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Herein, the desolvation, dehydroxylation and rehydroxylation of the metal organic frameworks UiO-66 and -67 are followed by in situ DRIFTS and TG–DSC. The spectra recorded on UiO-66 feature multiple bands corresponding to chemically inequivalent isolated hydroxyl groups, whereas UiO-67 has the expected single μ3-OH band from the Zr6O4(OH)4 cornerstone. Complete rehydration is demonstrated on both...