Rapid determination of γ-value and xanthate group distribution on viscose by liquid-state 1H NMR spectroscopy

• Stabilization of xanthate groups by reaction with 4-methylbenzyl bromide.
• Analysis of the resulting product by liquid-state 1H NMR.
• Analysis of the proton-spectrum using deconvolution.
• Determination of γ-value and distribution of xanthate groups on cellulose xanthate.

A method for the determination of the γ-value and more importantly the distribution of xanthate groups on cellulose xanthate produced during the viscose process is presented. The method is based upon stabilization of xanthate groups attached to the cellulose chain by reaction with 4-methylbenzyl bromide and analysis of the resulting product by liquid-state 1H NMR. Careful analysis of the proton-spectrum using deconvolution gave a very fast method for the measurement of the γ-value which compared well with the data obtained by IR spectroscopy. In addition it could be shown that the distribution of the xanthate groups on the anhydroglucose monomeric unit (xanthation at position 2, 3 or 6) changes significantly during ripening. The method gave useful results even for viscose with low γ-values of about 25.