Lignins from kraft and mechanical pulps were isolated before and after oxygen treatment with conventional methods (acidolysis and enzymatic isolation) and with a novel two-step method combining an enzymatic treatment and acidolysis. Results showed that the combined enzymatic hydrolysis-acidolysis made it possible to extract lignin from pulp with a better yield than acidolysis alone and with a higher degree of purity than after enzymatic hydrolysis alone. The lignin samples isolated with the two-step method were analysed by 13 C NMR, 19 F NMR and by gel permeation chromatography. It was shown that the behaviour of mechanical pulp lignin during oxygen treatment was different from that of kraft pulp lignin. Most of these differences could be explained by the lower phenolic content and larger molecular size of the mechanical pulp lignin. As a consequence, oxygen had a poor delignifying effect. Finally, 19 F NMR spectroscopy showed that oxygen could destroy some quinones induced by the alkaline conditions of the O stage.
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