Formation of interfacial nanoscale voids in Al during room-temperature caustic corrosion was characterized by positron annihilation spectroscopy (PAS) and compared with measurements of deuterium absorption using secondary ion mass spectrometry (SIMS). The hypothesis was investigated that voids are created from vacancy-hydrogen (Vac-H) defects introduced during corrosion. Evidence for both mobile and immobile forms of absorbed hydrogen was obtained, the latter present within distances of 50 nm from the metal-oxide interface, where voids were also found. During corrosion, the immobile hydrogen was found only during discrete 1-2 min intervals of time separated by periods of 1-2 min when it was not present. Model calculations suggested that this transient behavior is consistent with repeated nucleation and dissolution of clusters of Vac-H defects. Only some aspects of the time-dependence of the void concentration from PAS corresponded with that of absorbed hydrogen; the former is believed to be influenced by metallic impurities.