The atmospheric boundary layer (ABL) is the layer of air directly influenced by the Earth’s surface and is the layer of the atmosphere most important to humans as this is the air we live in. Methods for measuring the properties of the ABL include three general approaches: satellite-based, ground- based and airborne. A major research challenge is that many contemporary methods provide a restricted spatial resolution or coverage of variations of ABL properties such as how wind speed varies across a landscape with complex topography. To enhance our capacity to measure the properties of the ABL, this thesis presents a new technique that involves a small unmanned aircraft system (sUAS) equipped with a customized payload for measuring wind speed and particulate matter. The research presented herein outlines two key phases in establishing the proof-of-concept of the payload and its integration on the sUAS: (1) design and testing and (2) field demonstration. The first project focuses on measuring wind speed, which has been measured with fixed wing sUASs in previous research, but not with a helicopter sUAS. The second project focuses on the measurement of particulate matter, which is a major air pollutant typically measured with ground- based sensors. Results from both proof-of-concept projects suggest that ABL research could benefit from the proposed techniques.