The replacement of fossil-based fuels by renewable fuels (biofuels) was proposed in the IPCC report, as an alternative to reduce greenhouse gas emission and reach out to a low-carbon economy. On this perspective, the Brazilian government had implemented a renewable energy program based on the use of ethanol in the transport sector. This work evaluates the scenario of pollutant gas emissions and particulate material that comes from the biomass burning process involved in ethanol production cycle, in the city of Campos dos Goytacazes, Brazil. The gases and particulate material emitted by sugarcane and bagasse burning processes-the last one in energy co-generation mills-were analyzed. A laboratory-controlled burning of both samples was realized in an oven with temperature ramp from 250 to 400 °C, at a regular rate of 50 °C. The gas samples were collected directly from the oven's exhaust pipe. The particulates obtained were the residual material taken out of the burned samples: a powder with the aspect of soot. A photoacoustic spectroscopy system coupled with quantum cascade laser and electrochemical analyzers was used to measure the emission of polluting gases such as N2O, CO2, CO, NOx (NO, NO2), and SO2 in ppmv range. Fluorescent X-ray spectrometry was applied to evaluate the chemical composition of particulate material, enabling the identification of elements such as Si, Al, Ca, K, Fe, S, P, Ti, Mn, Cu, Zn, Sc, V, Cu, and Sr.