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One of the most significant drawbacks of metal oxide (MOS) based chemiresistive gas sensors is the requirement of high operating temperature (250–450 °C), which results in significant power consumption and shorter lifetime. To develop room temperature (21±2 °C) MOS chemiresistive gas sensors, the sensing performance of different MOS nanostructures (i.e., tin (IV) oxide (SnO2) nanoparticles (NPs), indium (III) oxide (In2O3) NPs, zinc oxide (ZnO) NPs, tungsten trioxide (WO3) NPs, copper oxide (CuO) nanotubes (NTs), and indium tin oxide (In90Sn10O3 (ITO)) NPs) were systematically investigated toward different toxic industrial chemicals (TICs) (i.e., nitrogen dioxide (NO2), ammonia (NH3), hydrogen sulfide (H2S), carbon monoxide (CO), sulfur dioxide (SO2) and volatile organic compounds (VOCs) (i.e., acetone (C3H6O), toluene (C6H5CH3), ethylbenzene (C6H5CH2CH3), and p-xylene (C6H4(CH3)2)) in the presence and absence of 400 nm UV light illumination. Sensing performance enhancement through photoexcitation is strongly dependent on the target analytes. Under 400 nm UV photoexcitation at 76.0 mW/cm2 intensity, room temperature (21±2 °C) NO2 sensing was readily achieved where SnO2 NPs exhibited the highest sensor response (S = 474.4 toward 10 ppmm (parts per million by mass)) with good recovery followed by ZnO NPs > In2O3 NPs > ITO NPs. Meanwhile, indirect bandgap n-type WO3 NPs showed limited NO2 sensing performance under illumination, whereas p-type CuO NTs showed relatively good sensing response. The most significant improvements in SnO2 compared to other MOS nanoparticles might be attributed to the highest number of photogeneration electrons, which rapidly reacted with adsorbed species to enhance the reaction kinetics. WO3 NPs showed a unique sensing response toward aromatic compounds (e.g., ethylbenzene and p-xylene) under UV illumination, where maximum sensitivity was achieved under 36 mW/cm2 irradiation. Changing light intensity from 0.0 to 36.4 mW/cm2, WO3 showed 15.4-fold and 6.3-fold enhancement in sensing response toward 25 ppmm ethylbenzene and 100 ppmm p-xylene, respectively. 400 nm optical excitation has a limited effect on the sensing performance toward CO, SO2, toluene, and acetone.