The standard Gibbs energy of formation of the spinel MgAl 2 O 4 from component oxides, MgO and ␣-Al 2 O 3 , has been determined in the temperature range 900 to 1250 K using a solid-state cell incorporating single-crystal CaF 2 as the solid electrolyte. The cell can be represented as The standard Gibbs energy of formation from binary oxides, computed from the reversible emf, can be represented by the expression ⌬G°f ,ox = −23600 − 5.91T (±150) J/mol The ''second-law'' enthalpy of formation of MgAl 2 O 4 obtained in this study is in good agreement with hightemperature solution calorimetric studies reported in the literature.