Formation of NiFe
2O
4 from iron hydroxides. and an oxide has been studied in high temperature water by in situ measurements. The five kinds of Fe compounds used in the experiments are known as components of Fe crud in BWR condensate water. Among the reactants and products, only NiFe
2O
4 shows ferromagnetism. An in situ method, using a magnetic balance, was developed to measure the mass of NiFe
2O
4 in high temperature water. The lower detection limit of this method is 0.01 mg of NiFe
2O
4 with a maximum detection error of ±2%. The iron hydroxides react with Ni(OH)
2 to form NiFe
2O
4 and α-Fe
2O
3 through a dehydration reaction in 553 K water. Amorphous iron hydroxide and γ-FeOOH react rapidly, reaching saturated values of the conversion to NiFe
2O
4 within a few hours at 553 K. The dissolved oxygen has no influence on the NiFe
2O
4 formation. The amount of generated NiFe
2O
4 decreases with the reduction of the pH value, due to dissolution of the reactant. The rate of NiFe
2O
4 formation increases with reaction temperature, while the saturated value of formed NiFe
2O
4 decreases.
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