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A calibration experiment was orchestrated on February 7, 2001 at the Salar de Arizaro, Argentina to assess the on-orbit radiometric and spectral calibration of Hyperion. At this high-altitude homogeneous dry salt lakebed, Hyperion, Airborne Visible/Infrared Imaging Spectroradiometer (AVIRIS) and in situ measurements were acquired. At a designated calibration target on Salar de Arizaro, the radiance spectra measured by Hyperion and AVIRIS were compared. In the spectral range from 430-900 nm [visible near-infrared (VNIR)], the ratio of Hyperion over AVIRIS was 0.89, and in the 900-2390-nm [shortwave infrared (SWIR)] spectral range the ratio was 0.79. A comparison of the Hyperion radiance spectrum with a radiative-transfer-code-predicted spectrum for the calibration target showed similar results. These results in conjunction with prelaunch laboratory measurements, on-orbit lunar measurements, other on-orbit calibration experiment results, as well as comparison with Landsat-7, lead to an update of Hyperion radiometric calibration in December 2001. The compromise update was to increase the Hyperion radiometric calibration coefficients by 8% in the VNIR and 18% in the SWIR spectrometers. In addition to radiometric accuracy, the on-orbit radiometric precision of Hyperion was assessed at Salar de Arizaro. Noise-equivalent delta radiance was calculated from Hyperion dark signal data and found to be five to ten times higher in comparison to AVIRIS. Also, from a homogeneous portion of Salar de Arizaro the Hyperion SNR was estimated at 140 in the VNIR and 60 in the 2200-nm region of the SWIR spectral range. Cross-track radiometric response was assessed with the AVIRIS dataset that spanned the full Hyperion swath. Within the accuracy of the registration of the datasets, the Hyperion cross-track response was shown to be uniform. Hyperion spectral calibration was assessed with a spectral fitting algorithm using the high spectral resolution radiative transfer modeled spectra for Salar de Arizaro.