, Volume 19, Issue 5, pp 1557–1565 | Cite as

Viscosity measurements of dilute aqueous suspensions of cellulose nanocrystals using a rolling ball viscometer

  • Erick González-Labrada
  • Derek G. GrayEmail author
Original Paper


Cellulose nanocrystals (NCC) are produced through acidic hydrolysis and mechanical disintegration of cellulose. Plans to produce NCC on an industrial scale point to the need for an efficient method to characterize its suspensions. Viscosity is a bulk property that could be used for this characterization since it accurately describes the suspension and the inherent properties of the nanocrystals. Our objective was to develop a convenient way to characterize diluted aqueous NCC suspensions without the need of complex instrumentation. The viscosity of dilute suspensions was measured with an automated rolling ball viscometer, which requires only a small amount of sample. The feasibility of the proposed procedure was confirmed by using dextran solutions as standards. The NCC suspensions were characterized by their intrinsic viscosity [η], which is directly related to the hydrodynamic dimensions of the nanocrystals. The data obtained were analyzed using the equations established by Huggins and by Fedors. Fedors’ approach gave more accurate results, leading to a value of 213 mL g−1 for the intrinsic viscosity, [η]. The non-Newtonian character of NCC suspensions at increasing concentrations was evaluated.


Rolling ball viscometer Cellulose nanocrystals Dextran solutions Dilute suspensions Viscosity 



We thank NSERC for support, and FPInnovations for a sample of NCC aqueous suspension. Thanks to Dr. Elisabeth Kloser for conductometric titration of the NCC suspension.


  1. Agoda-Tandjawa G, Durand S, Berot S, Blassel C, Gaillard C, Garnier C, Doublier JL (2010) Rheological characterization of microfibrillated cellulose suspensions after freezing. Carbohydr Polym 80(3):677–686CrossRefGoogle Scholar
  2. AMVn automated viscometer (2008) Instruction manual. Anton Paar, AustriaGoogle Scholar
  3. Antoniou E, Buitrago CF, Tsianou M, Alexandridis P (2010) Solvent effects on polysaccharide conformation. Carbohydr Polym 79(2):380–390CrossRefGoogle Scholar
  4. Araki J, Wada M, Kuga S, Okano T (1998) Flow properties of microcrystalline cellulose suspension prepared by acid treatment of native cellulose. Colloids Surf A-Physicochem Eng Asp 142(1):75–82CrossRefGoogle Scholar
  5. Araki J, Wada M, Kuga S, Okana T (1999) Influence of surface charge on viscosity behavior of cellulose microcrystal suspension. J Wood Sci 45(3):258–261CrossRefGoogle Scholar
  6. Bagchi A, Chhabra RP (1991) Rolling ball viscometry for Newtonian and power law liquids. Chem Eng Process 30(1):11–13CrossRefGoogle Scholar
  7. Beck-Candanedo S, Roman M, Gray DG (2005) Effect of reaction conditions on the properties and behavior of wood cellulose nanocrystal suspensions. Biomacromolecules 6(2):1048–1054CrossRefGoogle Scholar
  8. Bercea M, Navard P (2000) Shear dynamics of aqueous suspensions of cellulose whiskers. Macromolecules 33(16):6011–6016CrossRefGoogle Scholar
  9. Boluk Y, Lahiji R, Zhao LY, McDermott MT (2011) Suspension viscosities and shape parameter of cellulose nanocrystals (CNC). Colloids Surf A-Physicochem Eng Asp 377(1–3):297–303CrossRefGoogle Scholar
  10. Chhabra R, Richardson JF (2008) Non-Newtonian flow and applied rheology engineering applications. Butterworth-Heinemann/Elsevier, AmsterdamGoogle Scholar
  11. Dong XM, Kimura T, Revol JF, Gray DG (1996) Effects of ionic strength on the isotropic-chiral nematic phase transition of suspensions of cellulose crystallites. Langmuir 12(8):2076–2082CrossRefGoogle Scholar
  12. Fedors RF (1979) An equation suitable for describing the viscosity of dilute to moderately concentrated polymer solutions. Polymer 20(2):225–228CrossRefGoogle Scholar
  13. Gericke M, Schlufter K, Liebert T, Heinze T, Budtova T (2009) Rheological properties of cellulose/ionic liquid solutions: from dilute to concentrated states. Biomacromolecules 10(5):1188–1194CrossRefGoogle Scholar
  14. Habibi Y, Lucia LA, Rojas OJ (2010) Cellulose nanocrystals: chemistry, self-assembly, and applications. Chem Rev 110(6):3479–3500CrossRefGoogle Scholar
  15. Hasani M, Cranston ED, Westman G, Gray DG (2008) Cationic surface functionalization of cellulose nanocrystals. Soft Matter 4(11):2238–2244CrossRefGoogle Scholar
  16. Intrinsic viscosity, molar mass, and K value of polymers in dilute solution (2008) Application note. Anton Paar, AustriaGoogle Scholar
  17. Klemm D, Kramer F, Moritz S, Lindström T, Ankerfors M, Gray D, Dorris A (2011) Nanocelluloses: a new family of nature-based materials. Angew Chem Int Ed 50(24):5438–5466CrossRefGoogle Scholar
  18. Kulicke W-M (2004) Viscosimetry of polymers and polyelectrolytes. Springer, BerlinGoogle Scholar
  19. Lasseuguette E, Roux D, Nishiyama Y (2008) Rheological properties of microfibrillar suspension of TEMPO-oxidized pulp. Cellulose 15(3):425–433CrossRefGoogle Scholar
  20. Lima MMD, Borsali R (2004) Rodlike cellulose microcrystals: structure, properties, and applications. Macromol Rapid Commun 25(7):771–787CrossRefGoogle Scholar
  21. Ma J, Liang B, Cui P, Dai H, Huang R (2003) Dilute solution properties of hydrophobically associating polyacrylamide: fitted by different equations. Polymer 44(4):1281–1286CrossRefGoogle Scholar
  22. Moon RJ, Martini A, Nairn J, Simonsen J, Youngblood J (2011) Cellulose nanomaterials review: structure, properties and nanocomposites. Chem Soc Rev 40(7):3941–3994CrossRefGoogle Scholar
  23. Revol JF, Bradford H, Giasson J, Marchessault RH, Gray DG (1992) Helicoidal self-ordering of cellulose microfibrils in aqueous suspension. Int J Biol Macromol 14(3):170–172CrossRefGoogle Scholar
  24. Revol JF, Godbout L, Dong XM, Gray DG, Chanzy H, Maret G (1994) Chiral nematic suspensions of cellulose crystallites—phase separation and magnetic field orientation. Liq Cryst 16(1):127–134CrossRefGoogle Scholar
  25. Schoff CK, Kamarchik P (2005) Rheology and rheological measurements. In: Kirk-Othmer Encyclopedia of Chemical Technology. Wiley, New York. doi: 10.1002/0471238961.1808051519030815.a01.pub2
  26. Šesták J, Ambros F (1973) On the use of the rolling-ball viscometer for the measurement of rheological parameters of power law fluids. Rheol Acta 12(1):70–76CrossRefGoogle Scholar
  27. Tirtaatmadja V, Dunstan DE, Roger DV (2001) Rheology of dextran solutions. J Nonnewton Fluid Mech 97(2–3):295–301CrossRefGoogle Scholar
  28. Ureña-Benavides EE, Ao G, Davis VA, Kitchens CL (2011) Rheology and phase behavior of lyotropic cellulose nanocrystal suspensions. Macromolecules 44:8990–8998CrossRefGoogle Scholar
  29. van Voorst C, van Duijn C (1976) An improved and simplified design for a Hoeppler-type (rolling ball) microviscometer. J Phys E: Sci Instrum 9:613–615CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media B.V. 2012

Authors and Affiliations

  1. 1.Pulp and Paper Research Center, Department of ChemistryMcGill UniversityMontrealCanada

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