, Volume 15, Issue 4, pp 547–553 | Cite as

The residual amide content of cellulose sequentially solvent-exchanged and then vacuum-dried

  • Daisuke Ishii
  • Akira Isogai


Most celluloses are soluble in 8 mass % lithium chloride/N,N-dimethylacetamide (LiCl/DMAc) and/or 8 mass % LiCl/1,3-dimethyl-2-imidazolidinone (LiCl/DMI) with solvent-exchange treatment from water to DMAc or DMI through acetone. In this study, the residual DMAc or DMI adsorbed on celluloses after the solvent-exchange and then vacuum-drying at 60 °C for 48 h was determined by UV spectroscopy and elementary analysis. Significant amounts of DMI or DMAc remain in the solvent-exchanged celluloses even after vacuum drying: about 1.2 mmol/g and 1.0 mmol/g for DMI and DMAc, respectively. Thus, corrections of molecular-mass parameters of celluloses, which were reported in previous literatures based on the assumption that no residual amides are present in the solvent-exchanged and then vacuum-dried celluloses, are needed.


Solvent exchange LiCl/DMAc LiCl/DMI Residual amide UV spectroscopy Molecular mass determination 



This research was supported by a Grant-in-Aid for Young Scientists (Grant number 19-4140) from the Japan Society for the Promotion of Science (JSPS). The authors thank Mr. Takehiko Uematsu of our laboratory, who is a visiting researcher from Kao Corporation, Japan, for his help in determining nitrogen contents of celluloses.


  1. Ishii D, Tatsumi D, Matsumoto T (2003) Effect of solvent exchange on the solid structure and dissolution behavior of cellulose. Biomacromolecules 4:1238–1243CrossRefGoogle Scholar
  2. Ishii D, Kanazawa Y, Tatsumi D, Matsumoto T (2007) Effect of solvent exchange on the pore structure and dissolution behavior of cellulose. J Appl Polym Sci 103:3976–3984CrossRefGoogle Scholar
  3. Ishii D, Tatsumi D, Matsumoto T (2008) Effect of solvent exchange on the supramolecular structure, the molecular mobility and the dissolution behavior of cellulose in LiCl/DMAc. Carbohydr Res (in press) doi:  10.1016/j.carres.2008.01.035
  4. Isogai A, Atalla RH (1998) Dissolution of cellulose in aqueous NaOH solutions. Cellulose 5:309–319CrossRefGoogle Scholar
  5. Heinze T, Liebert T (2001) Unconventional methods in cellulose functionalization. Prog Polym Sci 26:1689–1762CrossRefGoogle Scholar
  6. Matsumoto T, Tatsumi D, Tamai N, Takaki T (2002) Solution properties of celluloses from different biological origins in LiCl·DMAc. Cellulose 8:275–282CrossRefGoogle Scholar
  7. McCormick CL, Callais PA, Hutchinson BH Jr (1985) Solution studies of cellulose in lithium chloride and N,N-dimethylacetamide. Macromolecules 18:2394–2401CrossRefGoogle Scholar
  8. Potthast A, Rosenau T, Sixta H, Kosma P (2002) Degradation of cellulosic materials by heating in DMAc/LiCl. Tetrahedron Lett 43:7757–7759CrossRefGoogle Scholar
  9. Sjöholm E, Gustafsson K, Berthold F, Colmsjö A (2000) Influence of the carbohydrate composition on the molecular weight distribution of kraft pulps. Carbohydr Polym 41:1–7CrossRefGoogle Scholar
  10. Tamai N, Tatsumi D, Matsumoto T (2004) Rheological properties and molecular structure of tunicate cellulose in LiCl/1,3-dimethyl-2-imidazolidinone. Biomacromolecules 5:422–432CrossRefGoogle Scholar
  11. Turbak A (1984) Recent developments in cellulose solvent systems. Tappi J 67:94–96Google Scholar
  12. Yanagisawa M, Shibata I, Isogai A (2004) SEC-MALLS analysis of cellulose using LiCl/1,3-dimethyl-2-imidazolidinone as an eluent. Cellulose 11:169–176CrossRefGoogle Scholar
  13. Yanagisawa M, Shibata I, Isogai A (2005a) SEC-MALLS analysis of softwood kraft pulp using LiCl/1,3-dimethyl-2-imidazolidinone as an eluent. Cellulose 12:151–158CrossRefGoogle Scholar
  14. Yanagisawa M, Isogai A (2005b) SEC-MALS-QELS study on the molecular conformation of cellulose in LiCl/amide solutions. Biomacromolecules 6:1258–1265CrossRefGoogle Scholar
  15. Zhang L, Ruan D, Zhou J (2001) Structure and properties of regenerated cellulose films prepared from cotton linters in NaOH/urea aqueous solution. Ind Eng Chem Res 40:5923–5928CrossRefGoogle Scholar
  16. Zhang L, Ruan D, Gao S (2002) Dissolution and regeneration of cellulose in NaOH/thiourea aqueous solution. J Polym Sci Polym Phys 40:1521–1529CrossRefGoogle Scholar

Copyright information

© Springer Science+Business Media B.V. 2008

Authors and Affiliations

  1. 1.Graduate School of Agricultural and Life SciencesThe University of TokyoTokyoJapan

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