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The structural evolution of a trioctahedral mica from Cava St. Antonio, Mt. Vulture, Potenza, Italy, has been studied in the temperature range 100-1023 K using in situ single-crystal X-ray diffraction techniques. The sample used shows a Ti-rich composition close to the phlogopite-annite join with the following crystal-chemical formula: (K 0.85 Na 0.11 Ba 0.03 )(Al 0.17 Mg 1.98 Mn 0.01 Fe 2+  0.29 Fe 3+  0.37 Ti 0.18 )(Si 2.75 Al 1.25 ) O 10.66 (F 0.13 OH 1.20 Cl 0.01 ). In the present study, the chemical and structural changes and the deprotonation process involved during heating have been characterized. Analysis of the data showed that a, b, and c cell parameters expand almost linearly up to 823 K, while the β angle remains constant. A sharp decrease in the unit-cell dimensions was observed at 873 and 1023 K. Linear trends obtained during reversal experiments from 1023 K to room temperature demonstrated the irreversibility of these events.

Thermal behavior of a Ti-rich phlogopite from Mt. Vulture (Potenza, Italy): An in situ X-ray single-crystal diffraction study