Thermal analysis complimented with evolved gas mass spectrometry has been applied to hydrotalcites containing carbonate prepared
by coprecipitation and with varying divalent/trivalent cation ratios. The resulting materials were characterised by XRD, and
TG/DTG to determine the stability of the hydrotalcites synthesised. Hydrotalcites of formula Mg4(Fe,Al)2(OH)12(CO3)·4H2O, Mg6(Fe,Al)2(OH)16(CO3)·5H2O, and Mg8(Fe,Al)2(OH)20(CO3)·8H2O were formed by intercalation with the carbonate anion as a function of the divalent/trivalent cationic ratio.
XRD showed slight variations in the d-spacing between the hydrotalcites. The thermal decomposition of carbonate hydrotalcites
consists of two decomposition steps between 300 and 400°C, attributed to the simultaneous dehydroxylation and decarbonation
of the hydrotalcite lattice. Water loss ascribed to dehydroxylation occurs in two decomposition steps, where the first step
is due to the partial dehydroxylation of the lattice, while the second step is due to the loss of water interacting with the
interlayer anions. Dehydroxylation results in the collapse of the hydrotalcite structure to that of its corresponding metal
oxides and spinels, including MgO, MgAl2O4, and MgFeAlO4.