In contrast to a petrol refinery a lignocellulosic biorefinery uses woody materials as feedstock. The main products are the structural polymers cellulose, hemicelluloses and lignin, which are used directly or in a more degraded or modified form after different treatments. As the composition of natural feedstock varies, fast and robust screening methods are required to determine the raw material quality and processing conditions. The objective of the following work was to establish analytical methods for the different carbohydrate fractions found in biorefinery product streams: polymers, oligomers and monomers. For the separation and quantification of commonly found sugars in wood different methods can be used.1 The established methods often suffer from poor recovery rates and thus require correction factors to obtain meaningful results. Additionally, samples containing a major fraction of interfering matrix (e.g. plant hydrolysates) often cause problems during analysis. Here we introduce a High Performance Thin Layer Chromatography (HPTLC) method which is capable to separate and quantify monomeric carbohydrates found in wood and can overcome matrix related problems. Analytical methods for the oligomeric fraction in lignocellulosic analysis are quite rare.2 In general, oligomeric fractions are more or less neglected in biorefinery concepts. However, these compounds can be a valuable resource. To close this analytical gap we took different analytical approaches. After the production of oligomeric standards we established a quantitative HPTLC method; and extended an existing Size Exclusion Chromatography (SEC) method. For cellulose, which represents most of the polymeric part in lignocellulosic samples, SEC-MALLS (Multi Angle Laser Light Scattering) is the method of choice yielding absolute molar mass averages (Mw) without the need of calibration.3 The sensitivity of light scattering for cellulose is unfortunately limited in the oligomeric range. Hence combined calibration methods are investigated to analyse the whole range of molar masses in degraded celluloses down into the oligomeric range with methods allowing for accurate molar mass analysis. 1. Churms, S. C. J. Chrom. A 1990, 500, 555-583 2. Vejdovskzy, P.; Oberlerchner J.; Rosenau, T; Potthast, A. Adv. Polym. Sci. 2015, 1-40 3. Oberlerchner J.; Rosenau T.; Potthast A. Molecules 2015, 20, 10313-10341

From monomers to polymers across the oligomeric region: Advanced biorefinery analytics

251st National Meeting (2016)

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