In this work the synthesis of hercynite from Fe₂O₃ and Al₂O₃ powders was carried out by arc-melting method under the protective argon atmosphere. The obtained material was characterized with the use of powder X-ray diffractometry (XRD) and Mössbauer spectroscopy (MS). A Mössbauer effect in hercynite obtained by the arc-melting method indicated the cations distribution in the spinel structure among the tetrahedral and octahedral interstices. The presence of Fe²⁺ ions was detected in both tetrahedral and octahedral sites while Fe³⁺ ions occupied only the octahedral interstices. The approximate formula of the obtained iron-aluminate spinel was as follows (Fe²⁺ _0.77Al³⁺ _0.23) (Fe³⁺ _0.07Fe²⁺ _0.05Al_0.88)₂O₄.