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Real time spectroscopic ellipsometry from 1.5 to 4.0 eV has been applied to monitor surfaces of optical quality diamond thin films during exposure to low energy Ar and H ion beams, and atomic H. Monolayer‐level sensitivity to the conversion of diamond to optically absorbing sp2 bonded carbon upon ion impact is demonstrated. For Ar ions, a beam voltage of 50 V is found to be sufficient to convert the surface to the equivalent of a single monolayer of sp2 bonded carbon, whereas the topmost 12–16 Å is converted at the threshold for sputter etching, between 100 and 150 V. Atomic H and low energy H ion treatments (≤50 V) are found to eliminate optically absorbing defects within 15 Å of the surface. The overall results provide optimism that real time spectroscopic ellipsometry will be a highly sensitive real time probe of diamond surface and bulk microstructure in the reactive environments of enhanced chemical vapor deposition.