Wide-angle X-ray scattering Bioorganic Chemistry Physical Chemistry Organic Chemistry Polymer Sciences
Content Type	Text
Resource Type	Article
Subject	Polymers and Plastics

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