A new methodology was developed using a Thermo-Gravimetric Furnace coupled to a Fourier Transform Infrared Spectrometer (TGF-FTIR) to study the low temperature treatment of waste lubricating oils. The sample was heated from room temperature to a final temperature of 1,000°Cat an initial heating rate of 3 °C/min, to slow down the oxidative pyrolysis process allowing for the events taking place to be observable. It was found that the majority of the process in terms of weight loss and gas-phase evolution was over by 650 °C, and thus, the remainder of the sample heating was accomplished at a rate of 5 °C/ min. The sample was kept at a temperature of 1,000 °C for 60 minutes in order to allow the remaining solid material to achieve a state of equilibrium (necessary for the solid morphological study). The applicability of TGF-FTIR using this methodology to research in the environmental field was proven to be quite successful, since it allowed for precise control over environmental conditions while simultaneously allowing for data gathering on both IMPLICATIONS Thermal treatment of waste oils is becoming an attractive disposal option. However, the information on the thermal behavior of wastes and their generated pollutants in industrial-size reactors is scarce due to the complexity and the lack of accessibility of such systems to detailed experimental studies that are capable of fundamental interpretation. The research described provides a reliable and practical approach to determine events taking place in waste treatment systems. Specifically, it would be applicable when pyrolysis, oxidative pyrolysis and oxidation processes are involved (as is the case in actual incineration systems). Design of new, practical waste combustion systems depends on the rate and extent of these processes. The proposed method will allow for studying specific environmental concerns such as effect of various process parameters (heating rate, residence time, temperature) on release, formation or destruction of gaseous pollutants. Such information would help to design practical systems in which waste oils were thermally treated.sample weight and gas-phase evolution. The developed methodology proved to be reliable, giving repeatable results. The information gathered was used to understand and explain the evolution of the waste oil from initial liquid state to a final solid ash state. It was accomplished in four steps, including (1) release of moisture/light hydrocarbons, (2) bulk volatilization of hydrocarbons, (3) solid material deposition, and (4) solids oxidation.