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Using synchrotron radiation with a photon energy of 15 keV, the molecular structure of an adsorbed n-triacontanol layer at the n-hexadecane - water interface in different its phase states has been studied by the method of diffuse X-ray scattering. The analysis of the experimental data shows that a transition to the multilayer adsorption occurs at a temperature below the two-dimensional vapor - liquid transition at the interface. This transition has been attributed to a feature in the temperature dependence of the concentration of micelles in a surface layer 100 - 200 {\AA} thick.

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