Core Facility Analysis of Lignocellulosics (ALICE)

University of Natural Resources and Life Sciences Vienna (BOKU)

Tulln an der Donau | Website

Open for Collaboration

Short Description

The BOKU Core Facility Analysis of Lignocellulosics (ALICE) offers method development and state-of-the-art chromatographic, spectroscopic and chemical analysis for the advanced characterization of lignocellulose and various biorefinery products.

Contact Person

Ivan Sumerskii

Research Services

Cellulose analysis
• Molar mass distribution of celluloses by SEC-MALLS;
• Carbonyl group profiles of celluloses (“CCOA method”); Carboxyl group profiles of celluloses (“FDAM method”);
• Cellulose cystallinity and allomorphs (solid-state nuclear magnetic resonance (NMR) spectroscopy);
• Hemicellulose content and monosaccharide composition (methanolysis / total hydrolysis);
• Degree of substitution in cellulose derivatives (solid-state and solution NMR spectroscopy).

Lignin Analysis:
• Isolation and purification of technical lignins by precipitation, XAD adsorption or ultrafiltration methods;
• Functional group analysis (methoxy, ethoxy and other alkoxy groups, hydroxy and carboxy groups, sulfonic acid groups) by headspace isotope-dilution GC-MS method, various NMR methods or NIR/IR/chemometrics;
• Molar mass distribution by SEC-MALLS, advanced polymer chromatography (APC) or asymmetric flow field-flow fractionation;
• Determination of carbohydrate components by methanolysis or HPTLC methods;
• Characterisation linkages by one- and two-dimensional NMR or quantitative 13C NMR;
• Characterisation of lignin by thermogravimetry (TGA) and differential scanning
calorimetry (DSC).

Content and characterisation of extractives:
• Extraction of lipophilic compounds / secondary metabolites by means of accelerated solvent extraction or supercritical CO2 fluid extraction (SFE);
• Separation and analysis of lipophilic extractives by supercritical fluid chromatography UPC2 and GC-MS/FID or q-ToF-MS.

Methods & Expertise for Research Infrastructure

A largely unique combination of methods is available for the analysis of celluloses, covering the entire range of cellulosic materials, from pulp and paper, via nanostructured celluloses and cellulosic fibres, to textiles, cellulose derivatives and historical cellulosic objects. Determination of molar mass distribution, profiles of oxidized groups (carbonyls and carboxyls) in relation to the molar mass distribution, characterization of cellulose allomorphs and crystallinity, the analysis of hemicellulosic components, thermal stability and rapid screening by means of one of the largest cellulose NIR/IR databases, is just a short list of offered methods.

Lignins analyses are performed by several spectroscopic, chromatographic and wet chemical methods, which in combination by far exceed the information provided by conventional or individual analytical techniques. Native lignins, near-native lignins (e.g., milled-wood lignin) and all types of technical lignins (Kraft, lignosulfonate, organosolv, biorefinery lignins) are processed. Based on an extensive lignin database, fast methods by NIR/IR/chemometrics are available.

In the field of chemistry of renewable resources, separation techniques and extractions play a special role, both for fractionation and purification, as well as for the extraction of special substances and for pure preparations. In this area, the extraction of celluloses for the determination of secondary constituents, such as hemicelluloses, as well as the separation and purification of technical lignins from the process matrices are performed. Besides conventional approaches, ALICE core facility offers the most advanced techniques, such as supercritical CO2 fluid extraction and accelerated solvent extraction. If required, supercritical extraction can be combined with supercritical chromatographic separation and identification by means of high class quadrupole time-of-flight mass spectrometry.


EQUIPMENT
- Further services include advanced data interpretation as well as professional training sessions.
- Wyatt Technology SEC-MALLS(488)-RI-FL
- Wyatt Technology SEC-MALLS(785)-RI-UV
- Wyatt Technology AF4-Eclipse®
- Wyatt DLS Dynapro® Nanostar ®
- Waters Aquity® APC
- Agilent HS 7697A-coupled to 6890N GC and 5975B MSD
- Thermo Scientific™ LTQ XL™ ion trap mass spectrometer
- Waters ACQUITY UPC2®
- Waters QTof™-MS Xevo® G2
- NMR Spectrometer Bruker Avance III™ HD 400 MHz (Solid State)
- RETSCH Cryomill
- scCO2 extraction unit
- Climate chamber

Equipment

• Infrared Spectrometer
• 2D - Gelpermeationschromatographie
• Pyrolysator
• Ionenchromatograph