Direct Characterization of Chemical Properties of Fibers

  • P. Stenius
  • T. Vuorinen
Part of the Springer Series in Wood Science book series (SSWOO)


This chapter describes analytical methods that are applicable for the characterization of the chemical composition of fibers as such, without a previous separation of the components or component groups from each other. Although the details of the structure and composition generally can be obtained only to a limited extent, these direct methods possess definite advantages. For example, a minimum of preparation is required. Often samples can be analyzed more or less directly and, in some cases, the lateral and vertical distribution of different chemical structures in the fibers can be determined. The methods can be roughly divided into the following groups:
  1. 1.

    “Dry” methods for the characterization of structural features of fiber constituents. These methods include different spectroscopies: nuclear magnetic resonance (NMR), infrared (IR), Raman and ultraviolet/visible (UV/Vis) as well as pyrolysis gas chromatography (Py-GC).

  2. 2.

    “Dry” methods for the surface analysis of fibers. By far the most important of these methods are electron spectroscopy for chemical analysis (ESCA), also known as X-ray photoelectron spectroscopy (XPS), and secondary ion mass spectroscopy (SIMS).

  3. 3.

    “Wet” methods for the determination of the amounts of different components and functional groups in the fibers as a whole or on the fiber surfaces by using both chemical and enzymatic treatments.



Attenuate Total Reflectance Kraft Pulp Nuclear Magnetic Resonance Spectroscopy Chemical Shift Anisotropy Conductometric Titration 
These keywords were added by machine and not by the authors. This process is experimental and the keywords may be updated as the learning algorithm improves.


Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.


  1. Agarwal UP, Atalla RH 1995 Raman spectroscopy. In: Conners TE, Banerjee S (eds) Surface analysis of paper. CRC Press, New York 152–181Google Scholar
  2. Alén R, Kuoppala E, Oesch P 1996 Formation of the main degradation compound groups from wood and its components during pyrolysis. J Anal Appl Pyrolysis 36: 137–148CrossRefGoogle Scholar
  3. Arisz PW, Lomax JA, Boon JJ 1990 High-performance liquid chromatography/chemical ionization mass spectrometric analysis of pyrolysates of amlylose and cellulose. Anal Chem 62: 1519–1522CrossRefGoogle Scholar
  4. Atalla RH, Agarwal UP 1986 Recording Raman spectra from plant cell walls. J Raman Spectrosc 17: 229–231CrossRefGoogle Scholar
  5. Briggs D, Beamson G 1992 High resolution XPS of organic polymers. Wiley, New York, 306 pp Briggs D, Brown A, Vickerman JC 1989 Handbook of static secondary ion mass spectrometry SIMS. Wiley, New York, 164 ppGoogle Scholar
  6. Briggs D, Seah MP (eds) 1990 Practical surface analysis vol 1. Auger and X-ray photoelectron spectroscopy, 2nd edn. Wiley, New York, 674 ppGoogle Scholar
  7. Briggs D, Seah MP (eds) 1992 Practical surface analysis vol 2. Ion and neutral spectroscopy, 2nd edn. Wiley, New York, 738 ppGoogle Scholar
  8. Brinen JS, Greenhouse S, Dunlop-Jones N 1991 SIMS imaging: a new approach for studying paper surfaces. Nord Pulp Pap Res J 1: 30–36Google Scholar
  9. Brinen JS, Proverb RJ 1993 SIMS imaging of paper surfaces. Part 2. Distribution of organic surfactants. Nord Pulp Pap Res J 4: 177–183Google Scholar
  10. Buchert J, Siika-Aho M, Bailey M, Puls J, Valkeajärvi A, Pere J, Viikari L 1993 Quantitative determination of wood-derived soluble oligosaccharides by HPLC. Biotechnol Tech 7: 785790Google Scholar
  11. Buchert J, Teleman A, Harjunpää V, Tenkanen M, Viikari L, Vuorinen T 1995 Effect of cooking and bleaching on the structure of xylan in conventional pine kraft pulp. Tappi 78 (11): 125–130Google Scholar
  12. Conners TE, Banerjee S (ed) 1995 Surface analysis of paper. CRC Press, Boca Raton, 346 ppGoogle Scholar
  13. Detter-Hoskin LD, Busch KL 1995 SIMS: secondary ion mass spectrometry. In: Conners TE, Banerjee S (ed) Surface analysis of Paper. CRC Press, Boca Raton, 207–234Google Scholar
  14. Dorris GM, Gray DG 1978a The surface analysis of paper and wood fibers by ESCA I. Application to cellulose and lignin. Cellul Chem Technol 12: 9–23Google Scholar
  15. Dorris GM, Gray DG 1978b The surface analysis of paper and wood fibers by ESCA. II. Surface composition of mechanical pulps. Cellul Chem Technol 12: 721–734Google Scholar
  16. Engstrand P, Sjögren B, Olander K, Htun M 1991 The significance of carboxylic groups for the physical properties of mechanical pulp fibers. Proc 6th Int Symp Wood and Pulping Chem, Melbourne, Australia 1: 75–79Google Scholar
  17. Eriksson E, Sjöström E 1968 The influence of acidic groups on the physical properties of high yield pulps. Tappi J 51 (1): 56–59Google Scholar
  18. Faix O 1992 Fourier transform infrared spectroscopy. In: Lin SY, Dence CW (eds) Methods in lignin chemistry. Springer, Berlin Heidelberg New York, 83–109CrossRefGoogle Scholar
  19. Friese MA, Banerjee S 1995 FTIR spectroscopy. In: Conners TE, Banerjee S (ed) Surface analysis of paper. CRC Press, Boca Raton, 119–141Google Scholar
  20. Gellerstedt G, Lindfors E 1984 Structural changes in lignins during kraft cooking. Part 4. Phenolic hydroxyl groups in wood and kraft pulps. Sven Papperstidn 87: R115 - R118Google Scholar
  21. Gran G 1950 Determination of the equivalent point in potentiometric titrations. Acta Chem Scand 4: 559–577CrossRefGoogle Scholar
  22. Gray DG 1978 The surface analysis of paper and wood fibers by ESCA. III. Interpretation of carbon is peak shape. Cellul Chem Technol 12: 735–743Google Scholar
  23. Hatfield GR, Sardashti M, Maciel GE 1987 Analysis of molecular orientational order in solid samples by nuclear magnetic resonance: application to lignin and cellulose in wood. Anal Chem 59: 1659–1664CrossRefGoogle Scholar
  24. Heitner C, Min T 1987 The effect of sulphite treatment on the brightness and bleachability of chemithermomechanical pulp. Cellul Chem Technol 21: 289–296Google Scholar
  25. Helleur RJ 1987 Characterization of the saccharide composition of heteropolysaccharides by pyrolysis-capillary gas chromatography-mass spectrometry. J Anal Appl Pyrolysis 11: 297–311CrossRefGoogle Scholar
  26. Horii F, Hirai A, Kitamaru R 1983 Relationship between carbon-13 chemical shifts and conformation of oligosaccharides and cellulose in the solid state. Bull Magn Reson 5: 190–195Google Scholar
  27. Istone WK 1995 X-Ray photoelectron spectroscopy XPS. In: Conners TE, Banerjee S (eds) Surface analysis of paper. CRC Press, Boca Raton, 235–268Google Scholar
  28. Katz S, Beatson RP, Scallan AM 1984 The determination of strong and weak acidic groups in sulphite pulps. Sevensk Papperstidn 87 (6): R48–53Google Scholar
  29. Kleen M 1993 Characterization of wood and pulp using analytical pyrolysis and multivariate data analysis. Dissertation, Royal Institute of Technology, StockholmGoogle Scholar
  30. Kulick RJ, Brinen JS 1996 Probing paper surfaces with TOF SIMS–a new tool for problem solving. Proc Tappi Papermakers Conf 325–334Google Scholar
  31. Kushelevsky AP, Slifkin MA 1987 Photoacoustic spectroscopy of printing inks. J Oil Colour Chem Assoc 70: 99–101Google Scholar
  32. Lai Y-Z, Guo X, Situ W 1990 Estimation of phenolic hydroxyl groups in wood by a peroiodate oxidation method. J Wood Chem Technol 10: 365–377CrossRefGoogle Scholar
  33. Laine J, Buchert J, Viikari L, Stenius P 1996 Characterization of unbleached kraft pulps by enzymatic treatment, potentiometric titration and polyelectrolyte adsorption. Holzforschung 50: 208–214CrossRefGoogle Scholar
  34. Laine J, Lövgren L, Stenius P, Sjöberg S 1994 Potentiometric titration of unbleached kraft cellulose fibre surfaces. Coll Surf A 88: 277–287CrossRefGoogle Scholar
  35. Laine J, Stenius P 1997 The effect of charge on the fibre and paper properties of bleached industrial kraft pulps. Pap Puu 79 (4): 257–266Google Scholar
  36. Laine J, Stenius P, Carlsson G, Ström G 1994 Surface characterization of unbleached kraft pulps by means of ESCA. Cellulose 1: 145–160CrossRefGoogle Scholar
  37. Larsson N, Stenius P, Eriksson JC, Maripuu R, Lindberg B 1982 ESCA studies of sulphated polyethylene surfaces modified by adsorption of polyethyleneimine and colloidal silica particles. J Colloid Interface Sci 90: 127–136CrossRefGoogle Scholar
  38. Larsson PT, Wickholm K, Iversen T 1997 A CP/MAS 13C NMR investigation of molecular ordering in celluloses. Carbohydr Res 302: 19–25CrossRefGoogle Scholar
  39. Leary GJ, Lloyd JA, Morgan KR 1988 A CP/MAS 13C NMR study of residual lignin in kraft pulps. Holzforschung 42: 199–202CrossRefGoogle Scholar
  40. Lindström T, Carlsson G 1982a The effect of chemical environment on fibre swelling. Svensk Papperstidn 85 (1): R14 - R20Google Scholar
  41. Lindström T, Carlsson G 1982b The effect of carboxyl groups and their ionic form during drying on the hornification of cellulose fibers. Svensk Papperstidn 85 (3): R146 - R151Google Scholar
  42. Meier D, Faix O 1992 Pyrolysis-gas chromatography-mass spectrometry. In: Lin SY, Dence CW (eds) Methods in lignin chemistry. Springer, Berlin Heidelberg New York, 177–199CrossRefGoogle Scholar
  43. Mitikka M, Teeäär R, Tenkanen M, Laine J, Vuorinen T 1995 Sorption of xylans on cellulose fibers. Proc 8th Int Symp Wood and Pulping Chem, Helsinki, 111: 231–236Google Scholar
  44. Newman RH 1994 Crystalline forms of cellulose in softwoods and hardwoods. J Wood Chem Technol 14: 451–466CrossRefGoogle Scholar
  45. Newman RH, Hemmington JA 1990 Determination of the degree of cellulose crystallinity in wood by carbon-13 nuclear magnetic resonance spectroscopy. Holzforschung 44: 351–355CrossRefGoogle Scholar
  46. Saastamoinen S, Likonen J, Neimo L, Paulapuro H, Stenius P 1994 SIMS study of the adsorption of calcium and aluminum ions on unbleached and hydrogen peroxide bleached pressurized groundwood. Pap Puu 76 (1–2): 74–80Google Scholar
  47. Scallan AM, Katz S, Argyropoulos DS 1988 Conductometric titration of cellulosic fibers. In: Schuerch C (ed) Cellulose and wood–chemistry and technology. Wiley, New York, 1457–1471Google Scholar
  48. Schrader B 1995 General survey of vibrational spectroscopy. In: Schrader B (ed) Infrared and Raman spectroscopy. VCH, Weinheim, 7–61CrossRefGoogle Scholar
  49. Scott JAN, Procter AR, Fergus BJ, Goring DAI 1969 The application of UV microscopy to the distribution of lignin in wood. Description and validity of the technique. Wood Sci Technol 3: 73–92Google Scholar
  50. Shafizadeh F, Fu YL 1973 Pyrolysis of cellulose. Carbohydr Res 29: 113–122CrossRefGoogle Scholar
  51. Sillén LG 1956 Some graphical methods for determining equilibrium constants. II. On “curve-fitting” methods for two-variable data. Acta Chem Scand 10: 186–202.CrossRefGoogle Scholar
  52. Sjöström E 1989 The origin of charge on cellulosic fibers. Nord Pulp Pap Res J 4: 90–93CrossRefGoogle Scholar
  53. Sjöström E 1993 Wood chemistry. Fundamentals and applications, 2nd edn. Academic Press, San Diego, 293 ppGoogle Scholar
  54. Sjöström E, Enström B 1966 A method for the separate determination of sulpho and carboxyl groups in sulphite pulps. Svensk Papperstidn 69 (3): 55–59Google Scholar
  55. Sjöström E, Eriksson E 1968 The influence of carboxyl and carbonyl groups on the brightness stability of bleached pulps. Tappi J 51 (1): 16–19Google Scholar
  56. Sjöström E, Haglund P 1961 Studies on factors affecting the determination of carboxyl groups in cellulose. Svensk Papperstidn 64 (11): 438–446Google Scholar
  57. Tan Z, Reeve DW 1992 Spatial distribution of organochlorine in fully bleached kraft pulp fibers. Nord Pulp Pap Res J 7: 30–36CrossRefGoogle Scholar
  58. Tenkanen M, Hausalo T, Siika-Aho M, Buchert J, Viikari L 1995 Use of enzymes in combination with anionic chromatography in the analysis of carbohydrate composition of kraft pulps. Proc 8th Int Symp Wood Pulping Chem, Helsinki, Finland 2: 189–194Google Scholar
  59. Tipson RS, Parker FS 1980 Infrared spectroscopy. In: Pigman W, Horton D, Wander JD (eds) The carbohydrates, chemistry and biochemistry, 2nd edn. Academic Press, New York, 1394–1436Google Scholar
  60. VanderHart DL, Atalla RH 1984 Studies of microstructure in native celluloses using solid-state 13C NMR. Macromolecules 17: 1465–1472CrossRefGoogle Scholar
  61. Vuorinen T, Buchert J, Teleman A, Tenkanen M, Fagerström P 1996 Selective hydrolysis of hexenuronic acid groups and its application in ECF and TCF bleaching of kraft pulps. Proc Int Pulp Bleaching Conf, Washington DC, 43–51Google Scholar
  62. Westall J 1982 FITEQL: a computer program for determination of chemical equilibrium constants from experimental data, version 2.0. Report 82–02, Department of Chemistry, Oregon State University, CorvallisGoogle Scholar
  63. Wâgberg L, Winter L, Lindström T 1985 Determination of ion-exchange capacity of carboxymethylated cellulose fibers using colloid and conductometric titrations. In: Punton V (ed) Papermaking raw materials. Mechanical Engineering Ltd, London 2: 917–923Google Scholar
  64. Westermark U, Samuelson B 1993 A spectrophotometric method for the determination of sulfonic acids in wood material. Nord Pulp Pap Res J 8: 358–359, 398Google Scholar

Copyright information

© Springer-Verlag Berlin Heidelberg 1999

Authors and Affiliations

  • P. Stenius
  • T. Vuorinen

There are no affiliations available

Personalised recommendations