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Cellulose

, Volume 21, Issue 2, pp 885–896 | Cite as

Idealized powder diffraction patterns for cellulose polymorphs

  • Alfred D. FrenchEmail author
Original Paper

Abstract

Cellulose samples are routinely analyzed by X-ray diffraction to determine their crystal type (polymorph) and crystallinity. However, the connection is seldom made between those efforts and the crystal structures of cellulose that have been proposed with synchrotron X-radiation and neutron diffraction over the past decade or so. In part, this desirable connection is thwarted by the use of different conventions for description of the unit cells of the crystal structures. In the present work, powder diffraction patterns from cellulose Iα, Iβ, II, IIII, and IIIII were calculated based on the published atomic coordinates and unit cell dimensions contained in modified “crystal information files” (.cif) that are supplied in the Supplementary Information. The calculations used peak widths at half maximum height of both 0.1 and 1.5° 2θ, providing both highly resolved indications of the contributions of each contributing reflection to the observable diffraction peaks as well as intensity profiles that more closely resemble those from practical cellulose samples. Miller indices are shown for each contributing peak that conform to the convention with c as the fiber axis, a right-handed relationship among the axes and the length of a < b. Adoption of this convention, already used for crystal structure determinations, is also urged for routine studies of polymorph and crystallinity. The calculated patterns are shown with and without preferred orientation along the fiber axis. Diffraction intensities, output by the Mercury program from the Cambridge Crystallographic Data Centre, have several uses including comparisons with experimental data. Calculated intensities from different polymorphs can be added in varying proportions using a spreadsheet program to simulate patterns such as those from partially mercerized cellulose or various composites.

Keywords

Cellulose crystal structure Miller indices Powder diffraction patterns Convention 

Notes

Acknowledgments

Paul Langan kindly provided the .cif file for cellulose II. The research was partly inspired by collaborative efforts with Cotton, Incorporated. Drs. Santiago Cintrón, Seong Kim and Xueming Zhang kindly commented on preliminary versions of the manuscript. Dr. Edwin Stevens consulted on the effects of preferred orientation on the cellulose Iα pattern.

Supplementary material

10570_2013_30_MOESM1_ESM.docx (28 kb)
Supplementary material 1 (DOCX 27 kb)

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Copyright information

© Springer Science+Business Media Dordrecht (outside the USA)  2013

Authors and Affiliations

  1. 1.U.S. Department of AgricultureSouthern Regional Research CenterNew OrleansUSA

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