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Potassium ferrate(VI) (K2FeO4) as a particularly strong oxidant represents an effective and environmentally friendly waste water treatment material. When produced by anodic oxidation in highly alkaline aqueous solution, the K2FeO4 product is separated and sealed in inert plastic bags with the retention of some liquid phase with high pH. This method proved to be excellent for long-term storage at moderately low temperature (5 °C) for industrial applications. It is still imperative to check the ferrate(VI) content of the product whenever it is to be used. Fe-57 Mössbauer spectroscopy is an excellent tool for checking the ratio of ferrate(VI) to the degradation product iron(III) in a sample. For this purpose, normally the spectral areas of the corresponding subspectra are considered; however, this approximation neglects the possible differences in the corresponding Mössbauer–Lamb factors. In this work, we have successfully determined the Mössbauer–Lamb factors for the ferrate(VI) and for the most common iron(III) degradation products observed. We have found superparamagnetic behavior and low-temperature phase transformation for another iron(III) degradation product that made the determination of the Mössbauer–Lamb factors impossible in that case. The identities of a total of three different iron(III) degradation products have been confirmed.

One of the most effective methods to produce ferrate ions (FeO42–) is electrochemical synthesis. During the transpassive anodic dissolution of iron, the formation of ferrate ions and the evolution of oxygen occur simultaneously, and only the sum of the currents generated by the two processes can be observed in the voltammetric curves. Products of the above process have been investigated in 45 % (m/m) aqueous NaOH solutions by using the dual dynamic voltammetry (DDV)&rotating ring-disk electrode (RRDE) method (i.e., applying dynamic potential programs to the disk and the ring electrodes of the RRDE disk electrode and the RRDE ring electrode simultaneously) combined with spectrophotometric measurements. Fe disk/Pt ring and Pt disk/Pt ring RRDE tips were used in the voltammetric experiments. The electrode potential regions where ferrate ions and oxygen are forming could effectively be identified. The results imply that, under the applied experimental conditions, the oxygen evolved at the disk cannot be reduced at the ring. This can be explained by the fact that elemental oxygen practically does not dissolve in concentrated aqueous sodium hydroxide solutions due to the “salting-out effect”. By using the dual voltammetric method, it was also possible to determine the optimal potential range for the electrochemical production of ferrate ions in terms of charging efficiency. The latter quantity has an important impact on the economics of practical applications. The approach proposed in this study proved to be very promising for the simultaneous detection of different dissolution products.