An experimental technique of combined thermogravimetric analysis (TGA)-mass spectrometry (MS) was used to study the pyrolysis process during binder removal from a ceramic/binder system. The effect of a fluorocarbon surfactant on the pyrolysis process was also investigated and it was discovered that the surfactant had no significant effect on pyrolysis. A simple paraffin binder system was implemented so as to enhance the effects of the surfactant. The identification of the fragments created during pyrolysis is also discussed.