Emanation thermal analysis (ETA), thermogravimetry, DTA and XRD were used in thermal characterization of natural vermiculite
(Santa Olalla, Huelva, Spain) and of Na+- and - exchanged vermiculite samples during heating in air in the range 25-1100C. A good agreement between the results of
these methods was found. Changes in the radon release rate measured by ETA, which reflected the decrease and collapse of the
interlayer space after the release of water as well as the formation of new crystalline phases were evaluated using a mathematical
model. The model used for the evaluation was found suitable for the quantitative characterization of microstructure changes
during in situ conditions of heating of vermiculite samples.