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Small unmanned aerial systems (sUAS) are a promising technology for atmospheric monitoring of trace atmospheric gases. While sUAS can be navigated to provide information with higher spatiotemporal resolution than tethered balloons, they can also bridge the gap between the regions of the atmospheric boundary layer (ABL) sampled by ground stations and manned aircraft. Additionally, sUAS can be effectively employed in the petroleum industry, e.g., to constrain leaking regions of hydrocarbons from long gasoducts. Herein, sUAS are demonstrated to be a valuable technology for studying the concentration of important trace tropospheric gases in the ABL. The successful detection and quantification of gases is performed with lightweight sensor packages of low-power consumption that possess limits of detection on the ppm scale or below with reasonably fast response times. The datasets reported include timestamps with position, temperature, relative humidity, pressure, and variable mixing ratio values of ~400 ppm CO, ~1900 ppb CH, and ~5.5 ppb NH. The sensor packages were deployed aboard two different sUAS operating simultaneously during the second CLOUDMAP flight campaign in Oklahoma, held during 26–29 June 2017. A Skywalker X8 fixed wing aircraft was used to fly horizontally at a constant altitude, while vertical profiles were provided by a DJI Phantom 3 (DJI P3) quadcopter flying upward and downward at fixed latitude-longitude coordinates. The results presented have been gathered during 8 experiments consisting of 32 simultaneous flights with both sUAS, which have been authorized by the United States Federal Aviation Authority (FAA) under the current regulations (Part 107). In conclusion, this work serves as proof of concept showing the atmospheric value of information provided by the developed sensor systems aboard sUAS. View Full-Text