This chapter describes good potential for H2 production through gasification of refuse derived fuel in comparison to Clean Wood gasification. Concentration profiles of higher order hydrocarbons were presented which provided insight into the likely reaction sequences occurring during the gasification of the samples. Many companies are turning to gasification of Municipal solid waste, biomass and mixtures of these to produce fuels and chemicals. Gasification is a process for converting solid carbonaceous materials to a combustible. The products of gasification exit the furnace and are sampled using a rapid syringe capture technique that condenses moisture from the gas evolution products for subsequent gas chromatograph analysis. The equipment consists of an Instrument Specialists Temperature Programmer Interface/Thermal Analyzer that can regulate the temperature and heating rate of the quartz furnace in the Dupont 951 Thermogravimetric Analyzer. A more reactive sample would begin decomposition earlier and possess lower global activation energy.