Natural brucite and two precipitated Mg(OH)2 samples were analysed in a simultaneous TG-DTG-DSC analyser. The initial dehydroxylafion temperature of natural brucite is lower than those of the precipitated samples, but the maximum and final temperatures of the former are higher than those of the latter. The maximum temperatures of individual samples obtained from DTG and DSC curves are almost the same: Heats of reaction derived from peak areas for the three samples are not exactly the same, as they are influenced by the specific surface area of the individual sample. Activation energies deduced by Freeman and Carroll's method are very different from one another. This is attributed to the difference in pressure when the sample is crimped. A linear relationship is observed between the deduced activation energy and the specific height of the DSC peak.In a series of papers [1 ], Freeman and Carroll's treatment was applied to investigate the kinetic parameters of some reactions in solution. Activation energies and orders of reaction derived therefrom agree very well with the accepted values.The thermal dehydroxylation of Mg(OH)2 has been investigated by many authors, but agreeing conclusions were not obtained. Thus, Gregg and Razouk [2] found that the rate of dehydroxylation was of two-thirds order. The activation energies for two brucite samples of 10-80 mesh and 100-200 mesh were 21.0 and 27.6 kcal/mole, respectively. The activation energies of several precipitated Mg(OH)2 samples varied from 12.4 to 27.4 kcal/mole. Kenya [3] claimed that the initial stage of dehydration of Mg(OH)2 was a first-order reaction, and an activation energy of 23 kcal/mole was observed. Turner, Hoffman and Chen [4] investigated several preparations of Mg(OH)2 with a thermobalance. Assuming a two-thirds order reaction and taking the first two terms of Schlomich's expansion as the approximation of the integral, they obtained 51.4 and 57.0 kcal/mole for the activation energies of the precipitated Mg(OH)2 and natural brucite, respectively. Their values are much higher than the previous ones. A review has recently been published by Sharp [5]. Activation energies varying from 16 to 95 kcal/mole, and reaction orders varying from 0 to 1.8 have been reported by various authors for the dehydroxylation of different types of Mg(OH)2 samples, using different methods of data treatment. It is desirable, therefore, to apply Freeman and Carroll's method to analyse thermogravimetric data for the dehydroxylation of Mg(OH)2.