Thermochemical processes (pyrolysis and gasification) are alternatives that minimize and convert fuel derived from solid urban waste (CDRSU) into energy, as combustible gases such as CO, H2 and C1-C6 and other non-combustible gases can be generated fuels: CO2, N2, O2, etc. Therefore, this work reports for the first time a method for the simultaneous determination of H2, O2, N2, CO, CO2, CH4, C2H2, C2H4, C2H6, C3H4 (propadiene and propyne), C3H6, C3H8 and C4H10 (n-butane and iso). -butane) by gas chromatography (GC) using thermal conductivity (DCT) and flame ionization (DIC) detectors. GC/DCT/DIC separations were obtained in a capillary column (0.32 mm internal diameter, 30 m long and 15 µm porous film layer thickness). The method was optimized and validated according to the protocols recommended by the National Institute of Metrology, Standardization and Industrial Quality (INMETRO) in Brazil. Under the optimized chromatographic conditions, the determination of the number of moles of the analytes ranged from 1.410 5 to 4.110 4 moles with a value of r 0.99 in its linear range and the limits of quantitation ranged from 1.410 5 to 2.710 4 mols (depending on the analyte). Furthermore, it was demonstrated that the method developed by CG/DCT/DIC can be applied to quantify these analytes during the pyrolysis process of CDRSU, PET bottles and PS cups, as it showed high accuracy, with recoveries ranging from 98-101%, and high precision, with a relative standard deviation of less than 2%.