The purpose of this investigation was to evaluate the application of a spark-source mass spectrograph equipped with a spinning-electrode system for the study of various high molecular-weight materials derived from coal. Eight structural types having molecular weights from 178 to 252 corresponding to those substances previously seen in an electron-impact mass spectrum of the coal-tar pitch were affirmed by this technique. Easily interpreted mass spectra of phenanthrene, anthracene, and chrysene were obtained by the spinning-electrode system. Mass spectra obtained from synthetic mixtures of anthracene and chrysene demonstrated that the technique is applicable for semiquanitative analysis.