Coal chemical wastewater (CCW) with the features of high toxicity and poor biodegradability is a big issue in environmental remediation, posing a great threat to aquatic ecosystems and to human beings. Such complex molecular mixtures are notoriously difficult to characterize without initial physical separation. Herein, we present the 3D diffusion
ordered spectroscopy (DOSY) analysis for CCW using DOSY-COSY and DOSY-HSQC methods, the advantages of this strategy have been demonstrated in the analysis of mixtures of aliphatic oxygenates and aromatic compounds, before being implemented on a genuine CCW sample in this study. The results showed that 3D DOSY is a robust and reliable tool for providing superior resolution and virtual separation of complex pollutants, and can be used as a general approach for structural elucidation.