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Quantitative and Qualitative Analysis of Surface Modified Cellulose Utilizing TGA-MS

Adhesive Bonding Technology and Surfaces, Fraunhofer Institute for Manufacturing Technology and Advanced Materials IFAM, Wiener Strasse 12, Bremen 28359, Germany
Department of Biology/Chemistry (FB2), University of Bremen, Leobener Strasse NW2C, Bremen 28359, Germany
Department NMR-supported Structural Biology, Leibniz-Institut für Molekulare Pharmakologie, Robert-Rössle-Strasse 10, Berlin 13125, Germany
Author to whom correspondence should be addressed.
Academic Editor: Kim L. Pickering
Materials 2016, 9(6), 415;
Received: 31 March 2016 / Revised: 13 May 2016 / Accepted: 20 May 2016 / Published: 25 May 2016
(This article belongs to the Special Issue Bio- and Natural-Fiber Composites)
PDF [3909 KB, uploaded 25 May 2016]


With the aim to enhance interfacial adhesion of a hydrophobic polymer matrix and cellulosic fibers and fillers, chemical surface modifications with silane coupling agents are performed. Thermogravimetric analysis (TGA) could be used to determine the degree of surface functionalization. However, similar thermal properties of treated and untreated cellulose hamper a precise determination of silane loading. This contribution deals with quantitative determination of silane loading combining both TGA and elemental analysis. Firstly, silane modified celluloses were studied by FT-IR, Raman, solid state NMR spectroscopy, and polarized light microscopy in order to determine functional groups and to study the impact of chemical treatment on cellulose morphology. Secondly, thermal stability and pyrolysis processes were studied by TG-MS analysis. In order to determine the exact silane loading, the mass percentages of the appropriate elements were quantified by elemental analysis and correlated with the charred residues determined by TGA yielding a linear dependency. With that correlation, it was possible to determine silane loadings for additional samples utilizing simple TGA measurements. The main advantage of that approach is that only one calibration is necessary for routine analyses of further samples and TGA-MS coupling gives additional information on thermal stability and pyrolysis routes, simultaneously. View Full-Text
Keywords: thermogravimetric analysis; evolved gas analysis; silane treatment; microcrystalline cellulose; thiol functionalization thermogravimetric analysis; evolved gas analysis; silane treatment; microcrystalline cellulose; thiol functionalization

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Loof, D.; Hiller, M.; Oschkinat, H.; Koschek, K. Quantitative and Qualitative Analysis of Surface Modified Cellulose Utilizing TGA-MS. Materials 2016, 9, 415.

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