In this work, the results of the enzymatic oxidation of TMP-fibers (thermomechanical pulp) and a well-structured lignin model compound, the dehydropolymer (DHP), were investigated by different 14 C and 13 C methods, caused by a Laccase-Mediator-System (LMS). These methods are the nuclear magnetic resonance spectroscopy ( 13 C-NMR) with DHP (unmarked) and the determination of the 14 CO 2 release of 14 C-marked DHP and TMP-fibers. The 13 C-NMR measurements were chosen to analyze the structural changes of the LMS-treated DHP model compounds and TMP-fibers qualitatively and quantitatively. The data of 14 CO 2 release give an explanation of the demethylation of DHP and TMP-fibers. The effect of the LMS is shown by comparing the results in respect of DHP and TMP-fibers, which were only treated with laccase and of an inactivated LMS as the control. Comparing the results of the 13 C-NMR method, in particular the use of the Mediator during the enzymatical treatment, showed significant changes in the structure of the DHP. Also, the TMP-fibers were materially influenced by the LMS. The analysis of the 14 CO 2 release data of the 14 C-marked DHP and TMP-fibers revealed that the rate of 14 CO 2 increases in the 14 C-2 atom as well as in the O 14 CH 3 group within the first hour of Laccase-Mediator incubation. Therefore, the 14 CO 2 release from the DHP was higher than from the TMP-fibers.
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