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+0.05Al0.88)2O4.