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The impact of acid hydrolysis conditions on carbohydrate determination in lignocellulosic materials: a case study with Eucalyptus globulus bark

  • Ricardo Jorge Oliveira , Bruna Santos , Maria J. Mota , Susana R. Pereira ORCID logo EMAIL logo , Pedro C. Branco and Paula C. R. Pinto
Published/Copyright: April 20, 2021
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Holzforschung
From the journal Holzforschung Volume 75 Issue 10

Abstract

Lignocellulosic biomass represents a suitable feedstock for production of biofuels and bioproducts. Its chemical composition depends on many aspects (e.g. plant source, pre-processing) and it has impact on productivity of industrial bioprocesses. Numerous methodologies can be applied for biomass characterisation, with acid hydrolysis being a particularly relevant step. This study intended to assess the most suitable procedures for acid hydrolysis, taking Eucalyptus globulus bark as a case study. For that purpose, variation of temperature (90–120 °C) was evaluated over time (0–5 h), through monosaccharides and oligosaccharides contents and degradation. For glucose, the optimal conditions were 100 °C for 2.5 h, reaching a content of 48.6 wt.%. For xylose, the highest content (15.2 wt.%) was achieved at 90 °C for 2 h, or 120 °C for 0.5 h. Maximum concentrations of mannose and galactose (1.0 and 1.7 wt.%, respectively) were achieved at 90 and 100 °C (2–3.5 h) or at 120 °C (0.5–1 h). These results revealed that different hydrolysis conditions should be applied for different sugars. Using this approach, total sugar quantification in eucalyptus bark was increased by 4.3%, which would represent a 5% increase in the ethanol volume produced, considering a hypothetical bioethanol production yield. This reflects the importance of feedstock characterization on determination of economic viability of industrial processes.

Keywords: bioprocesses; carbohydrate degradation; eucalyptus; hardwood; hydrolysis optimization; process economics
Corresponding author: Susana R. Pereira, RAIZ - Forest and Paper Research Institute, Quinta de S. Francisco, Rua José Estevão (EN 230-1), Aveiro3800-783, Portugal, E-mail:

Funding source: Project Inpactus – Innovative Products and Technologies from Eucalyptus

Award Identifier / Grant number: POCI-01-0247-FEDER-021874

  1. Author contributions: All the authors have accepted responsibility for the entire content of this submitted manuscript and approved submission.

  2. Research funding: This work was carried out under the Project Inpactus – Innovative Products and Technologies from Eucalyptus, Project No. 21874 funded by Portugal 2020 through European Regional Development Fund (ERDF) in the frame of COMPETE 2020 n° 246/AXIS II/2017.

  3. Conflict of interest statement: The authors declare no conflicts of interest regarding this article.

References

Aguilar, R., Ramírez, J.A., Garrote, G., and Vázquez, M. (2002). Kinetic study of the acid hydrolysis of sugar cane bagasse. J. Food Eng. 55: 309–18. https://doi.org/10.1016/s0260-8774(02)00106-1.Search in Google Scholar

Basumallick, L. and Rohrer, J. (2013). Determination of hydroxymethylfurfural in honey and biomass. Application Note 270. Waltham: Thermo Scientific.Search in Google Scholar

Blakeney, A.B., Harris, P.J., Robert, J.H., and Stone, B.A. (1983). A simple and rapid preparation of alditol acetates for monosaccharide analysis. Carbohydr. Res. 113: 291–99. https://doi.org/10.1016/0008-6215(83)88244-5.Search in Google Scholar

CELPA (2019). Boletim Estatístico Indústria Papeleira Portuguesa 2019.Search in Google Scholar

Chovau, S., Degrauwe, D., and Van Der Bruggen, B. (2013). Critical analysis of techno-economic estimates for the production cost of lignocellulosic bio-ethanol. Renew. Sustainable Energy Rev. 26: 307–21. https://doi.org/10.1016/j.rser.2013.05.064.Search in Google Scholar

De Carvalho, D.M. and Colodette, J.L. (2017). Comparative study of acid hydrolysis of lignin and polysaccharides in biomasses. Bioresources 12: 6907–23. https://doi.org/10.15376/biores.12.2.3088-3107.Search in Google Scholar

EU Eurostat Database (2020). Roundwood production, Available at: https://appsso.eurostat.ec.europa.eu/nui/submitViewTableAction.do (Accessed 12 Aug 2020).Search in Google Scholar

Faaij, A. (2018). Biomass resources, worldwide. In: Meyers, R.A. (Ed.). Encyclopedia of sustainability science and technology. New York: Springer, pp. 1–53.10.1007/978-1-4939-2493-6_259-3Search in Google Scholar

Feng, S., Cheng, S., Yuan, Z., Leitch, M., and Xu, C. (2013). Valorization of bark for chemicals and materials: a review. Renew. Sustainable Energy Rev. 26: 560–578. https://doi.org/10.1016/j.rser.2013.06.024.Search in Google Scholar

Food and Agriculture Organization (2019). Global forest products - facts and figures 2018. Rome: Forest Products and Statistics Team.Search in Google Scholar

Garrote, G., Domínguez, H., and Parajó, J.C. (2001a). Generation of xylose solutions from Eucalyptus Globulus wood by autohydrolysis-posthydrolysis processes: posthydrolysis kinetics. Bioresour. Technol. 79: 155–64. https://doi.org/10.1016/s0960-8524(01)00044-x.Search in Google Scholar

Garrote, G., Domínguez, H., and Parajó, J.C. (2001b). Kinetic modelling of corncob autohydrolysis. Process Biochem. 36: 571–578. https://doi.org/10.1016/s0032-9592(00)00253-3.Search in Google Scholar

Gnansounou, E., and Dauriat, A. (2010). Techno-economic analysis of lignocellulosic ethanol: a review. Bioresour. Technol. 101: 4980–91. https://doi.org/10.1016/j.biortech.2010.02.009.Search in Google Scholar

Hames, B.R. (2009). Biomass compositional analysis for energy applications. In: Biofuels. Totowa, NJ: Humana Press, pp. 145–167.10.1007/978-1-60761-214-8_11Search in Google Scholar PubMed

Hess, J.R., Christopher, T.W., and Kenney, L. (2007). Cellulosic biomass feedstocks and logistics for ethanol production. Biofuel. Bioprod. Biorefin. 1: 181–90. https://doi.org/10.1002/bbb.26.Search in Google Scholar

Iakovlev, M., and van Heiningen, A. (2011). SO2-ethanol-water (SEW) pulping: I. Lignin determination in pulps and liquors. J. Wood Chem. Technol. 31: 233–249.https://doi.org/10.1080/02773813.2010.523161.Search in Google Scholar

ICNF (2015). 6.o Inventário Florestal Nacional (IFN6) - 2015 Relatório Final. Instituto da Conservação da Natureza e das Florestas.Search in Google Scholar

Jana, A., Ghosh, D., Dasgupta, D., Das Mohapatra, P.K., and Mondal, K.C. (2017). Biopulping of lignocellulose. In: Kulia, A., and Sharma, V. (Eds.), Lignocellulosic biomass production and industrial applications. Beverly: Scrivener Publishing LLC, pp. 93–109.10.1002/9781119323686.ch5Search in Google Scholar

Karimi, K., and Taherzadeh, M.J. (2016). A critical ceview of analytical methods in pretreatment of lignocelluloses: composition, imaging, and crystallinity. Bioresour. Technol. 200: 1008–18. https://doi.org/10.1016/j.biortech.2015.11.022.Search in Google Scholar

Krasznai, D., Hartley, R.C., Roy, H.M., Champagne, P., and Cunningham, M.F. (2018). Compositional analysis of lignocellulosic biomass: conventional methodologies and future outlook. Crit. Rev. Biotechnol. 38: 199–217. https://doi.org/10.1080/07388551.2017.1331336.Search in Google Scholar

Lavarack, B.P., Griffin, G.J., and Rodman, D. (2002). The acid hydrolysis of sugarcane bagasse hemicellulose to produce xylose, arabinose, glucose and other products. Biomass Bioenergy 23: 367–80. https://doi.org/10.1016/s0961-9534(02)00066-1.Search in Google Scholar

Lenihan, P., Orozco, A., O’Neill, E., Ahmad, M.N.M., Rooney, D.W., and Walker, G.M. (2010). Dilute acid hydrolysis of lignocellulosic biomass. Chem. Eng. J. 156: 395–403. https://doi.org/10.1016/j.cej.2009.10.061.Search in Google Scholar

Lenihan, P., Orozco, A., O’Neill, E., Ahmad, M.N.M., Rooney, D.W., Mangwandi, C., and Walker, G.M. (2011). Kinetic modelling of dilute acid hydrolysis of lignocellulosic biomass. In: Bernardes, M.A.D.S. (Ed.), Biofuel production-recent developments and prospects. Rijeka: Intech, pp. 293–308.10.5772/17129Search in Google Scholar

Liu, Y., Nie, Y., Lu, X., Zhang, X., and He, H. (2019). Cascade utilization of lignocellulosic biomass to high-value products. Green Chem. 21: 3499–3535. https://doi.org/10.1039/c9gc00473d.Search in Google Scholar

Maloney, M.T., Chapman, T.W., and Baker, A.J. (1986). An engineering analysis of the production of xylose by dilute acid hydrolysis of hardwood hemicellulose. Biotechnol. Prog. 2: 192–202. https://doi.org/10.1002/btpr.5420020407.Search in Google Scholar

Mellouk, H., Meullemiestre, A., Maache-Rezzoug, Z., Bejjani, B., Dani, A., and Rezzoug, S.-A. (2016). Valorization of industrial wastes from French maritime pine bark by solvent free microwave extraction of volatiles. J. Clean. Prod. 112: 4398–4405. https://doi.org/10.1016/j.jclepro.2015.06.129.Search in Google Scholar

Miranda, I., Gominho, J., Mirra, I., and Pereira, H. (2013). Fractioning and chemical characterization of barks of Betula pendula and Eucalyptus globulus. Ind. Crop. Prod. 41: 299–305. https://doi.org/10.1016/j.indcrop.2012.04.024.Search in Google Scholar

Mota, I., Rodrigues Pinto, P.C., Novo, C., Sousa, G., Guerreiro, O., Guerra, A.R., and Rodrigues, A.E. (2012). Extraction of polyphenolic compounds from Eucalyptus globulus bark: process optimization and screening for biological activity. Ind. Eng. Chem. Res. 51: 6991–7000. https://doi.org/10.1021/ie300103z.Search in Google Scholar

Negahdar, L., Delidovich, I., and Palkovits, R. (2016). Aqueous-phase hydrolysis of cellulose and hemicelluloses over molecular acidic catalysts: insights into the kinetics and reaction mechanism. Appl. Catal. B 184: 285–298. https://doi.org/10.1016/j.apcatb.2015.11.039.Search in Google Scholar

Neiva, D.M., Gominho, J., and Pereira, H. (2014). Modeling and optimization of Eucalyptus globulus bark and wood delignification using response surface methodology. Bioresources 9: 2907–2291. https://doi.org/10.15376/biores.9.2.2907-2921.Search in Google Scholar

Neiva, D.M., Gominho, J., Fernandes, L., Lourenço, A., Chemetova, C., Simões, R.M., and Pereira, H. (2016). The potential of hydrothermally pretreated industrial barks from E. globulus as a feedstock for pulp production. J. Wood Chem. Technol. 36: 383–392. https://doi.org/10.1080/02773813.2016.1184280.Search in Google Scholar

Neiva, D.M., Araújo, S., Gominho, J., Carneiro, A.C., and Pereira, H. (2018). Potential of Eucalyptus globulus industrial bark as a biorefinery feedstock: chemical and fuel characterization. Ind. Crop. Prod. 123: 262–270. https://doi.org/10.1016/j.indcrop.2018.06.070.Search in Google Scholar

NREL Laboratory Analytical Procedure (2006). Determination of sugars, byproducts, and degradation products in liquid fraction process samples. Colorado: NREL.Search in Google Scholar

NREL Laboratory Analytical Procedure (2008). Determination of structural carbohydrates and lignin in biomass. Colorado: NREL.Search in Google Scholar

Pásztory, Z., Mohácsiné, I.R., Gorbacheva, G., and Börcsök, Z. (2016). The utilization of tree bark. Bioresources 11: 7859–7888. https://doi.org/10.15376/biores.11.3.pasztory.Search in Google Scholar

Pinto, P.C., Oliveira, C., Costa, C.A., and Rodrigues, A.E. (2016). Performance of side-streams from eucalyptus processing as sources of polysaccharides and lignins by kraft delignification. Ind. Eng. Chem. Res. 55: 516–526. https://doi.org/10.1021/acs.iecr.5b03712.Search in Google Scholar

Rasmussen, H., Sørensen, H.R., and Meyer, A.S. (2014). Formation of degradation compounds from lignocellulosic biomass in the biorefinery: sugar reaction mechanisms. Carbohydr. Res. 385: 45–57. https://doi.org/10.1016/j.carres.2013.08.029.Search in Google Scholar

Ritter, G.J., Mitchell, R.L., and Seboro, R.M. (1933). Some factors that influence the conversion of cellulosic materials to sugar. J. Am. Chem. Soc. 55: 2989–2891. https://doi.org/10.1021/ja01334a063.Search in Google Scholar

Rodríguez-López, J., Romaní, A., González-Muñoz, M.J., Garrote, G., and Parajó, J.C. (2012). Extracting value-added products before pulping: hemicellulosic ethanol from Eucalyptus globulus wood. Holzforschung 66: 591–599. https://doi.org/10.1515/hf-2011-0204.Search in Google Scholar

Romaní, A., Larramendi, A., Yáñez, R., Cancela, Á., Sánchez, Á., Teixeira, J.A., and Domingues, L. (2019). Valorization of Eucalyptus nitens bark by organosolv pretreatment for the production of advanced biofuels. Ind. Crop. Prod. 132: 327–335. https://doi.org/10.1016/j.indcrop.2019.02.040.Search in Google Scholar

Roth, J.C.G., Hoeltz, M., and Benitez, L.B. (2020). Current approaches and trends in the production of microbial cellulases using residual lignocellulosic biomass: a bibliometric analysis of the last 10 years. Arch. Microbiol. 202: 935–951. https://doi.org/10.1007/s00203-019-01796-9.Search in Google Scholar

Ruiz, H.A., Thomsen, M.H., and Trajano, H.L. (2017). Hydrothermal processing in biorefineries. Cham: Springer International Publishing.10.1007/978-3-319-56457-9Search in Google Scholar

Saeman, J.F., Bubl, J.L., and Harris, E.E. (1944). The quantitative saccharification of wood and cellulose. Ind. Eng. Chem. Anal. Ed. 17: 35–37.10.1021/i560137a008Search in Google Scholar

Saeman, J.F., Moore, W.E., Mitchell, R.L., and Millett, M.A. (1954). Techniques for the determination of pulp constituents by quantitative paper chromatography. Tappi J. 37: 336–343.Search in Google Scholar

Selvendran, R.R., March, J.F., and Ring, S.G. (1979). Determination of aldoses and uronic acid content of vegetable fiber. Anal. Biochem. 96: 282–292. https://doi.org/10.1016/0003-2697(79)90583-9.Search in Google Scholar

Shatalov, A.A., Evtuguin, D.V., and Neto, C.P. (1999). 2-O-α-D-galactopyranosyl-4-O-methyl-α-D-glucurono)-D-xylan from Eucalyptus globulus Labill. Carbohydr. Res. 320: 93–99. https://doi.org/10.1016/s0008-6215(99)00136-6.Search in Google Scholar

Sluiter, J.B., Ruiz, R.O., Scarlata, C.J., Sluiter, A.D., and Templeton, D.W. (2010). Compositional analysis of lignocellulosic feedstocks. 1. Review and description of methods. J. Agric. Food Chem. 58: 9043–9053. https://doi.org/10.1021/jf1008023.Search in Google Scholar

Świątek, K., Gaag, S., Klier, A., Kruse, A., Sauer, J., and Steinbach, D. (2020). Acid hydrolysis of lignocellulosic biomass: sugars and furfurals formation. Catalysts 10: 437.10.3390/catal10040437Search in Google Scholar

TAPPI standard (1991). T UM 250. Acid-soluble lignin in wood and pulp. Atlanta: TAPPI.Search in Google Scholar

TAPPI standard (2000). T 249. Cm-00, carbohydrate composition of extractive-free wood and wood pulp by gas-liquid chromatography. Atlanta: TAPPI.Search in Google Scholar

TAPPI standard (2002). T 211. Om-02, ash in wood, pulp, paper and paperboard: combustion at 525 °C. Atlanta: TAPPI.Search in Google Scholar

TAPPI standard (2006). T 222. Om-06, acid-insoluble lignin in wood and pulp. Atlanta: TAPPI.Search in Google Scholar

TAPPI standard (2007). T 204. Cm-97, solvent extractives of wood and pulp. Atlanta: TAPPI.Search in Google Scholar

Templeton, D.W., Wolfrum, E.J., Yen, J.H., and Sharpless, K.E. (2016). Compositional analysis of biomass reference materials: results from an interlaboratory study. Bioenergy Res. 9: 303–314. https://doi.org/10.1007/s12155-015-9675-1.Search in Google Scholar

Tizazu, B.Z. and Moholkar, V.S. (2018). Kinetic and thermodynamic analysis of dilute acid hydrolysis of sugarcane bagasse. Bioresour. Technol. 250: 197–203. https://doi.org/10.1016/j.biortech.2017.11.032.Search in Google Scholar

Zoghlami, A. and Paës, G. (2019). Lignocellulosic biomass: understanding recalcitrance and predicting hydrolysis. Front. Chem. 7: 854. https://doi.org/10.3389/fchem.2019.00874.Search in Google Scholar

Supplementary Material

The online version of this article offers supplementary material (https://doi.org/10.1515/hf-2020-0250).

Received: 2020-11-30
Accepted: 2021-02-24
Published Online: 2021-04-20
Published in Print: 2021-10-26

© 2021 Walter de Gruyter GmbH, Berlin/Boston

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https://doi.org/10.1515/hf-2020-0250
Keywords for this article
bioprocesses; carbohydrate degradation; eucalyptus; hardwood; hydrolysis optimization; process economics

Articles in the same Issue

  1. Frontmatter
  2. Original articles
  3. Ultrasound to estimate the physical-mechanical properties of tropical wood species grown in an agroforestry system
  4. Natural durability and improved resistance of 20 Amazonian wood species after 30 years in ground contact
  5. Cellular-level chemical changes in Japanese beech (Fagus crenata Blume) during artificial weathering
  6. Evaluation of water related properties of birch wood products modified with different molecular weight phenol-formaldehyde oligomers
  7. Superhydrophobic wood surface fabricated by Cu2O nano-particles and stearic acid: its acid/alkali and wear resistance
  8. Dynamic strength properties and structural integrity of wood modified with cyclic N-methylol and N-methyl compounds
  9. Indoor storage time affects the quality and quantity of volatile monoterpenes emitted from softwood timber
  10. The impact of acid hydrolysis conditions on carbohydrate determination in lignocellulosic materials: a case study with Eucalyptus globulus bark
  11. Improved chemical pulping and saccharification of a natural mulberry mutant deficient in cinnamyl alcohol dehydrogenase
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