A formulation of the methodology for determining semi-volatile organic emissions from hazardous waste incinerators was subjected to an intensive series of laboratory experiments to determine the viability of the method. Using a selected series of test compounds, a method detection limit was established for GC/MS quantitations of each species. A matrixed-experiment was performed to evaluate the recovery of the test compounds introduced into a flue gas simulation system under two levels of component concentration and mixed with moisture, HCl, SO2, NOx. Low recoveries were measured for pyridine and urethane and will require further study. The methodology was insensitive to the environment variables introduced by the flue gas simulation experiments.