The determination of pH of solutions is one of the most frequent tasks in analytical laboratories. Currently, the most accurate, rapid and widespread method is potentiometric determination method. Glass electrodes, which are traditionally used to determine the pH, are sensitive to mechanical stress and require special preparation before measurement. As an alternative to glass electrodes, different metal oxide electrodes are studied as pH sensors [1-4].  In this work, Ti/TiO2,SbOx electrodes were prepared by plasma electrolytic oxidation (PEO) in an alkaline electrolytes containing antimony hydroxocomplexes and used as pH sensors in potentiometric analysis. According to the energy dispersive analysis, the antimony content in the oxide layers is about 1 at.%. As to X-ray photoelectron spectroscopy, antimony is in the form of Sb2O3 and Sb2O5 in the surface layers. Figure 1 shows that the E-pH functions of all PEO-electrodes have a linear form in the pH range of 2.0–10.0. The Ti/TiO2,SbOx electrodes are more sensitive than Ti/TiO2 ones, they have nearNernstian values of the slopes of the E-pH electrode function (Table). The potential jumps E/V arising at the point of equivalence during the acid-base titration (0.1 M HCl by 0.1 M NaOH) using Ti/TiO2,SbOx electrodes are comparable to or greater than E/V for the traditional glass electrode (Table). The prepared Ti/TiO2,SbOx electrodes were used in potentiometric titrations of different acids such as HCl, CH3COOH and H2CrO4. The error in quantitative determination of the acids does not exceed 2%. The results of the potentiometric determination of alkalinity in the surface and technogenic waters using indicator Ti/TiO2,SbOx electrodes are comparable with the conventionally used glass electrode. The advantages of Ti/TiO2,SbOx electrodes are high sensitivity, good reproducibility, low cost, high mechanical stability and a simple preparation procedure of electrodes.