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Chalcedony consists of hydroxylated 50–100 nanometre measuring α-quartz (SiO₂) crystallites that lose their surface silanole groups (Si–OH) upon heating between 350°C and 600°C. The loss of the chalcedony's ≈1% of silanole groups allows for the healing of water related defects in the crystallites. We investigated these crystallographic transformations using Fourier Transform mid Infrared Spectroscopy in direct transmission, Attenuated Total Reflection (ATR) and the reflectivity. We found that an absorption band that is specific for chalcedony at 555cm⁻¹ disappears gradually upon heating between 350°C and 600°C. The reduction of the band is correlated to the loss of surface silanoles. This result leads to the assignment of the band to free Si–O vibrations in non bridging Si–OH groups that have a lower natural frequency than Si–O vibrations in bridging Si–O–Si. The recognition of a silanole signal in the mid …