The Determination of Lignin

  • C. W. Dence
Part of the Springer Series in Wood Science book series (SSWOO)

Abstract

The determination of lignin is an analysis that is performed routinely for characterizing lignocellulosic material, for assessing the effects of chemical, physical, and biological treatments of wood and pulp, for monitoring effluents in wood processing industries and, in the case of chemical pulps, for estimating bleach chemical requirements. The general approaches followed in this determination, together with their associated procedural variations, have been outlined and thoroughly detailed by several authors (Brauns 1952, Brauns and Brauns 1960, Browning 1967a, Pearl 1967). Therefore, the content of this section is confined mainly to a description and discussion of the preferred and/or widely accepted methods for determining lignin when present in a variety of representative lignified materials.

Preview

Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.

References

  1. Alén R, Hartus T (1988) UV spectrophotometric determination of lignin from alkaline pulping liquors. Cellul Chem Technol 22: 613–618Google Scholar
  2. Bagby MO, Cunningham RL, Maloney RL (1973) Ultraviolet spectral determination of lignin. Tappi 56 (4): 162–163Google Scholar
  3. Bagby MO, Nelson GH, Helman EG, Clark TF (1971) Determination of lignin in non-wood plant fiber sources. Tappi 54: 1876–1878Google Scholar
  4. Barnes CA, Collias EE, Felicetta VF, Goldschmid O, Hrutfiord BF, Livingston A, McCarthy JL, Toombs GL, Waldichuk M, Westley R (1963) A standardized Pearl-Benson, or nitroso, method recommended for the examination of spent sulfite liquor or sulfite waste liquor concentration in waters. Tappi 46: 347–351Google Scholar
  5. Bartunek R (1959) A nonhydrolytic spectrophotometric method for determining lignin in high-purity pulps. Tappi 42: 553–556Google Scholar
  6. Berzins V (1965) A rapid procedure for the determination of kappa number. Tappi 48: 15–20Google Scholar
  7. Berzins V (1966) Micro-kappa numbers. Pulp Pap Mag Can 67: T206–T208Google Scholar
  8. Bethge PO, Gran G, Ohlsson K-E (1952) Determination of lignin in chemical wood pulp. I. Principles and methods. Sven Papperstidn 55: 44–48Google Scholar
  9. Bilikova A (1973) Verification of analytical methods for the determination of lignin in water. Vodni Hospod 23(2):44; Abstr Bull Inst Pap Chem 48: 1245Google Scholar
  10. Birkett MD, Gambino MJT (1989) Estimation of pulp kappa number with near-infrared spectroscopy. Tappi J 72 (9): 193–197Google Scholar
  11. Bland DE (1956) Spectrophotometric determination of lignin in eucalypt soda pulp. Appita 10: 287–295Google Scholar
  12. Bogomolov BD, Pivovarova VA, Gorbunova OF (1986) Determination of lignin and ether-soluble substances in aqueous solutions by fluorimetry. Khim Drev (Riga) 2: 54–57Google Scholar
  13. Bolker HI, Somerville NG (1962) Ultraviolet spectroscopic studies of lignins in the solid state. I. Isolated lignin preparations. Tappi 45: 826–829Google Scholar
  14. Boutelje JB, Eriksson I (1982) A UV-microscopy study of lignin in middle lamella fragments from fibers of mechanical pulp of spruce. Sven Papperstidn 85: R39–R42Google Scholar
  15. Boutelje JB, Jonsson U (1980) Ultraviolet microscope photometry of pulp fibers. UV- absorbance and its relationship to chlorine number, kapp number and lignin content. Cellul Chem Technol 14: 53–67Google Scholar
  16. Brauns FE (1952) The chemistry of lignin. Academic Press, New York, 151–177CrossRefGoogle Scholar
  17. Brauns FE, Brauns DA (1960) The chemistry of lignin: supplement volume. Academic Press, New York, 127–167CrossRefGoogle Scholar
  18. Browning BL (1967a) Methods of wood chemistry Vol. II. Interscience, New York, 785–823Google Scholar
  19. Browning BL (1967b) Methods of wood chemistry Vol. I. Wiley-Interscience, New York, 14Google Scholar
  20. Bublitz WJ (1981) Fluorescence of pulping liquors: a tool for digester control? Tappi 64 (6): 73–76Google Scholar
  21. Bublitz WJ, Meng TY (1978) The fluorometric behavior of pulping waste liquors: a valuable tool for lignin and pulping research. Tappi 61 (2): 27–30Google Scholar
  22. Cho NS (1984) Spectrophotometric determination of lignin in woody samples. J Tappik 16 (1): 3–9Google Scholar
  23. Colombo P, Corbetta D, Pirotta A, Ruffini G (1962) Chlorine number as a method for evaluation of lignin content of a pulp. Pulp Pap Mag Can 63: T126–T140Google Scholar
  24. Effland MJ (1977) Modified procedure to determine acid-insoluble lignin in wood and pulp. Tappi 60 (10): 143–144Google Scholar
  25. Ellis GH (1949) Report on lignin and cellulose in plants. J Assoc Off Agric Chem 32: 287–291Google Scholar
  26. Felicetta VF, McCarthy JL (1963) Spent sulfite liquor. X. The Pearl-Benson, or nitroso, method for the estimation of spent sulfite liquor concentration in waters. Tappi 46: 337–347Google Scholar
  27. Fergus BJ, Goring DAI (1970) The distribution of lignin in birchwood as determined by ultraviolet microscopy. Holzforschung 24: 118–124CrossRefGoogle Scholar
  28. Fergus BJ, Procter AR, Scott JAN, Goring DAI (1969) The distribution of lignin in sprucewood as determined by ultraviolet microscopy. Wood Sci Technol 3: 117–138CrossRefGoogle Scholar
  29. Genco JM, Hassler JC, Busayasakul N (1984) Total organic carbon as an indicator of wood delignification. Tappi 67 (7): 92–95Google Scholar
  30. Germer ZI, Maiorova ID (1972) [Proposed] changes in the method of determining the degree of delignification of pulp. Bumazh Prom 8:23–24; Abstr Bull Inst Pap Chem 43: 8400Google Scholar
  31. Giertz HW (1945) Bestamning av restlignin. En kolorimetrisk method for knotroll av blekningsforloppet (Determination of residual lignin. A colorimetric method for control of bleaching). Sven Papperstidn 48: 485–489Google Scholar
  32. Goldschmid O (1971) Ultraviolet spectra. In: Sarkanen KV, Ludwig CH (eds) Lignins. Occurrence, formation, structure and reactions. Wiley-Interscience, New York, 160–263Google Scholar
  33. Hardell H-L, Leary GJ, Stoll M, Westermark U (1980) Variation in lignin structure in defined morphological parts of spruce. Sven Papperstidn 83: 44–49Google Scholar
  34. Hatton JV (1975) Kappa number-permanganate number relationships for softwoods and hardwoods. Tappi 58 (10): 150–151Google Scholar
  35. Haw JF, Maciel GE, Schroeder HA (1984) Carbon-13 nuclear magnetic resonance spectrometric study of wood and wood pulping with cross polarization and magic-angle spinning. Anal Chem 56: 1323–1329CrossRefGoogle Scholar
  36. Hemmingson JA, Newman RH (1985) A CP/MAS 13C NMR study of the effect of steam explosion processes on wood composition and structure. J Wood Chem Technol 5: 159–188CrossRefGoogle Scholar
  37. Henriksen A, Kesler RB (1970) The Nu-number, a measure of lignin in pulp. Tappi 53: 1131–1140Google Scholar
  38. Hess CL (1952) An investigation of the homogeneity of isolated native black spruce lignin. Tappi 35: 312–320Google Scholar
  39. Iiyama K, Wallis AFA (1988a) An improved acetyl bromide procedure for determining lignin in woods and wood pulps. Wood Sci Technol 22: 271–280CrossRefGoogle Scholar
  40. Iiyama K, Wallis AFB (1988b) Spectrophotometric determination of lignin in polyphenol-containing eucalyptus woods by the acetyl bromide method. Appita 41: 442–446Google Scholar
  41. Jayme G, Jerratsch H-J (1960) Die Kj-Methode, eine modifizierte Kappa-Zahl-Bestimmung fur Halbzellstoffe in iiber 70% Ausbeute (The Kj-method, a modified kappa-number determination for semichemical pulps of more than 70% yield). Papier 14: 718–723Google Scholar
  42. Johansson D (1935) Testing methods for evaluation of unbleached chemical pulp. Pap Trade J 101 (13): 101–104Google Scholar
  43. Johnson DB, Moore WE, Zank LC (1961) The spectrophotometric determination of lignin in small wood samples. Tappi 44: 793–798Google Scholar
  44. Joyce CS, Kleinert TN (1957) Short wavelength ultraviolet absorption of various lignin and related substances. II. Lignin determination in sulfite pulping liquors. Pulp Pap Mag Can 58 (6): 131–134Google Scholar
  45. Jurkiewicz S (1977) Problem of the effect of interfering factors in the quantitative determination of lignin compounds in aqueous solutions. Przegl Papier 33(1):30–35; Abstr Bull Inst Pap Chem 48: 1245Google Scholar
  46. Kleinert TN, Joyce CS (1957a) Short wavelength absorption of various lignins and related substances. IV. Lignin determination in sulfate pulping liquors. Pulp Pap Mag Can 58 (11): 147–152Google Scholar
  47. Kleinert TN, Joyce CS (1957b) Short wavelength absorption of various lignins and related substances. III. The flow-micro cuvette for continuous measurement of lignin concentration in sulfite cooking liquors. Pulp Pap Mag Can 58 (7): 215–219Google Scholar
  48. Kolboe S, Ellefsen O (1962) Infrared investigations of lignin. A discussion of some recent results. Tappi 45: 163–166Google Scholar
  49. Kratzl K, Billek G (1957) Synthesis and testing of lignin precursors. Tappi 40: 269–285Google Scholar
  50. Kyrklund B, Palenius I (1964) The total lignin content of sulphite pulps and its relation to the kappa number. Pap Puu 46: 513–520Google Scholar
  51. Kyrklund B, Strandell G (1967) A modified chlorine number for evaluation of cooking degree of high-yield pulps. Pap Puu 49: 99–106Google Scholar
  52. Kyrklund B, Strandell G (1969) Applicability of the chlorine number for evaluation of the lignin content of pulp. Pap Puu 51: 299–305Google Scholar
  53. Lai Y-Z, Sarkanen KV (1971) Isolation and structural studies. In: Sarkanen KV, Ludwig CH (eds) Lignins. Occurrence, formation, structure and reactions. Wiley-Interscience, New York, 190–195Google Scholar
  54. Leithe W (1973) The analysis of organic pollutants in water and waste water. Ann Arbor Science, Ann Arbor Michigan, 191–193Google Scholar
  55. Lindström T, Glad-Nordmark G (1978) Chemical characterization of the fines from unbleached kraft pulp. Sven Papperstidn 81: 489–492Google Scholar
  56. Loras V, Loschbrandt F (1956) Gravimetric and absorptiometric determination of lignin in pulp and wood. Nor Skogind 10: 1–12Google Scholar
  57. Loras V, Loschbrandt F (1961) Determination of lignin in sulfite pulps. Nor Skogind 15: 302–309Google Scholar
  58. Maekawa F, Ichizawa T, Koshijima T (1989) An evaluation of the acid-soluble lignin determination in analysis of lignin by the sulfuric acid method. J Wood Chem Technol 9: 549–567CrossRefGoogle Scholar
  59. Marton J (1967) Determination of lignin in small pulp and paper samples using the acetyl bromide method. Tappi 50: 335–337Google Scholar
  60. Marton J, Sparks HE (1967) Determination of lignin in pulp and paper by infrared multiple internal reflectance. Tappi 50: 363–368Google Scholar
  61. McLean JD (1965) Hypo number (chlorine number using sodium hypochlorite solution). Pulp Pap Mag Can 66 T103–T106Google Scholar
  62. McNaughton JG, Yean WO, Goring DAI (1967) Macromolecular properties of kraft lignins from spruce made soluble by a continuous flow process. Tappi 50: 548–553Google Scholar
  63. Michell AJ, Watson AJ, Higgins HG (1965) An infrared spectroscopic study of delignification of Eucalyptus regnans. Tappi 48: 520–532Google Scholar
  64. Morrison IM (1972a) A semimicro method for the determination of lignin and its use in predicting the digestibility of forage crops. J Sei Food Agric 23: 455–463CrossRefGoogle Scholar
  65. Morrison IM (1972b) Improvements in the acetyl bromide technique to determine lignin and digestibility and its application to legumes. J Sci Food Agric 23: 1463–1469CrossRefGoogle Scholar
  66. Ni Y, Kubes GJ, Van Heiningen ARP (1990) Methanol number: a fast method to determine the lignin content of pulp. J Pulp Pap Sci 16: J83–J86Google Scholar
  67. Obst JR (1982) Guaiacyl and syringyl lignin composition in hardwood cell components. Holzforschung 36: 143–152CrossRefGoogle Scholar
  68. Patterson RF, Keays JL, Hart JS, Strapp RK, Luner P (1951) The spectrophotometric determination of lignin in sulfite cooking liquor. Pulp Pap Mag Can 52 (12): 105–111Google Scholar
  69. PaulSK, Oswal N, Maheswari S (1985) Monitoring the progress of pulping by fluorometric analysis of spent sulfate liquor. Ind Pulp Pap 40: 11–16Google Scholar
  70. Pearl IA (1967) The chemistry of lignin. Marcel Dekker, New York, 32–58Google Scholar
  71. Pearl IA, Benson HK (1940) The determination of lignin in sulfite pulping liquors. Pap Trade J 111 (18): 35–36Google Scholar
  72. Pearl IA, Busche LR (1960) Studies on the chemistry of aspenwood. XI. The Klason lignin determination as applied to aspenwood with special reference to acid-soluble lignin. Tappi 43: 961–970Google Scholar
  73. Robinson DH (1977) A comprehensive study of the bleaching of mechanical pulps with hydrogen peroxide and sodium dithionite. MS thesis SUNY College of Environmental Science and Forestry, Syracuse, NY, 98 ppGoogle Scholar
  74. Saka S, Thomas RJ, Gratzl JS (1978) Lignin distribution. Determination by energy-dispersive analysis of X-rays. Tappi 61 (1): 73–76Google Scholar
  75. Schadenböck W, Prey V (1972) Eine neue quantitative Lignin-Bestimmung mit Hilfe der UV-Spektrophotometrie (A new quantitative lignin determination by ultraviolet spectrophotometry). Papier 26: 117–118Google Scholar
  76. Schöning AG, Johansson G (1965) Absorptiometric determination of acid-soluble lignin in semichemical bisulfite pulps and in some woods and plants. Sven Papperstidn 68: 607–613Google Scholar
  77. Schultz TP, Templeteon MC, McGinnis GD (1985) Rapid determination of lignocellulose by diffuse reflectance Fourier transform infrared spectrometry. Anal Chem 57: 2867–2869CrossRefGoogle Scholar
  78. Sjöström E, Enström B (1966) Spectrophotometric determination of the residual lignin in pulp after dissolution in cadoxene. Sven Papperstidn 69: 469–476Google Scholar
  79. Srinivasa Rao Y, Shukla RN, Maheshwari S, Kulkarni AY, Jivendra Y (1983) Determination of permanganate and kappa number of pulp with high ash content. IPPTA 20 (3): 55–56Google Scholar
  80. Stewart CM, Foster OH, Cohen WE, Leslie RT, Watson AJ (1951) The selection and preparation of a reporducible wood sample for chemical studies. Appita 5: 267–311Google Scholar
  81. Swan B (1965) Isolation of acid-soluble lignin from the Klason lignin determination. Sven Papperstidn 68: 791–795Google Scholar
  82. Tasman JE, Berzins V (1957a) The permanganate consumption of pulp materials. I. Development of a basic procedure. Tappi 40: 691–694Google Scholar
  83. Tasman JE, Berzins V (1957b) The permanganate consumption of pulp materials. II. The KAPPA number. Tappi 40: 695–699Google Scholar
  84. Tasman JE (1959) The permanganate consumption of pulp materials. IV. The kappa correction coefficient. Pulp Pap Mog Can 60 (No. C): 231–235Google Scholar
  85. Technical Association of the Pulp and Paper Industry, Atlanta, (1983) Acid-insoluble lignin in wood and pulp. Official Test Method T-222 om-8Google Scholar
  86. Technical Association of the Pulp and Paper Industry, Atlanta, (1985a) Micro kappa number. Useful Method UM 246Google Scholar
  87. Technical Association of the Pulp and Paper Industry, Atlanta, (1985b) Acid-soluble lignin in wood and pulp. Useful Method UM 250Google Scholar
  88. Timell TE (1969) The chemical composition of tension wood. Sven Papperstidn 72: 173–181Google Scholar
  89. Timell TE (1986) Compression wood in gymosperms, Vol. 1. Springer, Berlin Heidelberg New York Tokyo, 294, 295, 299, 311Google Scholar
  90. Trout PE, Franckowiak PA, Ham JL, Browning BL, Bublitz LO (1953) Routine determination of lignin in semichemical pulps by a modified Tingle procedure. Tappi 36: 123–126Google Scholar
  91. van Zyl JD (1978) Notes on the spectrophotometric determination of lignin in wood samples. Wood Sci Technol 12: 251–259CrossRefGoogle Scholar
  92. Whiting P, Favis BD, St. Germain FGT, Goring DAI (1981) Fractional separation of middle lamella and secondary wall tissue from spruce wood. J Wood Chem Technol 1: 29–42CrossRefGoogle Scholar
  93. Wu Y-T, Wilson JW (1967) Lignification within coniferous growth zones. Pulp Pap Mag Can 68:T159-T164, T-171Google Scholar
  94. Yean WO, Goring DAI (1965) The molecular weight of lignosulfonates from morphologically different subdivisions of wood structure. Sven Papperstidn 68: 787–790Google Scholar
  95. Yoshihara K, Kobayashi T, Fujii T, Akamatsu I (1984) A novel modification of Klason lignin quantitative method. J Jpn Tappi 38 (4): 86–95Google Scholar

Copyright information

© Springer-Verlag Berlin Heidelberg 1992

Authors and Affiliations

  • C. W. Dence

There are no affiliations available

Personalised recommendations