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NIR spectroscopy and chemometrics for ionic liquids : lignocellulosic biomass dissolution

NIR spectroscopy and chemometrics for ionic liquids : lignocellulosic biomass dissolution. Bettina Liebmann, Joana Rodrigues, Anton Friedl, Kurt Varmuza bettina.liebmann@tuwien.ac.at. Introduction.

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NIR spectroscopy and chemometrics for ionic liquids : lignocellulosic biomass dissolution

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  1. NIR spectroscopyandchemometricsforionicliquids: lignocellulosicbiomassdissolution Bettina Liebmann, Joana Rodrigues, Anton Friedl, Kurt Varmuza bettina.liebmann@tuwien.ac.at

  2. Introduction • The dissolution in ionic liquids (IL) is a new, alternative technology to disrupt the complex fibre network of lignocellulosic biomass at comparatively mild conditions. • Its three main compounds – cellulose, hemicelluloses, and lignin – are interesting renewable sources for biofuels, chemicals, and biomaterials. • Once dissolved in the IL, they can be separated by simple addition of an anti-solvent; e.g., the addition of water immediately precipitates amorphous cellulose from the IL. • In this preliminary study we investigate the applicability of NIR spectroscopy and chemometrics for quantifying the three main compounds of lignocelluloses in IL. Strawcomposition, schematically

  3. IonicLiquids • consist entirely of ions (salts) • melting point < 100°C (liquid at room T!) • negligible vapour pressure • excellent thermal stability up to 400°C • non flammable • electrically conducting, magnetic • many interesting applications! • “design” properties by ion combination Molecularstructureoftheionic liquid EMIM-Oac (1-ethyl-methyl-imidazolium acetate) After mixing the pure cellulose with EMIM-Oac, particles and agglomerations are dissolved by ultrasound and temperatures 40-60 °C for 7-24 hours to obtain clear solutions.

  4. Near-infraredspectroscopy (NIR) NIR spectrometer (BrimroseLuminar 5030, AOTF) NIR transflectance probe with variable pathlength for liquid samples (left); NIR diffuse reflectance probe for solid samples (right). NIR spectrum of the used IL; NIR spectra of pure solid cellulose, lignin, and xylan.

  5. NIR spectra and predicted concentration by PLS regression model SEPCV, standard error of prediction from leave-one-out cross validation; aCV, number of PLS componentsPLS-models with leave-one-out CV in software Unscrambler.

  6. Summaryand Outlook • Empirical models for the concentration of cellulose, lignin, and xylan in ionic liquid EMIM-OAc result in good prediction performance. • In the next step, experiments will focus on multi-component mixtures of cellulose, lignin, and xylan in the ionic liquid. • Good reference values for actually dissolved straw components in the IL is a limiting factor in PLS model building for industrial application.

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