{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,9,25]],"date-time":"2026-09-25T05:11:59Z","timestamp":1790313119134,"version":"4.1.0"},"reference-count":38,"publisher":"MDPI AG","issue":"5","license":[{"start":{"date-parts":[[2026,2,25]],"date-time":"2026-02-25T00:00:00Z","timestamp":1771977600000},"content-version":"vor","delay-in-days":0,"URL":"https:\/\/creativecommons.org\/licenses\/by\/4.0\/"}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Materials"],"abstract":"<jats:p>Hemp hurds (HHs), a lignocellulosic agricultural waste, have the potential for bioconversion into bio-based products. However, the matrix structure of biomass comprising cellulose, hemicellulose, and lignin makes cellulose inaccessible. Pre-treatment is essential for accessing cellulose by removing lignin, hemicellulose, and extractives. This study compares lignocellulose structure modification of HH using low-concentration chemical pretreatment methods, including organosolvent, 60% ethanol (EtOH), 3% hydrogen peroxide with 3% ammonia (H2O2\/NH3), and 2% sodium hydroxide (NaOH) with sonication. X-ray diffractor (XRD) analysis, using Segal method as a guide, showed that post treatments, the crystallinity index increased from 39.26% in untreated HH to 65.80% for NaOH-treated hurds. Polysaccharide content decreased compared to HH, attributed to the combination of solubilisation of hemicellulose, degradation of amorphous carbohydrates, and loss of sample during treatment wash. Although there was a reduction in polysaccharide content compared to HH, NaOH treated HH showed the highest total carbohydrate content of 48.6% and the most disrupted surface structure, based on scanning electron microscope (SEM) images at 2000\u00d7 magnification. Fourier-transform infrared spectrophotometer (FTIR) analysis indicated a reduction in lignin and hemicellulose peaks for NaOH and H2O2\/NH3 treatments, while thermogravimetric analyser (TGA) and derivative thermogravimetric analysis (DTG) results showed improved thermal stability for NaOH-treated samples. The ultrasound-assisted NaOH-treated sample had the most structural disruption in recovered solid fraction, based on comparative compositional and structural analyses. This gives a guide on the selection of pretreatment to pursue for HH processing.<\/jats:p>","DOI":"10.3390\/ma19050843","type":"journal-article","created":{"date-parts":[[2026,2,25]],"date-time":"2026-02-25T08:50:27Z","timestamp":1772009427000},"page":"843","update-policy":"https:\/\/doi.org\/10.3390\/mdpi_crossmark_policy","source":"Crossref","is-referenced-by-count":5,"title":["Low-Concentration Chemical Pretreatment of Lignocellulose Biomass Derived from Hemp Hurds, Agricultural Waste: Comparative Characterisation of Various Pretreatment Methods"],"prefix":"10.3390","volume":"19","author":[{"ORCID":"https:\/\/orcid.org\/0009-0005-5467-622X","authenticated-orcid":false,"given":"Ziningi Rosebud","family":"Myeni","sequence":"first","affiliation":[{"name":"Technology Transfer and Innovation Directorate, Durban University of Technology, Durban 4000, South Africa"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-3030-6268","authenticated-orcid":false,"given":"Farai","family":"Dziike","sequence":"additional","affiliation":[{"name":"Technology Transfer and Innovation Directorate, Durban University of Technology, Durban 4000, South Africa"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0003-4576-9975","authenticated-orcid":false,"given":"Tshwafo Elias","family":"Motaung","sequence":"additional","affiliation":[{"name":"Department of Chemistry & Chemical Technology, Sefako Makgatho Health Sciences University, Ga-Rankuwa 0204, South Africa"}],"role":[{"vocabulary":"crossref","role":"author"}]},{"ORCID":"https:\/\/orcid.org\/0000-0002-6278-1020","authenticated-orcid":false,"given":"Nirmala","family":"Deenadayalu","sequence":"additional","affiliation":[{"name":"Technology Transfer and Innovation Directorate, Durban University of Technology, Durban 4000, South Africa"}],"role":[{"vocabulary":"crossref","role":"author"}]}],"member":"1968","published-online":{"date-parts":[[2026,2,25]]},"reference":[{"key":"ref_1","doi-asserted-by":"crossref","unstructured":"Haregu, S., Likna, Y., Tadesse, D., and Masi, C. (2023). Recent development of biomass energy as a sustainable energy source to mitigate environmental change. Bioenergy: Impacts on Environment and Economy, Springer.","DOI":"10.1007\/978-981-99-3002-9_8"},{"key":"ref_2","doi-asserted-by":"crossref","first-page":"746","DOI":"10.1039\/D3SU00075C","article-title":"Bio-based agricultural products: A sustainable alternative to agrochemicals for promoting a circular economy","volume":"1","author":"Priya","year":"2023","journal-title":"RSC Sustain."},{"key":"ref_3","doi-asserted-by":"crossref","unstructured":"Guo, J., Zhang, Y., Fang, J., Ma, Z., Li, C., Yan, M., Qiao, N., Liu, Y., and Bian, M. (2024). Reduction and reuse of forestry and agricultural bio-waste through innovative green utilization approaches: A review. Forests, 15.","DOI":"10.3390\/f15081372"},{"key":"ref_4","doi-asserted-by":"crossref","first-page":"174","DOI":"10.17113\/ftb.56.02.18.5428","article-title":"Review of second generation bioethanol production from residual biomass","volume":"56","author":"Robak","year":"2018","journal-title":"Food Technol. Biotechnol."},{"key":"ref_5","doi-asserted-by":"crossref","first-page":"219","DOI":"10.1007\/s42114-024-01009-y","article-title":"Extraction strategies for lignin, cellulose, and hemicellulose to obtain valuable products from biomass","volume":"7","author":"Wang","year":"2024","journal-title":"Adv. Compos. Hybrid Mater."},{"key":"ref_6","doi-asserted-by":"crossref","first-page":"11","DOI":"10.1039\/C8SE00287H","article-title":"Cellulose solvent-based pretreatment for enhanced second-generation biofuel production: A review","volume":"3","author":"Satari","year":"2019","journal-title":"Sustain. Energy Fuels"},{"key":"ref_7","doi-asserted-by":"crossref","first-page":"1550","DOI":"10.1016\/j.tibtech.2022.09.014","article-title":"Creative biological lignin conversion routes toward lignin valorization","volume":"40","author":"Liu","year":"2022","journal-title":"Trends Biotechnol."},{"key":"ref_8","doi-asserted-by":"crossref","first-page":"126376","DOI":"10.1016\/j.ijbiomac.2023.126376","article-title":"Production of fermentable glucose from bioconversion of cellulose using efficient microbial cellulases produced from water hyacinth waste","volume":"252","author":"Tripathi","year":"2023","journal-title":"Int. J. Biol. Macromol."},{"key":"ref_9","doi-asserted-by":"crossref","unstructured":"Yuan, W., Du, Y., Yu, K., Xu, S., Liu, M., Wang, S., Yang, Y., Zhang, Y., and Sun, J. (2022). The production of pyruvate in biological technology: A critical review. Microorganisms, 10.","DOI":"10.3390\/microorganisms10122454"},{"key":"ref_10","doi-asserted-by":"crossref","unstructured":"Sharma, S., Tsai, M.-L., Sharma, V., Sun, P.-P., Nargotra, P., Bajaj, B.K., Chen, C.-W., and Dong, C.-D. (2022). Environment friendly pretreatment approaches for the bioconversion of lignocellulosic biomass into biofuels and value-added products. Environments, 10.","DOI":"10.3390\/environments10010006"},{"key":"ref_11","doi-asserted-by":"crossref","first-page":"6155","DOI":"10.1007\/s13399-022-02981-5","article-title":"Pretreatment of agricultural lignocellulosic biomass for fermentable sugar: Opportunities, challenges, and future trends","volume":"14","author":"Alawad","year":"2024","journal-title":"Biomass Convers. Biorefinery"},{"key":"ref_12","unstructured":"Rashid, M.H. (2016). 8\u2014Utilization of bioresources as fuels and energy generation. Electric Renewable Energy Systems, Academic Press."},{"key":"ref_13","doi-asserted-by":"crossref","first-page":"48928","DOI":"10.1007\/s11356-024-34473-6","article-title":"Chemical approaches for the biomass valorisation: A comprehensive review of pretreatment strategies","volume":"31","author":"Joshi","year":"2024","journal-title":"Environ. Sci. Pollut. Res."},{"key":"ref_14","doi-asserted-by":"crossref","first-page":"44","DOI":"10.1186\/s13068-023-02295-2","article-title":"Strategies of pretreatment of feedstocks for optimized bioethanol production: Distinct and integrated approaches","volume":"16","author":"Shukla","year":"2023","journal-title":"Biotechnol. Biofuels Bioprod."},{"key":"ref_15","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1080\/08827508.2024.2410287","article-title":"A comprehensive review on evolution behavior of particle size distribution during fine grinding process for optimized separation purposes","volume":"47","author":"Guo","year":"2024","journal-title":"Miner. Process. Extr. Metall. Rev."},{"key":"ref_16","doi-asserted-by":"crossref","first-page":"5317","DOI":"10.1007\/s13399-021-01506-w","article-title":"Biological pretreatment improved subsequent xylan chemical solubilization","volume":"13","author":"Felipuci","year":"2023","journal-title":"Biomass Convers. Biorefinery"},{"key":"ref_17","doi-asserted-by":"crossref","unstructured":"Shah, A.A., Seehar, T.H., Sharma, K., and Toor, S.S. (2022). Biomass pretreatment technologies. Hydrocarbon Biorefinery, Elsevier.","DOI":"10.1016\/B978-0-12-823306-1.00014-5"},{"key":"ref_18","doi-asserted-by":"crossref","first-page":"451","DOI":"10.3390\/waste2040024","article-title":"Physical\u2013Chemical\u2013Biological Pretreatment for Biomass Degradation and Industrial Applications: A Review","volume":"2","author":"Chen","year":"2024","journal-title":"Waste"},{"key":"ref_19","doi-asserted-by":"crossref","first-page":"771","DOI":"10.1080\/10643389.2023.2277670","article-title":"Biological pretreatment of lignocellulosic biomass: An environment-benign and sustainable approach for conversion of solid waste into value-added products","volume":"54","author":"Anu","year":"2024","journal-title":"Crit. Rev. Environ. Sci. Technol."},{"key":"ref_20","doi-asserted-by":"crossref","first-page":"13895","DOI":"10.1007\/s13762-023-04838-4","article-title":"Pre-treatment of lignocellulosic biomass: Review of various physico-chemical and biological methods influencing the extent of biomass depolymerization","volume":"20","author":"Baksi","year":"2023","journal-title":"Int. J. Environ. Sci. Technol."},{"key":"ref_21","first-page":"104","article-title":"Pretreatment Methods for Lignocellulosic-Based Biomass to Provide Sustainable Biofuel and Environmental Benefits. A Review","volume":"45","author":"Karamat","year":"2027","journal-title":"Port. Electrochim. Acta"},{"key":"ref_22","doi-asserted-by":"crossref","unstructured":"Gladysheva, E.K. (2025). Liquid Hot Water and Steam Explosion Pretreatment Methods for Cellulosic Raw Materials: A Review. Polymers, 17.","DOI":"10.3390\/polym17131783"},{"key":"ref_23","doi-asserted-by":"crossref","first-page":"1115","DOI":"10.18331\/BRJ2020.7.1.4","article-title":"Pretreatment methods for lignocellulosic biofuels production: Current advances, challenges and future prospects","volume":"7","author":"Cheah","year":"2020","journal-title":"Biofuel Res. J."},{"key":"ref_24","doi-asserted-by":"crossref","first-page":"350","DOI":"10.1021\/ac60111a017","article-title":"Colorimetric Method for Determination of Sugars and Related Substances","volume":"28","author":"Dubois","year":"1956","journal-title":"Anal. Chem."},{"key":"ref_25","doi-asserted-by":"crossref","first-page":"92","DOI":"10.1016\/j.apenergy.2017.08.076","article-title":"Characterization of char from biomass gasification and its similarities with activated carbon in adsorption applications","volume":"227","author":"Benedetti","year":"2018","journal-title":"Appl. Energy"},{"key":"ref_26","doi-asserted-by":"crossref","first-page":"82","DOI":"10.1016\/j.joei.2017.11.003","article-title":"Characterization of the physicochemical and structural evolution of biomass particles during combined pyrolysis and CO2 gasification","volume":"92","author":"Eshun","year":"2019","journal-title":"J. Energy Inst."},{"key":"ref_27","doi-asserted-by":"crossref","first-page":"1","DOI":"10.1016\/j.carbpol.2015.08.035","article-title":"Segal crystallinity index revisited by the simulation of X-ray diffraction patterns of cotton cellulose I\u03b2 and cellulose II","volume":"135","author":"Nam","year":"2016","journal-title":"Carbohydr. Polym."},{"key":"ref_28","doi-asserted-by":"crossref","first-page":"100186","DOI":"10.1016\/j.biteb.2019.100186","article-title":"A comparative study of thermochemical characteristics of lignocellulosic biomasses","volume":"8","author":"Kumar","year":"2019","journal-title":"Bioresour. Technol. Rep."},{"key":"ref_29","doi-asserted-by":"crossref","first-page":"122440","DOI":"10.1016\/j.indcrop.2025.122440","article-title":"Natural deep eutectic solvent for cellulose isolation from almond shell powder: A sustainable approach for by-product valorization","volume":"239","author":"Simal","year":"2026","journal-title":"Ind. Crops Prod."},{"key":"ref_30","doi-asserted-by":"crossref","first-page":"110030","DOI":"10.1016\/j.lwt.2020.110030","article-title":"Rhizopus oligosporus as a biotransforming microorganism of Anacardium othonianum Rizz. byproduct for production of high-protein, -antioxidant, and -fiber ingredient","volume":"135","author":"Lima","year":"2021","journal-title":"LWT"},{"key":"ref_31","doi-asserted-by":"crossref","first-page":"114884","DOI":"10.1016\/j.indcrop.2022.114884","article-title":"Reliable and realistic models for lignin content determination in poplar wood based on FT-Raman spectroscopy","volume":"182","author":"Gao","year":"2022","journal-title":"Ind. Crops Prod."},{"key":"ref_32","doi-asserted-by":"crossref","first-page":"100214","DOI":"10.1016\/j.bamboo.2025.100214","article-title":"Comprehensive characterization of Bengal bamboo (Bambusa tulda Roxb.) for advanced material applications: Physical, mechanical, thermal and microstructural insights","volume":"13","author":"Reddy","year":"2025","journal-title":"Adv. Bamboo Sci."},{"key":"ref_33","doi-asserted-by":"crossref","first-page":"116494","DOI":"10.1016\/j.carbpol.2020.116494","article-title":"Study on a Novel natural cellulosic fiber from Kigelia africana fruit: Characterization and analysis","volume":"244","author":"Siva","year":"2020","journal-title":"Carbohydr. Polym."},{"key":"ref_34","doi-asserted-by":"crossref","first-page":"145035","DOI":"10.1016\/j.ijbiomac.2025.145035","article-title":"Hemp-based lignocellulosic mass as a basis for producing textile fibers","volume":"318","author":"Makarov","year":"2025","journal-title":"Int. J. Biol. Macromol."},{"key":"ref_35","doi-asserted-by":"crossref","first-page":"116706","DOI":"10.1016\/j.carbpol.2020.116706","article-title":"Isolation and characterization of cellulose nanocrystals from Cucumis sativus peels","volume":"247","author":"Prasanna","year":"2020","journal-title":"Carbohydr. Polym."},{"key":"ref_36","doi-asserted-by":"crossref","first-page":"151","DOI":"10.1016\/S0964-8305(03)00052-0","article-title":"FTIR studies of the changes in wood chemistry following decay by brown-rot and white-rot fungi","volume":"52","author":"Pandey","year":"2003","journal-title":"Int. Biodeterior. Biodegrad."},{"key":"ref_37","doi-asserted-by":"crossref","unstructured":"Khumalo, N.L., Mohomane, S.M., and Motaung, T.E. (2024). Effect of Acetylation on the Morphology and Thermal Properties of Maize Stalk Cellulose Nanocrystals: A Comparative Study of Green-Extracted CNC vs. Acid Hydrolysed Followed by Acetylation. Crystals, 14.","DOI":"10.3390\/cryst14070636"},{"key":"ref_38","doi-asserted-by":"crossref","first-page":"26198","DOI":"10.1038\/s41598-025-10950-x","article-title":"Effect of synthesized silica on the properties of sugarcane bagasse cellulose\/silica nanocomposites via sol\u2013gel processing","volume":"15","author":"Shange","year":"2025","journal-title":"Sci. Rep."}],"container-title":["Materials"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/www.mdpi.com\/1996-1944\/19\/5\/843\/pdf","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2026,2,25]],"date-time":"2026-02-25T09:02:43Z","timestamp":1772010163000},"score":1,"resource":{"primary":{"URL":"https:\/\/www.mdpi.com\/1996-1944\/19\/5\/843"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2026,2,25]]},"references-count":38,"journal-issue":{"issue":"5","published-online":{"date-parts":[[2026,3]]}},"alternative-id":["ma19050843"],"URL":"https:\/\/doi.org\/10.3390\/ma19050843","relation":{},"ISSN":["1996-1944"],"issn-type":[{"value":"1996-1944","type":"electronic"}],"subject":[],"published":{"date-parts":[[2026,2,25]]}}}