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Stoichiometric polymer – surfactant complexes (SPSCs) of natural polymers, chitosan (CTS) and chitosan sulfate (CS), with oppositely charged surfactants have been studied. Water-insoluble SPSCs of chitosan with Na-dodecylbenzylsulfonate (DDBS-Na) and chitosan sulfate with dodecylpyridinium chloride (DDP-Cl) were synthesized by mixing of their aqueous solutions containing equimolar amounts of polyelectrolytes and surfactants, taken at pH 4 and pH 10, correspondingly. Compositions of SPSCs formed were examined by the analysis of supernatant liquids by potentiometric titration and spectrophotometry. The structure of SPSCs prepared was studied by means of wide-angle and small-angle X-ray scattering and differentially scanning calorimetry. It is established that the polymer – surfactant complex formed by chitosan and DDBS-Na is a completely amorphous compound just as the polymer – surfactant complex formed by chitosan sulfate and DDP-Cl has some crystallic inclusions in packing of the aliphatic radicals of dodecylpyridinium - anions in the lamellae of the complex.