The organic solvents use in automotive painting process, implies in great amounts of Volatile Organic Compounds (VOC’s) emissions to the environment and mainly to the atmosphere. Many of these compounds are extremely toxic, harmful to health, representing danger to workers, when observed in any industrial process and the environment health, in these compound emission case through chimneys, treated as volatile organic compounds emission. In this study, concentrations were determined as volatile organic compounds, related to propane, in an agricultural machines and harvester automaker plant, which uses many paint types from two manufacturers, BASF and PPG. Results were compared to the standard limit values of the Resolution 054/06-SEMA, in vigor at Paraná State, that controls, catalogue and limits any pollutant type, imposing limits and work concentration ranges. Some corrective measures were taken to adjust the plant painting process, the most important changes were: painting and drying line exhaust cleaning, painting and drying booth exhaust system swaying, water change from the painting booth, paint apply electromagnetic efficiency study using SPRAY pistol, sludge quantification along the painting process, painters team training to reduce the solvent use in the pistols cleaning and high solid contents paint evaluation and implant to the process. In this study the Mass Balance Methodology was used to quantify the production and the generated residues, and comparatively, the F.I.D technique, to verify possible inconsistencies in the measuring process of the methodology.