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Fe(III)-doped TiO2 nanoparticles with different Fe(III) content (at %, nominal) have been prepared at different pH using hydrothermal method. The products were characterized by X-ray powder diffraction, transmission electron microscope, electron diffraction, diffuse reflectance spectra, XPS and spot EDX analysis. All the studies showed that anatase, brookite and trace of hematite coexisted at lower pH (1.8 and 3.6) when Fe(III) content was as low as 0.5% and the distribution of iron ions was non-uniform between particles. But at higher pH (6.0), the uniform solid solution of iron-titanium oxide formed. The photoelectrochemical properties were studied by measuring photocurrent at different electrode potentials and the results showed the phenomena of p-n photoresponse existence in samples prepared at pH 1.8–6.0.