Operational characteristics have been determined for fused silica capillary column (FSCC) GC/MS as applied to 'extractable' priority pollutants. Chromatographic data show excellent relative retention time (RRT) intralaboratory precision and interlaboratory accuracy when multiple internal standards are employed. Potential chromatographic problems, such as column overload and 'double peaking', are addressed. Potential quantitative problems, such as saturation, are discussed. For certain aromatic priority pollutants interlaboratory RF agreement was observed. This was noted as perhaps the most important property of FSCC GC/MS analysis when the multiple internal standard approach is utilized. Determinations of extractable priority pollutants are directly compared for packed column GC/MS and FSCC GC/MS analysis of separate and composited extracts. For six extracts analyzed in triplicate, the latter configuration was shown to produce more consistent results. In view of the superior analysis logistics of composite extract FSCC GC/MS analysis, this approach was established as the preferred method for the analysis of priority pollutants classified as extractable.