Characterization of Diluted-acid Pretreatment of Water Hyacinth

Main Article Content

Auangfa Boontum
Jirapa Phetsom
Wawat Rodiahwati
Kanyarat Kitsubthawee
Teerachai Kuntothom


Water hyacinth (WH) is an abundant renewable lignocellulosic biomass. The renewable resources are widely studied to produce bioenergy and high value added products. The obstacle of converting the lignocellulosic biomass to products due to its recalcitrant structure, required disruption to enhance the chemical or enzyme accessibility. The aim of this study is to investigate the possibility of WH pretreatment with dilute sulfuric acid (DSA). The addition of sulfuric acid in pretreatment process was varied concentration at 1, 2, 3, and 4% (v/v). The chemical component was analyzed to optimize the pretreatment condition. The results showed that the 2% sulfuric acid had effect on cellulose recovery. The morphological changes of WH due to pretreatment were determined by Scanning Electron Microscopy (SEM). The images showed the destructive surface of all treated samples. The intact surface of native WH was destroyed after pretreatment process while the increment of acid concentration increased the rough surfaces. The Fourier Transform Infrared Spectrometer (FTIR) and X-ray diffraction (XRD) were used for analyzing functional groups and crystallinity, respectively. The FTIR patterns of DSA treated WH were slightly different due to the remained components in samples. The results showed the highest crystallinity index was 55% which was obtained from pretreated WH with 2% sulfuric acid, 80°C, 60 min. In the present study, it was found that DSA pretreatment is possible to modify the chemical structure of WH for developing economical processes.

Article Details

How to Cite
Boontum, A., Phetsom, J., Rodiahwati, W., Kitsubthawee, K., & Kuntothom, T. (2019). Characterization of Diluted-acid Pretreatment of Water Hyacinth. Applied Science and Engineering Progress, 12(4), 253–263. Retrieved from
Research Articles


[1] L. Gao and B. Li, “The study of a specious invasive plant, water hyacinth (Eichhornia crassipes): Achievements and challenges,” Acta-Phytoecologica- Sinica, vol. 28, pp. 735–752, 2004.

[2] D. C. Schmitz, J. D. Schardt, A. G. Leslie, F. A. Dray, J. A. Osborne, and B.V. Nelson, “The ecological impact and management history of three invasive alien aquatic plants in Florida,” in Biological Pollution the Control and Impact of Invasive Exotic Species. Indiana: Indiana Academy of Science, 1993, pp. 261.

[3] S. Dandelot, C. Robles, N. Pech, A. Cazaubon, and R. Verlaque, “Allelopathic potential of two invasive alien Ludwigia spp,” Aquatic Botany, vol. 88, pp. 311–316, 2008.

[4] A. K. Forrest, J. Hernandez, and M. T. Holtzapple, “Effects of temperature and pretreatment conditions on mixed acid fermentation of water hyacinth using a mixed culture of thermophilic microorganisms,” Bioresource Technology, vol. 10, pp. 7510–7515, 2010.

[5] R. Sindhu, P. Binod, A. Pandey, A. Madhavan, J. A. Alphonsa, N. Vivek, E. Gnansounou, E. Castro, and V. Faraco, “Water hyacinth a potential source for value addition: An overview,” Bioresource Technology, vol. 230, pp. 152–162, 2017.

[6] P. Bathla, “Phytoremediation of metals contaminated distillery effluent using water hyacinth (Eichhornia crassipes),” International Journal of Latest Technology in Engineering, Management & Applied Science, vol. 4, pp. 283–290, 2016.

[7] K. Blessy and M. L. Prabha, “Application of water hyacinth vermicompost on the growth of Capsicum annum,” International Journal of Pharmaceutical Sciences and Research, vol. 5, pp. 198–203, 2014.

[8] S. Vidya and L. Girish, “Water hyacinth as a green manure for organic farming,” International Journal of Research in Applied, Natural and Social Sciences, vol. 2, no. 6, pp. 65–72, 2014.

[9] A. B. Pitaloka, H. S. Asep, and N. Mohammad, “Water hyacinth for superabsorbent polymer material,” World Applied Sciences Journal, vol. 22, no. 5, pp. 747–754, 2013.

[10] K. Alagu, H. Venu, J. Jayaraman, V. D. Raju, L. Subramani, P. Appavu, and S. Dhanasekar, “Novel water hyacinth biodiesel as a potential alternative fuel for existing unmodified diesel engine: Performance, combustion and emission characteristics,” Energy, vol. 179, pp. 295–305, 2019.

[11] H. Venu, D. Venkataraman, P. Purushothaman, and D. R. Vallapudi, “Eichhornia crassipes biodiesel as a renewable green fuel for diesel engine applications: Performance, combustion, and emission characteristics,” Environmental Science and Pollution Research, pp. 1–14, 2019.

[12] V. B. Barua and A. S. Kalamdhad, “Biogas production from water hyacinth in a novel anaerobic digester: A continuous study,” Process Safety and Environmental Protection, vol. 127, pp. 82–89, 2019.

[13] I. Sunwoo, J. E. Kwon, T. H. Nguyen, G. T. Jeong, and S. K. Kim, “Ethanol production from water hyacinth (Eichhornia crassipes) hydrolysate by hyper-thermal acid hydrolysis, enzymatic saccharification and yeasts adapted to high concentration of xylose,” Bioprocess and Biosystems Engineering, pp. 1–8, 2019.

[14] S. Rezania, M. F. M. Din, S. F. Kamaruddin, S. M. Taib, L. Singh, E. L. Yong, and F. A. Dahalan, “Evaluation of water hyacinth (Eichhornia crassipes) as a potential raw material source for briquette production,” Energy, vol. 111, pp. 768–773, 2016.

[15] A. Kumar, L. K. Singh, and S. Ghosh, “Bioconversion of lignocellulosic fraction of water hyacinth (Eichhornia crassipes) hemicellulose acid hydrolysate to ethanol by Pichia stipitis,” Bioresour Technology, vol. 100, pp. 3293–3297, 2009.

[16] A. M. Boudet, S. Kajita, J. Grima-Pettenati, and D. Goffner, “Lignins and lignocellulosics: A better control of synthesis for new and improved uses,” Trends in Plant Science, vol. 8, no. 12, pp. 576–581. 2003.

[17] A. D. Moreno, E. Tomás-Pejó, M. Ballesteros, and M. J. Negro, “Pretreatment technologies for lignocellulosic biomass deconstruction within a biorefinery perspective,” in Biofuels: Alternative Feedstocks and Conversion Processes for the Production of Liquid and Gaseous Biofuels. Massachusetts: Academic Press, 2019, pp. 379–399.

[18] N. Mosier, C. Wyman, B. Dale, R. Elander, Y. Y. Lee, M. Holtzapple, and M. Ladisch, “Features of promising technologies for pretreatment of lignocellulosic biomass,” Bioresource Technology, vol. 96, no. 6, pp. 673–686, 2005.

[19] W. Rodiahwati and M. Sriariyanun, “Lignocellulosic biomass to biofuel production: Integration of chemical and extrusion (screw press) pretreatment,” KMUTNB Int J Appl Sci Technol, vol. 9, no. 4, pp. 289–298, 2016.

[20] E. Tomás-Pejó, P. Alvira, M. Ballesteros, and M. J. Negro, “Pretreatment technologies for lignocellulose-to-bioethanol conversion,” in Biofuels. Massachusetts: Academic press, 2011, pp. 149–176.

[21] N. Srivastava, R. Rawat, H. Singh Oberoi, and P. W. Ramteke, “A review on fuel ethanol production from lignocellulosic biomass,” International Journal of Green Energy, vol. 12, no. 9, pp. 949–960, 2015.

[22] M. Narra, J. Divecha, D. Shah, V. Balasubramanian, B. Vyas, M. Harijan, and K. Macwan, “Cellulase production, simultaneous saccharification and fermentation in a single vessel: A new approach for production of bio-ethanol from mild alkali pretreated water hyacinth,” Journal of Environmental Chemical Engineering, vol. 5, no. 3, pp. 2176– 2181, 2017.

[23] S. Y. Yoon, B. R. Kim, S. H. Han, and S. J. Shin, “Different response between woody core and bark of goat willow (Salix caprea L.) to concentrated phosphoric acid pretreatment followed by enzymatic saccharification,” Energy, vol. 81, pp. 21–26, 2015.

[24] P. Amnuaycheewa, R. Hengaroonprasan, K. Rattanaporn, S. Kirdponpattara, K. Cheenkachorn, and M. Sriariyanun, “Enhancing enzymatic hydrolysis and biogas production from rice straw by pretreatment with organic acids,” Industrial Crops and Products, vol. 87, pp. 247–254, 2016.

[25] P. Amnuaycheewa, W. Rodiahwati, P. Sanvarinda, K. Cheenkachorn, A. Tawai, and M. Sriariyanun, “Effect of organic acid pretreatment on Napier grass (Pennisetum purpureum) straw biomass conversion,” KMUTNB Int J Appl Sci Technol, vol. 10, no. 2, pp. 107–117, 2017.

[26] K. Rattanaporn, P. Tantayotai, T. Phusantisampan, P. Pornwongthong, and M. Sriariyanun, “Organic acid pretreatment of oil palm trunk: Effect on enzymatic saccharification and ethanol production,” Bioprocess and Biosystems Engineering, vol. 41, no. 4, pp. 467–477, 2018.

[27] N. Junnienkul, M. Sriariyanun, T. Douzou, P. Yasurin, and S. Asavasanti, “Optimization of alkyl imidazolium chloride pretreatment on rice straw biomass conversion,” KMUTNB Int J Appl Sci Technol, vol. 11, no. 3, pp. 199–207, 2018.

[28] J. Gao, L. Chen, Z. Yan, and L. Wang, “Effect of ionic liquid pretreatment on the composition, structure and biogas production of water hyacinth (Eichhornia crassipes),” Bioresource Technology, vol. 132, pp. 361–364, 2013.

[29] R. Alayoubi, N. Mehmood, E. Husson, A. Kouzayha, M. Tabcheh, L. Chaveriat, and I. Gosselin, “Low temperature ionic liquid pretreatment of lignocellulosic biomass to enhance bioethanol yield,” Renewable Energy, vol. 145, pp. 1808–1816, 2020.

[30] Z. Zhang, I. M. O’Hara, and W. O. Doherty, “Pretreatment of sugarcane bagasse by acid-catalysed process in aqueous ionic liquid solutions,” Bioresource Technology, vol. 120, pp. 149–156, 2012.

[31] P. Engel, R. Mladenov, H. Wulfhorst, G. Jäger, and A. C. Spiess, “Point by point analysis: How ionic liquid affects the enzymatic hydrolysis of native and modified cellulose,” Green Chemistry, vol. 12, no. 11, pp. 1959–1966, 2010.

[32] R. Akkharasinphonrat, T. Douzou, and M. Sriariyanun, “Development of ionic liquid utilization in biorefinery process of lignocellulosic biomass.” KMUTNB Int J Appl Sci Technol, vol. 10, no. 2, pp. 89–96, 2017.

[33] P. F. H. Harmsen, W. Huijgen, L. Bermudez, and R. Bakker, “Literature review of physical and chemical pretreatment processes for lignocellulosic biomass,” Wageningen UR-Food & Biobased Research, Wageningen, Nederland, Rep. 1184, Sep. 2010.

[34] Y. H. Jung and K. H. Kim, “Acidic pretreatment.” in Pretreatment of Biomass. Amsterdam, Nederland: Elsevier, 2015, pp. 27–50.

[35] J. C. Solarte-Toro, J. M. Romero-García, J. C. Martínez-Patiño, E. Ruiz-Ramos, E. Castro- Galiano, and C. A. Cardona-Alzate, “Acid pretreatment of lignocellulosic biomass for energy vectors production: A review focused on operational conditions and techno-economic assessment for bioethanol production,” Renewable and Sustainable Energy Reviews, vol. 107, pp. 587–601, 2019.

[36] Y. Chen, R. R. Sharma-Shivappa, D. Keshwani, and C. Chen, “Potential of agricultural residues and hay for bioethanol production,” Applied Biochemistry and Biotechnology, vol. 142, no. 3, pp. 276–290, 2007.

[37] C. Li, B. Knierim, C. Manisseri, R. Arora, H. V. Scheller, M. Auer, K. P. Vogel, B. A. Simmons, and S. Singh, “Comparison of dilute acid and ionic liquid pretreatment of switchgrass: Biomass recalcitrance, delignification and enzymatic saccharification,” Bioresource Technology, vol. 101, no.13, pp. 4900–4906, 2010.

[38] A. Duque, P. Manzanares, I. Ballesteros, and M. Ballesteros, “Steam explosion as lignocellulosic biomass pretreatment,” in Biomass Fractionation Technologies for a Lignocellulosic Feedstock Based Biorefinery. Amsterdam, Nederland: Elsevier, 2016.

[39] P. Manzanares, I. Ballesteros, M. J. Negro, A. González, J. M. Oliva, and M. Ballesteros, “Processing of extracted olive oil pomace residue by hydrothermal or dilute acid pretreatment and enzymatic hydrolysis in a biorefinery context.” Renewable Energy, vol. 145, pp. 1235–1245, 2020.

[40] A. S. Patri, L. McAlister, C. M. Cai, R. Kumar, and C. E. Wyman, “CELF significantly reduces milling requirements and improves soaking effectiveness for maximum sugar recovery of Alamo switchgrass over dilute sulfuric acid pretreatment,” Biotechnology for Biofuels, vol. 12, no. 1, pp. 1–11, 2019.

[41] T. C. Hsu, G. L. Guo, W. H. Chen, and W. S. Hwang, “Effect of dilute acid pretreatment of rice straw on structural properties and enzymatic hydrolysis,” Bioresource Technology, vol. 101, no. 13, pp. 4907–4913, 2010.

[42] Z. Yu, Y. Du, X. Shang, Y. Zheng, and J. Zhou, “Enhancing fermentable sugar yield from cassava residue using a two-step dilute ultra-low acid pretreatment process,” Industrial Crops and Products, vol. 124, pp. 555–562, 2018.

[43] M. Kuglarz, M. Alvarado-Morales, K. Dąbkowska, and I. Angelidaki, “Integrated production of cellulosic bioethanol and succinic acid from rapeseed straw after dilute-acid pretreatment,” Bioresource Technology, vol. 265, pp. 191–199, 2018.

[44] H. B. Klinke, A. B. Thomsen, and B. K. Ahring, “Inhibition of ethanol-producing yeast and bacteria by degradation products produced during pre-treatment of biomass,” Applied Microbiology and Biotechnology, vol. 66, no. 1, pp. 10–26, 2004.

[45] M. Cantarella, L. Cantarella, A. Gallifuoco, A. Spera, and F. Alfani, “Effect of inhibitors released during steam-explosion treatment of poplar wood on subsequent enzymatic hydrolysis and SSF,” Biotechnology Progress, vol. 20, no. 1, pp. 200–206, 2004.

[46] S. Sarto, R. Hildayati, and I. Syaichurrozi, “Effect of chemical pretreatment using sulfuric acid on biogas production from water hyacinth and kinetics,” Renewable Energy, vol. 132, pp. 335–350, 2019.

[47] P. J. Van Soest, J. B. Robertson, and B. A. Lewis, “Methods for dietary fiber, neutral detergent fiber, and nonstarch polysaccharides in relation to animal nutrition,” Journal of Dairy Science, vol. 74, no. 10, pp. 3583–3597, 1991.

[48] L. Segal, J. J. Greely, A. E. J. Martin, and L. M. Conrad, “An empirical method for estimating the degree of crystallinity of native cellulose using X-ray diffractometer,” Textile Research Journal, vol. 29, pp. 780–794, 1959.

[49] S. Rezania, M. F. Md Din, S. M. Taib, J. Sohaili, S. Chelliapan, H. Kamyab, and B. B. Saha, “Review on fermentative biohydrogen production from water hyacinth, wheat straw and rice straw with focus on recent perspectives,” International Journal of Hydrogen Energy, vol. 42, no. 33, pp. 20955–20969, 2017.

[50] A. Singh and N. R. Bishnoi, “Comparative study of various pretreatment techniques for ethanol production from water hyacinth,” Industrial Crops and Products, vol. 44, pp. 283–289, 2013.

[51] S. Rezania, H. Alizadeh, J. Cho, N. Darajeh, J. Park, B. Hashemi, M. F. M. Din, S. Krishnan, K. K. Yadav, N. Gupta, and S. Kumar, “Changes in composition and structure of water hyacinth based on various pretreatment methods,” BioResources, vol. 14, no. 3, pp. 6088–6099, 2019.

[52] A. Singh, N. Singh, and N. R. Bishnoi, “Enzymatic hydrolysis of chemically pretreated rice straw by two indigenous fungal strains: A comparative study.” Journal of Scientific and Industrial Research, vol. 69, pp. 232–237, 2010.

[53] V. B. Barua and A. S. Kalamdhad, “Effect of various types of thermal pretreatment techniques on the hydrolysis, compositional analysis and characterization of water hyacinth,” Bioresource Technology, vol. 227, pp. 147–154, 2017.

[54] J. Li, G. Henriksson, and G. Gellerstedt, “Lignin depolymerization/ repolymerization and its critical role for delignification of aspen wood by steam explosion,” Bioresource Technology, vol. 98, pp. 3061– 3068, 2007.

[55] R. Kumar, G. Mago, V. Balan, and C. E. Wyman, “Physical and chemical characterizations of corn stover and poplar solids resulting from leading pretreatment technologies,” Bioresource Technology, vol. 100, no. 17, pp. 3948–3962, 2009.

[56] I. Kamdem, N. Jacquet, F. M. Tiappi, S. Hiligsmann, C. Vanderghem, A. Richel, P. Jacques, and P. Thonart, “Comparative biochemical analysis after steam pretreatment of lignocellulosic agricultural waste biomass from Williams Cavendish banana plant (Triploid Musa AAA group),” Waste Management and Research, vol. 33, no. 11, pp. 1022–1032. 2015.

[57] A. Xia, J. Cheng, R. Lin, J. Liu, J. Zhou, and K. Cen, “Sequential generation of hydrogen and methane from glutamic acid through combined photofermentation and methanogenesis,” Bioresource Technology, vol. 131, pp. 146–151, 2013.

[58] B. Sornvoraweat and J. Kongkiattikajorn, “Separated hydrolysis and fermentation of water hyacinth leaves for ethanol production,” Asia- Pacific Journal of Science and Technology, vol. 15, no. 9, pp. 794–802. 2010.

[59] J. G. Reales-Alfaro, L. T. Trujillo-Daza, G. Arzuaga-Lindado, H. I. Castaño-Peláez, and Á. D. Polo-Córdoba, “Acid hydrolysis of water hyacinth to obtain fermentable sugars,” CT&FCiencia Tecnologíay Futuro, vol. 5, no. 2, pp. 101–111, 2013.

[60] S. Kumari and D. Das, “Biohythane production from sugarcane bagasse and water hyacinth: A way towards promising green energy production,” Journal of cleaner production, vol. 207, pp. 689–701. 2019.

[61] B. T. N. Thi, L. K. Ong, D. T. N. Thi, and Y.-H. Ju, “Effect of subcritical water pretreatment on cellulose recovery of water hyacinth (Eichhornia crassipe),” Journal of the Taiwan Institute of Chemical Engineers, vol. 71, pp. 55–61, 2017.

[62] K. Satyanagalakshmi, R. Sindhu, P. Binod, K. U. Janu, R. K. Sukumaran, and A. Pandey, “Bioethanol production from acid pretreated water hyacinth by separate hydrolysis and fermentation,” Journal of Scientific & Industrial Research, vol. 70, pp. 156–161, 2011.

[63] A. Goshadrou, K. Karimi, and M. J. Taherzadeh, “Improvement of sweet sorghum bagasse hydrolysis by alkali and acidic pretreatments,” Bioenergy Technology, pp. 374–380, 2011.

[64] D. Fu, G. Mazza, and Y. Tamaki, “Lignin extraction from straw by ionic liquids and enzymatic hydrolysis of the cellulosic residues,” Journal of Agricultural and Food Chemistry, vol. 58, pp. 2915–2922, 2010.

[65] M. Kačuráková, A. Ebringerova, J. Hirsch, and Z. Hromadkova, “Infrared study of arabinoxylans,” Journal of the Science of Food and Agriculture, vol. 66, no. 3, pp. 423–427, 1994.

[66] R. C. Sun, J. Tomkinson, P. L. Ma, and S. F. Liang, “Comparative study of hemicelluloses from rice straw by alkali and hydrogen peroxide treatments,” Carbohydrate Polymers, vol. 42, no. 2, pp. 111–122, 2000.

[67] R. C. Sun and J. Tomkinson, “Characterization of hemicelluloses obtained by classical and ultrasonically assisted extractions from wheat straw,” Carbohydrate Polymers, vol. 50, no. 3, pp. 263–271, 2002.

[68] G. N. Juárez-Luna, E. Favela-Torres, I. R. Quevedo, and N. Batina, “Enzymatically assisted isolation of high-quality cellulose nanoparticles from water hyacinth stems,” Carbohydrate Polymers, vol. 220, pp.110–117, 2019.

[69] C. Li, B. Knierim, C. Manisseri, R. Arora, H. V. Scheller, M. Auer, K. P. Vogel, B. A. Simmon, and S. Singh, “Comparison of dilute acid and ionic liquid pretreatment of switchgrass: Biomass recalcitrance, delignification and enzymatic saccharification,” Bioresource Technology, vol. 101, no. 13, 4900–4906. 2010.

[70] I. Ballesteros, M. Ballesteros, P. Manzanares, M. J. Negro, J. M. Oliva, and F. Sáez, “Dilute sulfuric acid pretreatment of cardoon for ethanol production,” Biochemical Engineering Journal, vol. 42, no. 1, pp. 84–91, 2008.

[71] M. T. Sundari and A. Ramesh, “Isolation and characterization of cellulose nanofibers from the aquatic weed water hyacinth - Eichhornia crassipes,” Carbohydrate Polymers, vol. 87, no. 2, pp. 1701–1705, 2012.

[72] K. Karimi and M. J. Taherzadeh, “A critical review of analytical methods in pretreatment of lignocelluloses: Composition, imaging, and crystallinity,” Bioresource Technology, vol. 200, pp. 1008–1018, 2016.

[73] E. Abraham, B. Deepa, L. A. Pothan, M. Jacob, S. Thomas, and U. Cvelbar, and R. Anandjiwala, “Extraction of nanocellulose fibrils from lignocellulosic fibres: A novel approach,” Carbohydrate Polymers, vol. 86, pp. 1468–1475, 2011.

[74] F. Fahma, S. Iwamoto, N. Hori, T. Iwata, and A. Takemura, “Effect of pre-acid-hydrolysis treatment on morphology and properties of cellulose nanowhiskers from coconut husk,” Cellulose, vol. 18, pp. 443–450, 2011.

[75] R. Kumar, G. Mago, V. Balan, and C. E. Wyman, “Physical and chemical characterizations of corn stover and poplar solids resulting from leading pretreatment technologies,” Bioresource Technology, vol. 100, no. 17, pp. 3948–3962, 2009.