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Materials 2016, 9(6), 415; doi:10.3390/ma9060415

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

1
Adhesive Bonding Technology and Surfaces, Fraunhofer Institute for Manufacturing Technology and Advanced Materials IFAM, Wiener Strasse 12, Bremen 28359, Germany
2
Department of Biology/Chemistry (FB2), University of Bremen, Leobener Strasse NW2C, Bremen 28359, Germany
3
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
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)
View Full-Text   |   Download PDF [3909 KB, uploaded 25 May 2016]   |  

Abstract

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
This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. (CC BY 4.0).

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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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