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Lignosulfonates (LS) are water-soluble polyphenolic macromolecules derived from lignins and common industrial additives in plasticizers and dispersants. A key feature for a more efficient utilization of modified LS is the monitoring of their free phenol (OH phen ) content during various reactions as these phenols govern a large part of their chemical reactivity. Against this background, the UV difference spectroscopy (Δε i  method) and ClO 2  titration have been revisited. Synthetic LS model compounds with a SO 3 H group on their benzylic position and H, G, and S aromatic rings were synthesized and used to assess the suitability of both the ClO 2  titration and the Δε i  method on LS. The methodology combining the two analytical methods was then used to determine the molar extinction coefficient of a given LS allowing the calibration of the Δε i  method for a convenient and rapid monitoring of OH phen  in the course of LS reactions involving the OH phen  groups.

Monitoring of free phenol content in lignosulfonates by ClO 2 titration and UV difference spectroscopy