In a field evaluation study for semivolatile halogenated organic compounds listed in Title III of the Clean Air Act Amendments of 1990, dynamic spiking experiments using a liquid solution were performed in the field. Two of four quadruple sampling trains were spiked for eight sampling runs. Method 0010 train components were prepared and analyzed in three parts: filter/front halt rinse, XAD-2 resin, and condensate/condensate rinse. Because the results were at variance with results obtained for analytes spiked in laboratory studies and a previous field study, the sample preparation process was investigated in detail. Sample preparation procedures had followed Method 0010, but use of some procedures which were not specifically prohibited by Method 0010 had depressed compound recoveries. To ensure that the sample preparation procedures for Method 0010 train components were clear and unamibiguous, a new protocol to address preparation of Method 0010 train components for Method 8270 analysis was written.