Work described in this thesis contains the results on the study of volatile organic compounds (VOCs) in landfill gas from seven landfill sites in the western region of Melbourne, Victoria, Australia. Sampling methods including sampling with adsorption tubes, tedlar bags and cryogenic trapping were investigated and analytical systems were developed using adsorption tubes with solvent or thermal desorption followed by analysis of VOCs using gas chromatography with mass selective detection (GC/MS).