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Mössbauer measurements were performed at room temperature for a group of nonstoichiometric iron oxides of the Fe1‐xO type with 0.002≦x≦0.250. The measured spectra for the samples with x ranging from 0.002 to 0.083 represent quadrupole split Fe2+ doublets and an unseparated Fe3+ singlet. For the samples with x≧0.084 apart from asymmetric quadrupole splitting, a double Zeeman splitting appears, due to the formation ofmagnetite‐like clusters. The intensity ratio of the quadrupole pattern of the wüstite phase to the Zeeman pattern of the magnetite phase decreases with increasing x to zero for x = 0.250 (pure synthetized magnetite), which is in agreement with X‐ray diffraction analyses.

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