Skip to main content
SpringerLink
Log in

Comparison of different methods for determining lignin concentration and quality in herbaceous and woody plant residues

  • Methods Paper
  • Published:
Plant and Soil Aims and scope Submit manuscript

Abstract

Aims

Acid detergent lignin (ADL), acetyl bromide (AcBr), and cupric oxide oxidation (CuO) were compared as methods for determining lignin concentration and quality in plant residues.

Methods

These three methods were used to analyze 27 plant residues from different groups of species, i.e., legumes, crucifers, herbs, grasses, and trees.

Results

Median lignin concentrations of the 27 plant materials were 4.5% ADL and 6.0% AcBr lignin, significantly exceeding the median of 2.1% CuO lignin. ADL concentrations varied from 0.8 to 27.0%; those of AcBr and CuO lignin ranged from 1.8 to 12.2% and from 0.6 to 9.7%, respectively. AcBr lignin showed a significant negative, non-linear relationship with total N. In addition, the relationship of ADL and CuO data was negatively affected by total N.

Conclusion

The ADL method is simple and well reproducible, and large datasets are available for comparison. The AcBr procedure is fast, with less interference from non-lignin products than ADL. The CuO method is not interfered with by any other organic component in the plant material and gives additional information on the composition of the lignin. However, the release of phenolic units may be incomplete.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Log in via an institution

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Institutional subscriptions

Fig. 1
Fig. 2
Fig. 3
Fig. 4

Similar content being viewed by others

References

  • Althaus B, Papke G, Sundrum A (2013) Technical note: use of near infrared reflectance spectroscopy to assess nitrogen and carbon fractions in dairy cow feces. Anim Feed Sci Technol 185:53–59

    Article  CAS  Google Scholar 

  • Bierke A, Kaiser K, Guggenberger G (2008) Crop residue management effects on organic matter in paddy soils - the lignin component. Geoderma 146:48–57

    Article  CAS  Google Scholar 

  • Brinkmann K, Blaschke L, Polle A (2002) Comparison of different methods for lignin determination as a basis for calibration of near-infrared reflectance spectroscopy and implications of lignoproteins. J Chem Ecol 28:2483–2501

    Article  CAS  Google Scholar 

  • Chander K, Mohanty AK, Joergensen RG (2002) Decomposition of biodegradable packing materials jute, biopol, BAK and their composites in soil. Biol Fertil Soils 36:344–349

    Article  CAS  Google Scholar 

  • Crow SE, Filley TR, McCormick M, Szlávecz K, Stott DE, Gamblin D, Conyers G (2009) Earthworms, stand age, and species composition interact to influence particulate organic matter chemistry during forest succession. Biogeochem 92:61–82

    Article  Google Scholar 

  • Dao TT, Gentsch N, Mikutta R, Sauheitl L, Shibistova O, Wild B, Schnecker J, Bárta J, Čapek P, Gittel A, Lashchinskiy N, Urich T, Šantrůčková H, Richter A, Guggenberger G (2018) Fate of carbohydrates and lignin in north-east Siberian permafrost soils. Soil Biol Biochem 116:311–322

    Article  CAS  Google Scholar 

  • Dence CW (1992) The determination of lignin. In: Lin SY, Dence CW (ed) Methods in lignin chemistry. Springer, Heidelberg, Germany, pp 33–61

    Chapter  Google Scholar 

  • Derenne S, Largeau C (2001) A review of some important families of refractory macromolecules: composition, origin, and fate in soils and sediments. Soil Sci 166:833–847

    Article  CAS  Google Scholar 

  • Dignac MF, Bahri H, Rumpel C, Rasse DP, Bardoux G, Balesdent J, Girardin C, Chenu C, Mariotti A (2005) Carbon-13 natural abundance as a tool to study the dynamics of lignin monomers in soil: an appraisal at the Closeaux experimental field (France). Geoderma 128:3–17

    Article  CAS  Google Scholar 

  • Dignac MF, Pechot N, Thevenot M, Lapierre C, Bahri H, Bardoux G, Rumpel C (2009) Isolation of soil lignin by combination of ball-milling and cellulolysis: evaluation of purity and isolation efficiency with pyrolysis/GC/MS. J Anal Appl Pyrolysis 85:426–430

    Article  CAS  Google Scholar 

  • Faik A (2010) Xylan biosynthesis: news from the grasses. Plant Physiol 153:396–402

    Article  CAS  Google Scholar 

  • Fukushima RS, Hatfield RD (2004) Comparison of the acetyl bromide spectrophotometric method with other analytical lignin methods for determining lignin concentration in forage samples. J Agric Food Chem 52:3713–3720

    Article  CAS  Google Scholar 

  • Glaser B, Turrión MB, Salomon D, Ni A, Zech W (2000) Soil organic matter quantity and quality in mountain soils of the Alay range, Kyrgyzia, affected by land use change. Biol Fertil Soils 31:407–413

    Article  CAS  Google Scholar 

  • Goñi MA, Nelson B, Blanchette RA, Hedges JI (1993) Fungal degradation of wood lignins: geochemical perspectives from CuO-derived phenolic dimers and monomers. Geochim Cosmochim Acta 57:3985–4002

    Article  Google Scholar 

  • Hamer U, Marschner B (2002) Priming effects of sugars, amino acids, organic acids and catechol on the mineralization of lignin and peat. J Plant Nutr Soil Sci 165:261–268

    Article  CAS  Google Scholar 

  • Harrop-Archibald H, Didham RK, Standish RJ, Tibbett M, Hobbs RJ (2016) Mechanisms linking fungal conditioning of leaf litter to detritivore feeding activity. Soil Biol Biochem 93:119–130

    Article  CAS  Google Scholar 

  • Hatfield RD, Fukushima RS (2005) Can lignin be accurately measured? Crop Sci 45:832–839

    Article  CAS  Google Scholar 

  • Hatfield RD, Jung HJG, Ralph J, Buxton DR, Weimer PJ (1994) A comparison of the insoluble residues produced by the Klason lignin and acid detergent lignin procedures. J Sci Food Agric 65:51–58

    Article  CAS  Google Scholar 

  • Hatfield RD, Grabber J, Ralph J, Bret K (1999) Using the acetyl bromide assay to determine lignin concentrations in herbaceous plants: some cautionary notes. J Agric Food Chem 47:628–632

    Article  CAS  Google Scholar 

  • Hedges JI, Ertel JR (1982) Characterization of lignin by gas capillary chromatography of cupric oxide oxidation products. Anal Chem 54:174–178

    Article  CAS  Google Scholar 

  • Hedges JI, Mann DC (1979) The characterization of plant tissues by their lignin oxidation products. Geochim Cosmochim Acta 43:1803–1807

    Article  CAS  Google Scholar 

  • Hedges JI, Blanchette RA, Weliky K, Devol AH (1988) Effects of fungal degradation on the CuO oxidation products of lignin: a controlled laboratory study. Geochim Cosmochim Acta 52:2717–2726

    Article  CAS  Google Scholar 

  • Hensgen F, Bühle L, Donnison I, Heinsoo K, Wachendorf M (2014) Energetic conversion of European semi-natural grassland silages through the integrated generation of solid fuel and biogas from biomass: energy yields and the fate of organic compounds. Bioresour Technol 154:192–200

    Article  CAS  Google Scholar 

  • Iiyama K, Wallis AFA (1988) An improved acetyl bromide procedure for determining lignin in woods and wood pulps. Wood Sci Technol 22:271–280

    Article  CAS  Google Scholar 

  • Iiyama K, Wallis AFA (1990) Determination of lignin in herbaceous plants by an improved acetyl bromide procedure. J Sci Food Agric 51:145–161

    Article  CAS  Google Scholar 

  • Jacobs A, Kaiser K, Ludwig B, Rauber R, Joergensen RG (2011a) Application of biochemical degradation indices to the microbial decomposition of maize leaves and wheat straw in soils under different tillage systems. Geoderma 162:207–214

    Article  CAS  Google Scholar 

  • Jacobs A, Ludwig B, Schmidt JH, Bergstermann A, Rauber R, Joergensen RG (2011b) Influence of tillage on degradation kinetics using the litterbag method. Eur J Soil Biol 47:198–204

    Article  CAS  Google Scholar 

  • Johansson MB, Kögel I, Zech W (1986) Changes in the lignin fraction of spruce and pine needle litter during decomposition as studied by some chemical methods. Soil Biol Biochem 18:611–619

    Article  CAS  Google Scholar 

  • Jost DI, Joergensen RG, Sundrum A (2013) Effects of cattle faeces with different microbial biomass content on soil properties, gaseous emissions and plant growth. Biol Fertil Soils 49:61–70

    Article  Google Scholar 

  • Kalbitz K, Kaiser K, Bargholz J, Dardenne P (2006) Lignin degradation controls the production of dissolved organic matter in decomposing foliar litter. Eur J Soil Sci 57:504–516

    Article  CAS  Google Scholar 

  • Kiem R, Kögel-Knabner I (2003) Contribution of lignin and polysaccharides to the refractory carbon pool in C-depleted arable soils. Soil Biol Biochem 35:101–118

    Article  CAS  Google Scholar 

  • Klotzbücher T, Kaiser K, Guggenberger G, Gatzek C, Kalbitz K (2011) A new conceptual model for the fate of lignin in decomposing plant litter. Ecology 92:1052–1062

    Article  Google Scholar 

  • Kögel-Knabner I (1995) Composition of soil organic matter. In: Alef K, Nannipieri P (eds) Methods in applied soil microbiology and biochemistry. Academic Press, New York, pp 66–78

    Google Scholar 

  • Kögel-Knabner I, Guggenberger G, Kleber M, Kandeler E, Kalbitz K (2008) Organo-mineral associations in temperate soils: integrating biology, mineralogy, and organic matter chemistry. J Plant Nutr Soil Sci 171:61–82

    Article  Google Scholar 

  • Kondo T, Mizuno K, Kato T (1987) Some characteristics of forage plant lignin. Japan Agric Res Q 21:47–52

    CAS  Google Scholar 

  • Lobe I, Du Preez CC, Amelung W (2002) Influence of prolonged arable cropping on lignin compounds in sandy soils of the south African Highveld. Eur J Soil Sci 53:533–562

    Article  Google Scholar 

  • Lowry JB, Conlan LL, Schlink AC, McSweeney CS (1994) Acid detergent dispersible lignin in tropical grasses. J Sci Food Agric 65:41–49

    Article  CAS  Google Scholar 

  • Marschner B, Brodowski S, Dreves A, Gleixner G, Gude A, Grootes PM, Hamer U, Heim A, Jandl G, Ji R, Kaiser K, Kalbitz K, Kramer C, Leinweber P, Rethemeyer J, Schäffer A, Schmidt MWI, Schwark L, Wiesenberg GLB (2008) How relevant is recalcitrance for the stabilization of organic matter in soils? J Plant Nutr Soil Sci 171:91–110

    Article  CAS  Google Scholar 

  • Marten GC, Halgerson JL, Cherney JH (1983) Quality prediction of small grain forages by near infrared reflectance spectroscopy. Crop Sci 23:94–96

    Article  Google Scholar 

  • Martinez AT, Speranza M, Ruiz-Duenas FJ, Ferreira P, Camarero S, Guillén F, Martinez MJ, Gutiérrez A, del Rio JC (2005) Biodegradation of lignocellulosics: microbial, chemical, and enzymatic aspects of the fungal attack of lignin. Int Microbiol 8:195–204

    CAS  PubMed  Google Scholar 

  • Mehring AS, Kuehn KA, Thompson A, Pringle CM, Rosemond AD, First MR, Lowrance RR, Vellidis G (2015) Leaf litter nutrient uptake in an intermittent Blackwater river: influence of tree species and associated biotic and abiotic drivers. Funct Ecol 29:849–860

    Article  Google Scholar 

  • Melillo JM, Aber JD, Muratore JF (1982) Nitrogen and lignin control of hardwood leaf litter decomposition dynamics. Ecology 63:621–626

    Article  CAS  Google Scholar 

  • Moreira-Vilar FC, de Cássia Siqueira-Soares R, Finger-Teixeira A, de Oliveira DM, Ferro AP, da Rocha GJ, de Lourdes L, Ferrarese M, Dantas dos Santos W, Ferrarese-Filho O (2014) The acetyl bromide method is faster, simpler and presents best recovery of lignin in different herbaceous tissues than Klason and thioglycolic acid methods. PLoS One e110000:9

    Google Scholar 

  • Oestmann A, Südekum KH, Voigt K, Stangassinger M (1995) Zur Rolle von Lignin und phenolischen Monomeren in Futtermitteln für Wiederkäuer. I. Vorkommen, Funktionen und Nachweisverfahren. Uebers Tierernaehr 23:105–131

    Google Scholar 

  • Olk DC, Cassman KG, Schmidt-Rohr K, Anders MM, Mao JD, Deenik JL (2006) Chemical stabilization of soil organic nitrogen by phenolic lignin residues in anaerobic agroecosystems. Soil Biol Biochem 38:3303–3312

    Article  CAS  Google Scholar 

  • Otto A, Simpson MJ (2006) Evaluation of CuO oxidation parameters for determining the source and stage of lignin degradation in soil. Biogeochem 80:121–142

    Article  CAS  Google Scholar 

  • Preston CM, Trofymow JA, Niu J, Sayer BG (1997) 13C nuclear magnetic resonance spectroscopy with cross-polarization and magic-angle spinning investigation of the proximate-analysis fractions used to assess litter quality in decomposition studies. Can J Bot 75:1601–1613

    Article  CAS  Google Scholar 

  • Rasul G, Appuhn A, Müller T, Joergensen RG (2006) Salinity-induced changes in the microbial use of sugarcane filter cake added to soil. Appl Soil Ecol 2006:1–10

    Article  Google Scholar 

  • Rottmann N, Dyckmans J, Joergensen RG (2010) Microbial use and decomposition of maize leaf straw incubated in packed soil columns at different depths. Eur J Soil Biol 46:27–33

    Article  Google Scholar 

  • Rottmann N, Siegfried K, Buerkert A, Joergensen RG (2011) Litter decomposition in fertilizer treatments of vegetable crops under irrigated subtropical conditions. Biol Fertil Soils 47:71–80

    Article  Google Scholar 

  • Sarkanen KV, Ludwig CH (1971) Lignins. Wiley, New York

    Google Scholar 

  • Scheller E, Joergensen RG (2008) Decomposition of wheat straw differing in nitrogen content in soils under conventional and organic farming management. J Plant Nutr Soil Sci 171:886–892

    Article  CAS  Google Scholar 

  • Schmidt MWI, Torn MS, Abiven S, Dittmar T, Guggenberger G, Janssens IA, Kleber M, Kögel-Knabner I, Lehmann J, Manning DAC, Nannipieri P, Rasse DP, Weiner S, Trumbore SE (2011) Persistence of soil organic matter as an ecosystem property. Nature 478:49–56

    Article  CAS  Google Scholar 

  • Schneider T, Keiblinger KM, Schmid E, Sterflinger-Gleixner K, Ellersdorfer G, Roschitzki B, Richter A, Eberl L, Zechmeister-Boltenstern S, Riedel K (2012) Who is who in litter decomposition? Metaproteomics reveals major microbial players and their biogeochemical functions. ISME J 6:1749–1762

    Article  CAS  Google Scholar 

  • Sederoff RR, MacKay JJ, Ralph J, Hatfield RD (1999) Unexpected variation in lignin. Curr Opin Plant Biol 2:145–152

    Article  CAS  Google Scholar 

  • Taylor BR, Parkinson D, Parsons WFJ (1989) Nitrogen and lignin content as predictors of litter decay rates: a microcosm test. Ecology 70:97–104

    Article  Google Scholar 

  • Thevenot M, Dignac MF, Rumpel C (2010) Fate of lignins in soils: a review. Soil Biol Biochem 42:1200–1211

    Article  CAS  Google Scholar 

  • Van Soest E (1963) Use of detergents in the analysis of fibrous feeds. II A rapid method for the determination of fibre and lignin J AOAC Int 46:829–835

    Google Scholar 

  • Větrovský T, Steffen KT, Baldrian P (2014) Potential of cometabolic transformation of polysaccharides and lignin in lignocellulose by soil actinobacteria. PLoS One 9:e89108

    Article  Google Scholar 

  • Zech W, Johansson MB, Haumaier L, Malcolm RL (1987) CPMAS 13C NMR and IR spectra of spruce and pine litter and of the Klason lignin fraction at different stages of decomposition. Z Pflanzenernähr Bodenkd 150:262–265

    Article  CAS  Google Scholar 

  • Zimmer M (2002) Is decomposition of woodland leaf litter influenced by its species richness? Soil Biol Biochem 34:277–284

    Article  CAS  Google Scholar 

Download references

Acknowledgements

The technical assistance of Heike Maennicke, Gabi Dormann, Christiane Jatsch, and Sabine Ahlers is highly appreciated. We are grateful to Eberhardt Kölsch, Christine Wachendorf, Anja Sawallisch, and Gabriele Lehmann for their help and advice. The project was supported by the Research Training Group 1397 “Regulation of soil organic matter and nutrient turnover in organic agriculture” of the German Research Foundation (DFG).

Author information

Authors and Affiliations

  1. Soil Biology and Plant Nutrition, University of Kassel, Nordbahnhofstr. 1a, 37213, Witzenhausen, Germany

    Sibylle Faust & Rainer Georg Joergensen

  2. Soil Science and Soil Protection, Institute of Agricultural and Nutritional Sciences, Martin Luther University Halle-Wittenberg, von-Seckendorff-Platz 3, 06120, Halle, Germany

    Klaus Kaiser

  3. Soil Biogeochemistry, Institute of Agronomy and Nutritional Sciences, Martin Luther University Halle-Wittenberg, von-Seckendorff-Platz 3, 06120, Halle, Germany

    Katja Wiedner & Bruno Glaser

Authors
  1. Sibylle Faust
    View author publications

    You can also search for this author in PubMed Google Scholar

  2. Klaus Kaiser
    View author publications

    You can also search for this author in PubMed Google Scholar

  3. Katja Wiedner
    View author publications

    You can also search for this author in PubMed Google Scholar

  4. Bruno Glaser
    View author publications

    You can also search for this author in PubMed Google Scholar

  5. Rainer Georg Joergensen
    View author publications

    You can also search for this author in PubMed Google Scholar

Corresponding author

Correspondence to Sibylle Faust.

Additional information

Responsible Editor: Ingrid Koegel-Knabner.

Electronic supplementary material

ESM 1

(DOCX 37.6 kb)

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Faust, S., Kaiser, K., Wiedner, K. et al. Comparison of different methods for determining lignin concentration and quality in herbaceous and woody plant residues. Plant Soil 433, 7–18 (2018). https://doi.org/10.1007/s11104-018-3817-0

Download citation

  • Received:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s11104-018-3817-0

Keywords

Search

Navigation