The paper focuses on advanced oxidation process of Fe²⁺ activated persulfate (PS) coupled with activated carbon adsorption which was originally applied to treat bio-treated coking wastewater. The effects of PS dose, Fe²⁺ dose and initial pH in Fe²⁺/PS system on the treatment efficiency of bio-treated coking wastewater were investigated at the TOC concentration of 86.4mg/L and chroma of 338times in raw wastewaters. The results indicated that the removal rates of chroma and TOC were 87.17% and 68.16%, respectively, under the condition of 1.5mmol/L PS, 4mmol/L Fe²⁺, not adjusted pH value (pH=8) when reaction time was 60minutes. The advanced adsorption treatment on effluent of Fe²⁺/PS system was also carried out by two kinds of granular activated carbon A and B. The results showed that the activated carbon B had remarkable better adsorption performance, which could further eliminate residual persulfate by Fe²⁺/PS system. When the dose of activated carbon B was 15g/L, and reaction time was 120minutes, the effluent chroma and TOC concentration reached 14times and 11.86mg/L, respectively. After the treatment of Fe²⁺ activated persulfate oxidation coupled with activated carbon adsorption on biological treated coking wastewater, the total removal rates of chroma and TOC reached 95.86% and 86.27%, respectively. The results of three dimensional fluorescence spectra analysis for bio-treated coking wastewater, Fe²⁺/PS system effluent, and activated carbon adsorption effluent showed that Fe²⁺/PS system can decompose humic acid-like compounds in wastewater, and activated carbon adsorption may further remove residual humic acid-like compounds in wastewater.