Abstract: Mössbauer spectroscopy has been used to identify the iron-containing products that are formed during the thermal decomposition of ankerite in a CO₂ atmosphere. The decomposition takes place in three stages and evidence is produced to show that the first stage involves decomposition of ankerite to yield a periclase-wustite solid solution, (Mg,Fe)O, along with calcite and CO₂, the periclase-wustite then reacting with CO₂ to produce magnesioferrite (MgFe₂O₄) and CO. In the second stage the magnesioferrite and calcite react to produce periclase and dicalcium ferrite. The third stage does not involve reaction of Fe-containing phases and corresponds to the decomposition of calcite to CaO.