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Synthesis and Investigation of Alternative Solvents for Dissolution and Analysis of Biomass by NMR
ID Pečovnik Wutt, Naja (Author), ID Jereb, Marjan (Mentor) More about this mentor... This link opens in a new window, ID Petrovski, Željko (Comentor)

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Abstract
Biomass, derived from plants, consists primarily of cellulose, hemicellulose, and lignin. These building blocks of plant and algae cell walls have the potential to be used if separated into individual components. The applications could include the production of value-added chemicals and materials. Finding efficient solvent systems that are at the same time environmentally friendly and easily available could maximize the utility of biomass in diverse industrial and research contexts. This research explores alternative solvents for dissolving biomass, focusing on eutectic solvents such as guanidinium salts: urea (1:2) in combination with other suitable compounds to enable detailed NMR analysis. The guanidinium thiocyanate-urea eutectic mixture was synthesized and confirmed through ATR-FTIR analysis, which validated the presence of intermolecular interactions. Although it was not effective for dissolving cellulose on its own, its combination with DMSO and guanidine enhanced solubilization. A 1H NMR analysis of D-glucose revealed that the solvent system was suitable for small carbohydrates. However, cellulose samples generated low-resolution spectra. In contrast, glucomannan (a type of hemicellulose) dissolved more efficiently, particularly in eutectic mixtures with DMSO-d6 or deuterium oxide, which produced higher quality NMR spectra. While the initial efforts to dissolve cellulose were unsuccessful, the focus shifted to hemicellulose dissolution, demonstrating that various solvent systems could effectively aid in this process.

Language:English
Keywords:Eutectic solvent, Guanidinium thiocyanate, Urea, Cellulose and Hemicellulose dissolution, NMR spectroscopy
Work type:Bachelor thesis/paper
Typology:2.11 - Undergraduate Thesis
Organization:FKKT - Faculty of Chemistry and Chemical Technology
Year:2025
PID:20.500.12556/RUL-170201 This link opens in a new window
COBISS.SI-ID:243806723 This link opens in a new window
Publication date in RUL:02.07.2025
Views:194
Downloads:43
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Secondary language

Language:Slovenian
Title:Sinteza in raziskava nadomestnih topil za raztapljanje in analizo biomase z jedrsko magnetno resonanco (NMR)
Abstract:
Biomasa, pridobljena iz rastlin, je sestavljena predvsem iz celuloze, hemiceluloze in lignina. Te gradnike celičnih sten rastlin in alg bi bilo mogoče uporabiti, če jih ločimo na posamezne komponente. Možne uporabe vključujejo proizvodnjo kemikalij in materialov z dodano vrednostjo. Učinkoviti topilni sistemi, ki so hkrati okolju prijazni in lahko dostopni, bi lahko povečali uporabnost biomase v različnih industrijskih in raziskovalnih kontekstih. Ta raziskava preučuje alternativna topila za raztapljanje biomase, s poudarkom na evtektičnih topilih, kot so gvanidinske soli: urea (v razmerju 1:2) v kombinaciji z drugimi ustreznimi spojinami, ki omogočajo podrobno NMR-analizo. Evtektična zmes gvanidinijovega tiocianata in uree je bila sintetizirana in potrjena z ATR-FTIR-analizo, ki je potrdila prisotnost intermolekularnih interakcij. Čeprav sama po sebi ni bila učinkovita pri raztapljanju celuloze, je kombinacija z DMSO in guanidinom izboljšala topnost. Analiza D-glukoze z ¹H NMR je pokazala, da je bil topilni sistem primeren za manjše ogljikove hidrate. Vendar so vzorci celuloze dajali spekter z nizko ločljivostjo. Nasprotno pa se je glukomanan (vrsta hemiceluloze) raztapljal učinkoviteje, zlasti v evtektičnih mešanicah z DMSO-d₆ ali devterijevim oksidom, kar je omogočilo pridobitev spektra višje kakovosti. Čeprav so bili začetni poskusi raztapljanja celuloze neuspešni, se je raziskovalno delo osredotočilo na raztapljanje hemiceluloze in pokazalo, da lahko različni topilni sistemi učinkovito pripomorejo k temu procesu.

Keywords:Evtektična topila, Gvanidinijev tiocianat, Urea, Raztapljanje celuloze in hemiceluloze, NMR spektroskopija

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