Column chromatographic procedures have been developed for separating binary mixtures of commercial sodium dodecylbenzenesulfonate (DDBS) with the hydrotropes sodiumm‐xylenesulfonate (SXS) and 8‐[5(6)‐carboxy‐4‐hexyl‐cyclohex‐2‐enyl] octanoic acid (DAC) and ternary mixtures of these three materials. The materials are separated on a specially purified silica gel column. The C21 dicarboxylic acid (DAC) is eluted with 2:3 (v/v) chloroform/acetone in the presence of SXS, with 3:2 (v/v) chloroform/acetone in its absence. The DDBS is eluted with 1:9 (v/v) isopropyl alcohol/acetone in the presence of SXS, with methanol in its absence. The SXS is eluted with methanol in the presence of DAC, with 8:2 (v/v) isopropyl alcohol/acetone in its absence. The presence of SXS in mixtures with DDBS in greater than equimolar amounts interferes with the Hyamine 1622, mixed indicator titration for DDBS.