Core Facility Analysis of Lignocellulosics

The BOKU Core Facility ALICE (Analysis of Lignocellulosics) with its twin lab at Åbo Akademi University Turku, Finland, offers method development and state-of-the-art chromatographic, spectroscopic and chemical analysis for the advanced characterization of lignocellulose and biorefinery products.

Analysis of celluloses

A largely unique combination of methods is available for the analysis of celluloses, covering the entire range of cellulosic materials, from cellulosic pulp and paper, via nanostructured celluloses and cellulosic fibres, to textiles, cellulose derivatives and historical cellulosic objects of art. Solubility studies are part of the portfolio as well as the determination of molar mass distribution by multidetector-GPC (MALLS, RI, UV), the determination of cellulose allomorphs and crystallinity by solid-state NMR spectroscopy, the analysis of hemicellulosic components (methanolysis, total hydrolysis), thermal stability (TGA) and rapid screening by NIR/IR. The recording of profiles of oxidized groups (carbonyls and carboxyls) in relation to the molar mass distribution by means of multidetector-GPC with group-selective fluorescence labeling ("CCOA method" and "FDAM method") is performed worldwide only here. One of the largest cellulose databases with data of more than 3000 different cellulose samples is available for data matching and comparison.

Lignins analyses

are performed by several spectroscopic, chromatographic and wet chemical methods, which in combination 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. The first step is the isolation of lignins from their complex matrices and their separation from organic and inorganic accompanying substances, if needed. The lignins´ molar mass distribution is measured by multi-detector GPC and asFFFF, using the latest methodology (MALLS 785 nm) which avoids conventional calibration. The determination of functional groups (methoxyl, carboxyl, aliphatic and aromatic OH, sulfonic acid, reactive centers) is performed both NMR-spectroscopically (³¹P, acetylation) and by wet- chemical/chromatographic means with robot-automated methods (GCMS) optimized towards higher throughput. For general structure and linkage analysis, modern quantitative one-dimensional and multidimensional NMR spectroscopy methods, optimized for the special analyte lignin, are available. Based on an extensive lignin database, fast methods by NIR/IR/chemometrics are available.

Separation techniques and extractions

In the field of chemistry of renewable resources, especially in the most diverse biorefinery scenarios, 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 of technical lignins from the process matrices (liquors) are performed. Optimization of extraction parameters by means of accelerated solvent extraction is applied. Extractives, secondary metabolites or dyes are obtained both by solvent extraction and supercritical extraction (scCO₂, up to 2 L content), which can be combined with supercritical chromatographic separation (SFC) and identification (q-ToF-MS) if required.

Further services

For the above standard procedures, additional advanced data interpretation as well as professional training sessions are offered on request. Further services include special, tailor-made investigations of chromophore chemistry, aging and analysis of conservation methods of cellulosic materials as well as modification, properties and utilization of lignins.