Abstract: The anaerobic/aerobic（A/O） treatment process was an important process for linking pretreatment and deep treatment of coaltoliquids（CTL） wastewaterTherefore，in this study，the variation characteristic of DOM in A/O treatment process of CTL wastewater has been analyzed in deepThe purpose of this paper was to evaluate the treatment efficiency of A/O process，clarify the variation characteristics of DOM，select the characteristic pollutants after A/O treatment and provide theoretical basis and pertinent suggestions for subsequent deep treatmentWater samples were analyzed by GC/MS，resin fractionation，fluorescence spectroscopy and PARAFAC modelGC/MS experimental analysis revealed that A/O process could partially remove DOM in CTL wastewaterThe DOM fractionation results showed that wastewater were mainly hydrophobic substances before and after A/O treatment，but the compositions changedThe fluorescence spectrum analysis results showed that the A/O process could effectively remove organics with fluorescence response in humic acid and fulvic acid region in DOMOn the other hand，EEM conjunction with PARAFAC model could precisely monitor organic pollutants evolutionsIn summary，the A/O process could effectively remove the DOM from the coaltoliquid wastewater，and the removal of phenol and esters should be strengthened in the subsequent deep treatment