Laboratory applications for the analysis of PCBs (polychlorinated biphenyls) in environmental matrices such as soil/sediment/sludge and oil/waste oil were evaluated for potential reduction in waste, source reduction, and alternative techniques for final determination. As a consequence, new procedures were studied for solvent substitution, miniaturization of extraction and cleanups, minimization of reagent consumption, reduction of cost per analysis, and reduction of time. These new procedures provide adequate data that meet all the performance requirements for the determination of PCBs. Use of the new procedures reduced costs for all sample preparation techniques. Time and cost were also reduced by combining the new sample preparation procedures with the power of fast gas chromatography. Separation of Aroclor 1254 was achieved in less than 6 min by using DB-1 and SPB-608 columns. With the greatly shortened run times, reproducibility can be tested quickly and consequently with low cost. With performance-based methodology, the applications presented here can be applied now, without waiting for regulatory approval.