Gas sensing measurements were performed through drop casting the tindichalcogenides powders onto alumina substrates coated with interdigitated platinum electrode arrays (200 µm Pt fingers spaced 150 µm apart), followed by a heat treatment at 200 °C (at a heating rate of 5 °C/min and 2 h plateau) to remove the solvent and stabilize the material on the substrate. The sensors' electrical resistance was monitored using an Agilent unit (model 34972 A), with multiplexing module (model 34901), during NO2, CO, and H2 analyte cyclic exposure diluted in dry air (gas baseline) using mass-flow controllers (MKS GV50A). Cycles with analyte gas concentrations from 2 to 100 ppm were conducted for 20 min, followed by 60 min exposure to dry air. The total gas flow was kept constant at 100 sccm during the measurements. The sensors were balanced in synthetic air for 12 h for each working temperature to achieve a stable baseline resistance.