a b s t r a c tThere is an increasing desire to control and monitor gas emissions from coal-fired power plants and other industrial systems. With this desire, there is a growing need for distributed gas sensors to monitor these emissions at high temperature ( > 600 • C), especially for pollutants such as SO 2 and H 2 S. The objective of this work was to investigate molybdenum and tungsten binary and ternary oxide thick films on a chemiresistive sensor platform for monitoring of gas sulfur species. The work evaluated the SO 2 sensitivity of WO 3 , MoO 3 , SrMoO 4 , NiMoO 4 , Sr 2 MgMoO 6-␦ (SMM), Sr 2 MgWO 6-␦ (SMW), NiWO 4 , and SrWO 4 compositions at 600-1000 • C. The SrMoO 4 composition at both the micro-and nano-particulate scale showed the most promise in sensitivity, stability and selectivity to SO 2 up to 1000 • C. Hydrothermallysynthesized nano-SrMoO 4 showed the highest sensor response with the R max values of −17.2, −50.2 and −40.5 upon exposure to a 20 min pulse of 2000 ppm of SO 2 at 600 • C, 800 • C and 1000 • C, respectively. Similar sensitivity trends were distinguished down to 1-5 min SO 2 pulses. The nano-SrMoO 4 showed low cross-selectivity to H 2 and CO. Finally, the nano-SrMoO 4 sensor was also tested with H 2 and coal syngas containing 5-100 ppm H 2 S, where high sensitivities were realized for both, but the sensing mechanism was altered in the latter (n-type to p-type semiconducting behavior). In order to better understand the sensing mechanism, extensive microstructural, electronic and chemical property characterizations were completed in this work.