Detecting and distinguishing between hazardous gases with similar odors by using conventional sensor technology for safeguarding human health and ensuring food safety are significant challenges. Bulky, costly, and power-hungry devices, such as that used for gas chromatography−mass spectrometry (GC−MS), are widely employed for gas sensing. Using a single chemiresistive semiconductor or electric nose (e-nose) gas sensor to achieve this objective is difficult, mainly because of its selectivity issue. Thus, there is a need to develop new materials with tunable and versatile sensing characteristics. Phase engineering of twodimensional materials to better utilize their physiochemical properties has attracted considerable attention. Here, we show that MoSe 2 phase-transition/CeO 2 composites can be effectively used to distinguish ammonia (NH 3 ) and triethylamine (TEA) at room temperature. The phase transition of nanocomposite samples from semimetallic (1T) to semiconducting (2H) prepared at different synthesis temperatures is confirmed via X-ray photoelectron spectroscopy (XPS). A composite sensor in which the 2H phase of MoSe 2 is predominant lacks discrimination capability and is less responsive to NH 3 and TEA. An MoSe 2 /CeO 2 composite sensor with a higher 1T phase content exhibits high selectivity for NH 3 , whereas one with a higher 2H phase content (2H > 1T) shows more selective behavior toward TEA. For example, for 50% relative humidity, the MoSe 2 /CeO 2 sensor's signal changes from the baseline by 45% and 58% for 1 ppm of NH 3 and TEA, respectively, indicating a low limit of detection (LOD) of 70 and 160 ppb, respectively. The composites' superior sensing characteristics are mainly attributed to their large specific surface area, their numerous active sites, presence of defects, and the n-n type heterojunction between MoSe 2 and CeO 2 . The sensing mechanism is elucidated using Raman spectroscopy, XPS, and GC−MS results. Their phase-transition characteristics render MoSe 2 /CeO 2 sensors promising for use in distributed, low-cost, and room-temperature sensor networks, and they offer new opportunities for the development of integrated advanced smart sensing technologies for environmental and healthcare.