On the basis of laboratory experiments with model mixtures, the steps in the de novo synthesis of halogenated compounds were studied. The study was performed using a thermobalance to evaluate the temperature of the maximum rate and the kinetics of the decomposition of the materials in the presence of air. The effect of the presence of CuCl2 and CuO with an atmosphere of HCl was studied. Analysis of the volatiles and solids after combustion in a horizontal furnace confirms the presence of organochloride compounds (including PCDD/F) at various temperatures. With the procedure that we followed, combustion is separated from pyrolysis, and it is possible to analyze the essential factors involved in the combustion process.