A procedure for speciation and quantitation of Aroclors in capillary gas-liquid chromatography electron capture detector (GC-ECD) chromatograms is described. Four pentachlorobiphenyls (IUPAC no. PCB-87, -110, -118, and -105) and three heptachlorobiphenyls (PCB-183, -180, and - 170) are used as markers of Aroclor 1254 and Aroclor 1260, respectively. The Aroclor content of samples is estimated by comparing the congener composition with U. S. EPA Aroclor reference materials. In this study, the selected congener approach to Aroclor determination is applied to both California marine mussels (Mytilus californianus and M. edulis) and white croaker (Genyonemus lineatus) muscle. Both Aroclor 1254 and Aroclor 1260 were present in these species, and the congener patterns matched the Aroclor reference materials closely. In cases where reporting Aroclors is not appropriate, e.g., highly weathered samples, the method also provides PCB congener data.