β-FeOOH (akaganéite) was prepared by slow hydrolysis of an FeCl3 solution. X-ray diffraction measurements gave refined unit-cell parameters of a=10·535 Å, c=3·030 Å.
Two doublets with δ(Fe)=0·39, ΔEQ=0·95, and δ=0·38, ΔEQ=0·55 mm s−1, respectively, can be fitted to the Mössbauer spectrum taken at room temperature.
Magnetically split Mössbauer spectra were registered at 135 and 4°K. These can be resolved into at least three superimposed sextets, corresponding to different Fe3+ sites in the β-FeOOH structure. At 4°K a three sextet model gives parameters of δ=0·36, ΔEQ=0·90, Hi=473; δ=0·35, ΔEQ=0·30, Hi=479; and δ=0·37, ΔEQ=−0·05 mm s−1, Hi=486kOe, respectively.
The complexity of the Mössbauer spectra of β-FeOOH limits the usefulness of this method as a tool for the identification of akaganéite in composite natural samples.