Abstract：This study investigated the treatment efficiency of activated carbon adsorption， coagulation precipitation， ozonation and their combination process on the effluent from a full-scale biological coking wastewater treatment plant. Several methods were employed to characterize the solution properties， including molecular weight distribution， UV-vis spectra， excitation-emission-matrix spectroscopy （EEM） and GC/MS. Results showed that the optimal combination of advanced wastewater treatment was ozonation-coagulation-adsorption， and the optimal reaction conditions predicted by response surface model were： ozone oxidation reaction time of 62.56 min， polymeric ferric sulfate （PFS） dosage of 0.87 g·L-1， activated carbon dosage of 1.10 g·L-1. Under these conditions， 98.29% of the total organic carbon （TOC） was removed. The resultant relative deviation was 0.45% comparing to the simulated value of 98.74%. Selective separation and transformation on pollutants was shown for activated carbon adsorption， coagulation-precipitation and ozone oxidation. The combined process can effectively remove residual organic compounds， UV254 and fluorescent substances in the secondary effluent. There were enhancement feasibility between water quality and treatment process.