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Abstract We present new results on the conversion of pure, undoped synthetic ferrihydrite, wet‐annealed at pH 6.56 and 90°C without stabilizing ligands, to nanophase goethite, hematite, and an intermediate magnetic phase, nanophase maghemite. Our analyses included magnetic field and temperature‐dependent properties and characterization by powder X‐ray diffraction, Mössbauer spectra, and high‐resolution transmission electron microscopy. We sampled alteration products after 0.5 hr, and then in a geometric progression to 32 hr, yielding a detailed examination of the earliest alteration phases. There are many similarities to the latest studies of pure ferrihydrite alteration but with a significant difference: We observe early appearance of oriented nanophase goethite along with a soft magnetic contribution, while rhombohedral hematite crystals form later, as reported in previous studies. Our observations attest to the non‐uniqueness of the magnetic enhancement process and to its strong dependence on environmental conditions, with important implications for use of the hematite/goethite ratio as a paleoprecipitation proxy.