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Carbon nanofibres and multi-branched carbon nanotubes are synthesized by using a new, proposed in this study method. The acid-base, adsorption and geometric properties of nanomaterials are characterised. Next we present first comparative adsorption and calorimetric studies of phenol uptake from aqueous solutions on mentioned nano-sized carbon materials and on nanotubes having similar diameter. The comparison of carbon nanofibres, multi-branched carbon nanotubes, and multi walled carbon nanotubes shows that for non-porous carbon nanomaterials the concentration of basic surface functionalities determines the mechanism of phenol adsorption. In consequence, larger phenol adsorption is recorded for the most basic nanomaterials (nanofibres and multi walled nanotubes) and smaller for multi branched nanotubes having the smallest surface concentration of basic groups. Possible explanation of differences between enthalpy of phenol displacement on graphite and on studied carbon adsorbents is also given.