This study was conducted by the University of Southern California group to provide methods for the analysis of coal liquefaction wastes from coal conversion processing plants. Several methods of preliminary fractionation prior to analysis were considered. The most satisfactory method is that employing column separation, using macroreticular absorbent resins and dividing the wastewaters into hydrophobic and hydrophilic fractions. By subsequent use of ion exchange resins, each fraction was subdivided into acid, neutral, and basic subfractions. These subfractions yielded materials suitable for gas chromatography/mass spectrometric analysis performed by Finnigan Company. To identify the numerous compounds contained in each subfraction produced by the resin chromatographic separation, a GC/MS equipped with a computer library of mass spectra of 31,331 compounds was used. The peaks eluting from the GC can be individually and immediately analyzed for their spectra which can be compared to those in the computer library.