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In this study, a nickel ferrite (NiFe₂O₄) system was constructed to purify a phenol solution in water. During the process, the influences of several critical operating parameters including the NiFe₂O₄ amount, PS dosage, MW power, initial pH value, and different natural water anions were systematically studied. The results indicated that the constructed system performed excellently regarding the removal efficiency (97.74%) of phenol within 30 min. Meanwhile, the influence of co-existing anions such as Cl⁻, NO₃⁻, H₂PO₄⁻, and HCO₃⁻ was also studied, which displayed an inhibiting action on phenol degradation, while HA facilitated it. To explore the reaction mechanism of this system, major free radical quenching experiments were conducted, and it was confirmed that both SO₄•⁻ and HO• were primary radicals. Moreover, stability experiments confirmed the apt stability of the NiFe₂O₄ system. Besides, the mineralization and toxicity analysis performed during phenol degradation also confirmed the superiority of the as-constructed system. Furthermore, the possible degradation mechanism of phenol was proposed. Hence, this system could be applied in advanced wastewater treatment.