Hydrotalcites based upon gallium as a replacement for aluminium in hydrotalcite over a Mg/Al ratio of 2:1 to 4:1 were synthesised. The d(003) spacing varied from 7.83 Å for the 2:1 hydrotalcite to 8.15 Å for the 3:1 gallium containing hydrotalcite. A comparison is made with the Mg/Al hydrotalcite in which the d(003) spacing for the Mg/Al hydrotalcite varied from 7.62 Å for the 2:1 Mg hydrotalcite to 7.98 Å for the 4:1 hydrotalcite. The thermal stability of the gallium containing hydrotalcite was determined using thermogravimetric analysis. Four mass loss steps at 77, 263–280, 485 and 828 °C with mass losses of 10.23, 21.55, 5.20 and 7.58% are attributed to dehydration, dehydroxylation and decarbonation. The thermal stability of the gallium containing hydrotalcite is slightly less than the aluminium hydrotalcite.