Polycrystalline samples of cation-deficient FeAI204 spinel with Fe 3+ ions and vacancies on both octahedral and tetrahedral sites have been investigated by electron spin resonance (ESR). For samples annealing at 1100~ and slightly oxidized (~0.16wt% Fe3+), the ESR spectrum originates from Fe 3+ ions located in trigonally distorted octahedral sites of ~z-AI203 formed during the annealing and also from Fe 3+ ions introduced by oxidation at low temperature in octahedral sites of spinel structure. The samples with concentration between 0.1 6 and 1.6wt% Fe 3+ show the majority of Fe 3+ ions to be on tetrahedral sites and the rhombic symmetry around the Fe 3+ ions is attributed to the presence of cation vacancies.