Cellulose

, Volume 21, Issue 6, pp 3951–3963 | Cite as

Structure characterization of native cellulose during dehydration and rehydration

Original Paper

Abstract

The goal of this study is to investigate the hydration and dehydration induced structural changes of native cellulose. Never dried cotton, and never dried bacterial cellulose with and without added matrix polymer xyloglucan, are examined under the influence of dehydration and rehydration. Significant crystal structure changes were observed in the later stage of drying for both cotton and bacterial cellulose (BC). The 1 % lateral expansion in glucan chain spacing and 17 % decrease of calculated Scherrer dimension were detected for cotton due to the distortion of the structure possibly caused by mechanical stresses associated with drying. No detectable changes on average glucan chain spacings were observed for large BC crystals. However, an average width decrease by 4.4 nm was discovered in the (010) direction, which was more significant than that observed in the (100) and (110) directions. It is hypothesized that co-crystallized elementary fibrils preferentially disassociate along the (010) plane resulting in a significant reduction of crystal width. In the BC-xyloglucan model composite, the presence of xyloglucan does not interfere with the dehydration behavior. Rehydration leads to some structural changes but to a lesser extent than the initial drying. High temperature dehydration induced deformation and crystal size changes are found to be non-reversible due to the removal of the last hydration layer on the cellulose surface.

Keywords

Cellulose Bound water X-ray diffraction Dehydration Crystal structure Co-crystallization 

Supplementary material

10570_2014_435_MOESM1_ESM.doc (2.4 mb)
Supplementary material 1 (DOC 2475 kb)

References

  1. Abe K, Yamamoto H (2005) Mechanical interaction between cellulose microfibril and matrix substance in wood cell wall determined by X-ray diffraction. J Wood Sci 51:334–338CrossRefGoogle Scholar
  2. Abe K, Yamamoto H (2006) Change in mechanical interaction between cellulose microfibril and matrix substance in wood cell wall induced by hygrothermal treatment. J Wood Sci 52:107–110CrossRefGoogle Scholar
  3. Astley OM, Chanliaud E, Donald AM, Gidley MJ (2001) Structure of Acetobacter cellulose composites in the hydrated state. Int J Biol Macromol 29:193–202. doi:10.1016/s0141-8130(01)00167-2 CrossRefGoogle Scholar
  4. Atalla RH, Hackney JM, Uhlin I, Thompson NS (1993) Hemicelluloses as structure regulators in the aggregation of native cellulose. Int J Biol Macromol 15:109–112. doi:10.1016/0141-8130(93)90007-9 CrossRefGoogle Scholar
  5. Avci U, Pattathil S, Singh B, Brown VL, Hahn MG, Haigler CH (2013) Cotton fiber cell walls of Gossypium hirsutum and Gossypium barbadense have differences related to loosely-bound xyloglucan. PLoS One 8:e56315CrossRefGoogle Scholar
  6. Bootten TJ, Harris PJ, Melton LD, Newman RH (2008) WAXS and 13C NMR study of Gluconoacetobacter xylinus cellulose in composites with tamarind xyloglucan. Carbohydr Res 343:221–229CrossRefGoogle Scholar
  7. Brown Jr RM (1990) Microbial cellulose modified during synthesis. US Patent 4942128Google Scholar
  8. Carles J, Scallan AM (1973) The determination of the amount of bound water within cellulosic gels by NMR spectroscopy. J Appl Polym Sci 17:1855–1865CrossRefGoogle Scholar
  9. Chanliaud E, Burrows KM, Jeronimidis G, Gidley MJ (2002) Mechanical properties of primary plant cell wall analogues. Planta 215:989–996CrossRefGoogle Scholar
  10. Cousins SK, Brown RM Jr (1995) Cellulose I microfibril assembly: computational molecular mechanics energy analysis favours bonding by van der Waals forces as the initial step in crystallization. Polymer 36:3885–3888CrossRefGoogle Scholar
  11. Czaja W, Krystynowicz A, Bielecki S, Brown RM Jr (2006) Microbial cellulose—the natural power to heal wounds. Biomaterials 27:145–151CrossRefGoogle Scholar
  12. Davidson TC, Newman RH, Ryan MJ (2004) Variations in the fibre repeat between samples of cellulose I from different sources. Carbohydr Res 339:2889–2893CrossRefGoogle Scholar
  13. Debzi E, Chanzy H, Sugiyama J, Tekely P, Excoffier G (1991) The Iα → Iβ transformation of highly crystalline cellulose by annealing in various mediums. Macromolecules 24:6816–6822CrossRefGoogle Scholar
  14. Diddens I, Murphy B, Krisch M, Müller M (2008) Anisotropic elastic properties of cellulose measured using inelastic X-ray scattering. Macromolecules 41:9755–9759CrossRefGoogle Scholar
  15. Driemeier C, Bragatto J (2012) Crystallite width determines monolayer hydration across a wide spectrum of celluloses isolated from plants. J Phys Chem B 117:415–421CrossRefGoogle Scholar
  16. Fang L, Catchmark JM (2011) Characterization of exopolysaccharides from certain strains of Gluconacetobacter xylinus ASABE Annual Meeting. KY, LouisvilleGoogle Scholar
  17. Fang L, Catchmark JM (2014) Characterization of water-soluble exopolysaccharides from Gluconacetobacter xylinus and their impacts on bacterial cellulose crystallization and ribbon assembly. Cellulose. doi:10.1007/s10570-014-0443-8
  18. Fink H-P, Hofmann D, Philipp B (1995) Some aspects of lateral chain order in cellulosics from X-ray scattering. Cellulose 2:51–70Google Scholar
  19. Fink HP, Purz HJ, Bohn A, Kunze J (1997) Investigation of the supramolecular structure of never dried bacterial cellulose. J Macromol Symp 120:207–217CrossRefGoogle Scholar
  20. Gu J, Catchmark JM (2012) Impact of hemicelluloses and pectin on sphere-like bacterial cellulose assembly. Carbohydr Polym 88:547–557CrossRefGoogle Scholar
  21. Hackney JM, Atalla RH, VanderHart DL (1994) Modification of crystallinity and crystalline structure of Acetobacter xylinum cellulose in the presence of water-soluble β-1,4-linked polysaccharides: 13C-NMR evidence. Int J Biol Macromol 16:215–218. doi:10.1016/0141-8130(94)90053-1 CrossRefGoogle Scholar
  22. Haigler C, Brown R, Benziman M (1980) Calcofluor white ST alters the in vivo assembly of cellulose microfibrils. Science 210:903–906. doi:10.1126/science.7434003 CrossRefGoogle Scholar
  23. Haigler CH, White AR, Brown RM, Cooper KM (1982) Alteration of in vivo cellulose ribbon assembly by carboxymethylcellulose and other cellulose derivatives. J Cell Biol 94:64–69. doi:10.1083/jcb.94.1.64 CrossRefGoogle Scholar
  24. Haigler CH, Betancur L, Stiff MR, Tuttle JR (2012) Cotton fiber: a powerful single-cell model for cell wall and cellulose research. Front Plant Sci 3:104CrossRefGoogle Scholar
  25. Hanus J, Mazeau K (2006) The xyloglucan–cellulose assembly at the atomic scale. Biopolymers 82:59–73. doi:10.1002/bip.20460 CrossRefGoogle Scholar
  26. Heiner AP, Teleman O (1997) Interface between monoclinic crystalline cellulose and water: breakdown of the odd/even duplicity. Langmuir 13:511–518CrossRefGoogle Scholar
  27. Heiner AP, Kuutti L, Teleman O (1998) Comparison of the interface between water and four surfaces of native crystalline cellulose by molecular dynamics simulations. Carbohydr Res 306:205–220CrossRefGoogle Scholar
  28. Hestrin S, Schramm M (1954) Synthesis of cellulose by Acetobacter xylinum. 2. Preparation of freeze-dried cells capable of polymerizing glucose to cellulose. Biochem J 58:345Google Scholar
  29. Hill SJ, Kirby NM, Mudie ST, Hawley AM, Ingham B, Franich RA, Newman RH (2010) Effect of drying and rewetting of wood on cellulose molecular packing. Holzforschung 64:421–427Google Scholar
  30. Horii F, Hirai A, Kitamaru R (1987) CP/MAS carbon-13 NMR spectra of the crystalline components of native celluloses. Macromolecules 20:2117–2120CrossRefGoogle Scholar
  31. Horikawa Y, Sugiyama J (2008) Accessibility and size of Valonia cellulose microfibril studied by combined deuteration/rehydrogenation and FTIR technique. Cellulose 15:419–424CrossRefGoogle Scholar
  32. Horikawa Y, Sugiyama J (2009) Localization of crystalline allomorphs in cellulose microfibril. Biomacromolecules 10:2235–2239. doi:10.1021/bm900413k CrossRefGoogle Scholar
  33. Hsieh Y-L, Hu X-P, Wang A (2000) Single fiber strength variations of developing cotton fibers—strength and structure of G. hirsutum and G. barbedense. Text Res J 70:682–690CrossRefGoogle Scholar
  34. Hu X-P, Hsieh Y-L (2001) Effects of dehydration on the crystalline structure and strength of developing cotton fibers. Text Res J 71:231–239CrossRefGoogle Scholar
  35. Huwyler H, Franz G, Meier H (1979) Changes in the composition of cotton fibre cell walls during development. Planta 146:635–642CrossRefGoogle Scholar
  36. Ishida T, Sugano Y, Nakai T, Shoda M (2002) Effects of acetan on production of bacterial cellulose by acetobacter xylinum biosci. Biotechnol Biochem 66:1677–1681. doi:10.1271/bbb.66.1677 CrossRefGoogle Scholar
  37. Jarvis MC (2011) Plant cell walls: supramolecular assemblies. Food Hydrocoll 25:257–262CrossRefGoogle Scholar
  38. Jayme G, Rothamel L (1948) Development of a standard centrifugal method for determining the swelling values of pulps. Papier Bingen Ger 2:7–18Google Scholar
  39. Kennedy CJ, Cameron GJ, Šturcová A, Apperley DC, Altaner C, Wess TJ, Jarvis MC (2007) Microfibril diameter in celery collenchyma cellulose: X-ray scattering and NMR evidence. Cellulose 14:235–246CrossRefGoogle Scholar
  40. Klemm D, Schumann D, Udhardt U, Marsch S (2001) Bacterial synthesized cellulose—artificial blood vessels for microsurgery. Prog Polym Sci 26:1561–1603CrossRefGoogle Scholar
  41. Kocherbitov V, Ulvenlund S, Kober M, Jarring K, Arnebrant T (2008) Hydration of microcrystalline cellulose and milled cellulose studied by sorption calorimetry. J Phys Chem B 112:3728–3734CrossRefGoogle Scholar
  42. Larsson PT, Wickholm K, Iversen T (1997) A CP/MAS 13C NMR investigation of molecular ordering in celluloses. Carbohydr Res 302:19–25CrossRefGoogle Scholar
  43. Liu Y, Gamble G, Thibodeaux D (2010) Two-dimensional attenuated total reflection infrared correlation spectroscopy study of the desorption process of water-soaked cotton fibers. Appl Spectrosc 64:1355–1363CrossRefGoogle Scholar
  44. Manjunath B, Venkataraman A, Stephen T (1973) The effect of moisture present in polymers on their X-ray diffraction patterns. J Appl Polym Sci 17:1091–1099CrossRefGoogle Scholar
  45. Maréchal Y, Chanzy H (2000) The hydrogen bond network in Iβ cellulose as observed by infrared spectrometry. J Mol Struct 523:183–196CrossRefGoogle Scholar
  46. Matthews JF et al (2006) Computer simulation studies of microcrystalline cellulose Iβ. Carbohydr Res 341:138–152. doi:10.1016/j.carres.2005.09.028 CrossRefGoogle Scholar
  47. Nakamura K, Hatakeyama T, Hatakeyama H (1981) Studies on bound water of cellulose by differential scanning calorimetry. Text Res J 51:607–613CrossRefGoogle Scholar
  48. Newman RH, Davidson TC (2004) Molecular conformations at the cellulose–water interface. Cellulose 11:23–32CrossRefGoogle Scholar
  49. Nieduszynski I, Preston R (1970) Crystallite size in natural cellulose Nature: 273–274Google Scholar
  50. Nishiyama Y (2009) Structure and properties of the cellulose microfibril. J Wood Sci 55:241–249CrossRefGoogle Scholar
  51. Ogiwara Y, Kubota H, Hayashi S, Mitomo N (1970) Temperature dependency of bound water of cellulose studied by a high-resolution NMR spectrometer. J Appl Polym Sci 14:303–309CrossRefGoogle Scholar
  52. Park YB, Cosgrove DJ (2012) A revised architecture of primary cell walls based on biomechanical changes induced by substrate-specific endoglucanases. Plant Physiol 158:1933–1943CrossRefGoogle Scholar
  53. Park S, Venditti RA, Jameel H, Pawlak JJ (2006a) Changes in pore size distribution during the drying of cellulose fibers as measured by differential scanning calorimetry. Carbohydr Polym 66:97–103CrossRefGoogle Scholar
  54. Park S, Venditti RA, Jameel H, Pawlak JJ (2006b) Hard to remove water in cellulose fibers characterized by high resolution thermogravimetric analysis-methods development. Cellulose 13:23–30CrossRefGoogle Scholar
  55. Peng Y, Gardner DJ, Han Y, Kiziltas A, Cai Z, Tshabalala MA (2013) Influence of drying method on the material properties of nanocellulose I: thermostability and crystallinity. Cellulose 20:2379–2392CrossRefGoogle Scholar
  56. Rowland SP (1977) Cellulose: pores, internal surfaces, and the water interface. In: textile and paper chemistry and technology. American Chemical Society, pp 20–45Google Scholar
  57. Schlünder E-U (2004) Drying of porous material during the constant and the falling rate period: a critical review of existing hypotheses. Drying Technol 22:1517–1532CrossRefGoogle Scholar
  58. Seifert M, Hesse S, Kabrelian V, Klemm D (2004) Controlling the water content of never dried and reswollen bacterial cellulose by the addition of water-soluble polymers to the culture medium. J Polym Sci Part A: Polym Chem 42:463–470CrossRefGoogle Scholar
  59. Singh B et al (2009) A specialized outer layer of the primary cell wall joins elongating cotton fibers into tissue-like bundles. Plant Physiol 150:684–699CrossRefGoogle Scholar
  60. Sluiter A, Hames B, Ruiz R, Scarlata C, Sluiter J, Templeton D, Crocker D (2008) Determination of structural carbohydrates and lignin in biomass. Laboratory Analytical Procedure National Renewable Energy Laboratory, Golden COGoogle Scholar
  61. Somerville C (2006) Cellulose synthesis in higher plants. Annu Rev Cell Dev Biol 22:53–78CrossRefGoogle Scholar
  62. Sugiyama J, Vuong R, Chanzy H (1991) Electron diffraction study on the two crystalline phases occurring in native cellulose from an algal cell wall. Macromolecules 24:4168–4175. doi:10.1021/ma00014a033 CrossRefGoogle Scholar
  63. Toba K, Yamamoto H, Yoshida M (2012) Mechanical interaction between cellulose microfibrils and matrix substances in wood cell walls induced by repeated wet-and-dry treatment. Cellulose 19:1405–1412CrossRefGoogle Scholar
  64. Uhlin KI, Atalla RH, Thompson NS (1995) Influence of hemicelluloses on the aggregation patterns of bacterial cellulose. Cellulose 2:129–144CrossRefGoogle Scholar
  65. Valla S, Ertesvåg H, Tonouchi N, Fjærvik E (2009) Bacterial cellulose production: biosynthesis and applications. In: Rehm B (ed) Microbial production of biopolymers and polymer precursors: applications and perspectives. Caister Academic Press, Norfolk, pp 43–77Google Scholar
  66. Wada M, Okano T, Sugiyama J (1997) Synchrotron-radiated X-ray and neutron diffraction study of native cellulose. Cellulose 4:221–232CrossRefGoogle Scholar
  67. Watanabe K (1998) Structural features and properties of bacterial cellulose produced in agitated culture. Cellulose 5:187–200. doi:10.1023/a:1009272904582 CrossRefGoogle Scholar
  68. White DG, Brown Jr RM (1989) Prospects for the commercialization of the biosynthesis of microbial cellulose Cellulose and wood—chemistry and technology Wiley, New York: 573–590Google Scholar
  69. Whitney SEC, Brigham JE, Darke AH, Reid J, Gidley MJ (1998) Structural aspects of the interaction of mannan-based polysaccharides with bacterial cellulose. Carbohydr Res 307:299–309CrossRefGoogle Scholar
  70. Whitney SE, Gothard MG, Mitchell JT, Gidley MJ (1999) Roles of cellulose and xyloglucan in determining the mechanical properties of primary plant cell walls. Plant Physiol 121:657–664CrossRefGoogle Scholar
  71. Whitney SEC, Wilson E, Webster J, Bacic A, Reid JSG, Gidley MJ (2006) Effects of structural variation in xyloglucan polymers on interactions with bacterial cellulose. Am J Bot 93:1402–1414CrossRefGoogle Scholar
  72. Yamamoto H, Ruelle J, Arakawa Y, Yoshida M, Clair B, Gril J (2010) Origin of the characteristic hygro-mechanical properties of the gelatinous layer in tension wood from Kunugi oak (Quercus acutissima). Wood Sci Technol 44:149–163CrossRefGoogle Scholar
  73. Zabler S, Paris O, Burgert I, Fratzl P (2010) Moisture changes in the plant cell wall force cellulose crystallites to deform. J Struct Biol 171:133–141CrossRefGoogle Scholar
  74. Zhao Z, Shklyaev OE, Nili A, Mohamed MNA, Kubicki JD, Crespi VH, Zhong L (2013) Cellulose microfibril twist, mechanics, and implication for cellulose biosynthesis. J Phys Chem A 117:2580–2589CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media Dordrecht 2014

Authors and Affiliations

  1. 1.Department of Agricultural and Biological EngineeringThe Pennsylvania State UniversityUniversity ParkUSA

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