Single-phase anatase-TiO2 nanomaterials with a size of ca. 10 nm and variable quantities of anion impurities were prepared using a novel pathway based on the use of amorphous ammonium Ti-oxychloride precursors synthesized using Ti/Cl initial ratios between 1 and 6. The precursor nature and evolution under thermal treatment were studied using chemical analysis, XRD, XPS, DRIFTS, and mass spectrometry. The nature and concentration of anatase-TiO2 materials anion impurities were analyzed by XPS and DRIFTS. It is shown that negatively charged impurities located in substitutional positions of the anatase network are maximized for a sample synthesized using a Ti/Cl 1:1 atomic ratio and are responsible for the elimination of liquid-phase (phenol) and gas-phase (isopropanol or methylcyclohexane) pollutants under sunlight excitation. A link is established among the initial chemical characterization of the precursors, the final morphological, structural, and chemical composition of the oxide materials, and their photochemical properties.