Naturally occurring samples of iwakiite, Mrtl.* Fe,,vOI, have been annealed for 17 and 77 h at 1000 K in an investigation of order-disorder phenomena in Mn-Fe oxide spinels. TWO distinct magnetic hyperfine patterns, which correspond to Fe-and Mn-rich phases, were observed in the 57Fe Mijssbauer spectra for the two annealed samples. While the spectrum of the Fe-rich phase corresponds to a magnetically and crystallographically highly ordered cY-Fe,O,-like phase, the Mn-rich phase exhibits considerable disorder, as indicated by very broad linewidths and a low value for Neff. Annealing for longer periods of times leads to a considerable increase in the ordering of the Mn-rich spine1 phase, as evidenced by the considerable narrowing of the lines, from re2.40 mms-' to I'= 1.17 mm s-', and an increase. in HErf from 318 to 417 kOe at 29s K. The Fe-rich, cw-Fe20,-like phase is not affected by further annealing, as expected. At 85 K, the "'Fe Miissbauer spectrum of the Mn-rich. spine1 phase continues to exhibit rather broad lines, indicating the presence of significant cation disorder.