The synthesis and characterization of sodium titanates (ST), and their evaluation in the photocatalytic reduction of nitric oxide (NO) are described herein. The materials were synthesized by a hydrothermal route using 5 M NaOH as the mineralizer agent and a TiO 2 content of 0.06 mg/mL (expressed as the mass ratio of TiO 2 /mL of NaOH), at 170 °C for 48 hours, resulting in sodium tri-and hexa-titanates. A nanotubular morphology was observed for the ST, as proved by scanning electron microscopy (SEM); a subsequent heat-treatment at 400 °C allowed a complete transformation of sodium tri-to hexa-titanates and an increase in bandgap. The obtained ST were impregnated with Ag + and Zn + cations, ST-Ag and ST-Zn, respectively, to tune the materials' bandgap. XPS analysis of the ST-Ag materials showed evidence of metallic Ag, pointing to the formation of silver nanoparticles, whereas for ST-Zn oxide phases were mainly spotted. The materials were evaluated for the photocatalytic reduction of NO using a reactor fed with a continuous ow rate of NO, generated in situ at a ow of 280 mL/min using nitrogen and a 253 nm UV irradiation source. The photocatalytic tests showed that pristine ST (tri-and hexa-titanates) displayed better performance in the reduction of NO with respect to the impregnated samples (ST-Ag, ST-Zn).Maximum degradation e ciencies of 80% were achieved when 1 g of photocatalyst was used with a ow of 280 mL/min and a 253 nm UV lamp.