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Abstract: The surface and adsorbate chemistry of the TiO2(100) surface prepared at high temperatures and ambient conditions were studied by means of angle resolved X-ray photoelectron spectroscopy (AR-XPS), Low Energy Electron Diffraction (LEED) and Atomic Force Microscopy (AFM) based nanoshaving studies. The TiO2(100) surface shows a 1×1 structure with a 1×3 superstructure assigned to surface defects. A significant hydroxide surface concentration was revealed by means of AR-XPS measurements. The adsorbate formation of nonadecanoic acid (NDCA) from ethanolic solution led to disordered sub-monolayer surface coverage. The weak interaction between the carboxylic acid group and the TiO2 surface is assumed to be a combination of the neutral to acid behavior of the TiO2 surface and the stable hydroxide surface layer created under ambient conditions. [Copyright &y& Elsevier]