Small and pilot plant scale expts. showed that ion-exclusion chromatog. with Amberlite IR 140 columns is an efficient technique for the sepn. of spent sulfite liquor (SSL) components into reasonably pure and sugar-free lignosulfonate and tech. grade sugar fractions. The use of strongly acidic cation exchanger in the same ionic form as the SSL obviated the need for regeneration between samples, which are displaced with H2O.