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The use of Uncrewed Aerial Systems (UASs) for remote sensing applications has increased significantly in recent years due to their low cost, operational flexibility, and rapid advancements in sensor technologies. In many cases, UAS platforms are considered viable alternatives to conventional satellite and crewed airborne platforms, offering very high spatial, spectral, and temporal resolution data. However, the radiometric quality of UAS-acquired data has not received equivalent attention, particularly with respect to absolute calibration. In this study, we (1) evaluate the absolute radiometric performance of two commonly used UAS sensors: the Headwall Nano-Hyperspec hyperspectral sensor and the MicaSense RedEdge-MX Dual Camera multispectral system; (2) assess the effectiveness of the Empirical Line Method (ELM) in improving the radiometric accuracy of reflectance products generated by these sensors; and (3) investigate the influence of calibration target characteristics—including size, material type, reflectance intensity, and quantity—on the performance of ELM for UAS data. A field campaign was conducted jointly by the U.S. Geological Survey (USGS) Earth Resources Observation and Science (EROS) Center and the USGS National Uncrewed Systems Office (NUSO) from 15 to 18 July 2023, at the USGS EROS Ground Validation Radiometer (GVR) site in Sioux Falls, South Dakota, USA, over a 160 m × 160 m vegetated area. Absolute calibration accuracy was evaluated by comparing UAS sensor-derived reflectance to in situ measurements of the site. Results indicate that the Headwall Nano-Hyperspec and MicaSense sensors underestimated reflectance by approximately 0.05 and 0.015 reflectance units, respectively. While the MicaSense sensor demonstrated better inherent radiometric accuracy, it exhibited saturation over bright targets due to limitations in its automatic gain and exposure settings. Application of the ELM using just two calibration targets reduced discrepancies to within 0.005 reflectance units. Reflectance products generated using various target materials—such as felt, melamine, or commercially available validation targets—showed comparable agreement with in situ measurements when used with the Nano-Hyperspec sensor. Furthermore, increasing the number of calibration targets beyond two did not yield measurable improvements in calibration accuracy. At a flight altitude of 200 ft above ground level (AGL), a target size of 0.6 m × 0.6 m or larger was sufficient to provide pure pixels for ELM implementation, whereas smaller targets (e.g., 0.3 m × 0.3 m) posed challenges in isolating pure pixels. Overall, the standard manufacturer-recommended calibration procedures were insufficient for achieving high radiometric accuracy with the tested sensors, which may restrict their applicability in scenarios requiring greater accuracy and precision. The use of the ELM significantly improved data quality, enhancing the reliability and applicability of UAS-based remote sensing in contexts requiring high precision and accuracy.