In occupational and public health there is a need for measurement and speciation of chemicals in ambient air to achieve control of air pollution and minimize health risks. In this work two methods of analysis are developed for the analysis of polycyclic aromatic hydrocarbons (PAHs) and volatile organic compounds (VOCs) under ambient air conditions. Both methods involve the use of thermal desorption techniques with gas chromatography-mass spectrometry (GC-MS). For the measurement of polycyclic aromatic hydrocarbons (PAHs) airborne particulate samples are obtained by collection on small glass fibre filters. The volatile materials from these are thermally desorbed in two stages and transferred to a Gas Chromatograph-Mass Spectrometer analytical system. Results from studies of particulate samples obtained from sites in the region of Uxbridge, Middlesex are reported for eight selected polycyclic aromatic hydrocarbons (PAHs). Measurements on samples obtained directly from vehicle emission sources with the engine used under different running conditions are also reported. In the method of analysis of volatile organic compounds in air, samples are absorbed into 4mm Carbotrap 300 tubes and thermally desorbed and passed into a gas chromatography-mass spectrometry (GC/MS) or gas chromatography (GC) using helium as carrier gas. The Carbotrap absorbers used, show complete absorb/desorb reversibility, are thermally stable and do not react chemically with injected hydrocarbon standards. To demonstrate the value of the method analytical results obtained under ambient air conditions on the Brunel University campus (Uxbridge, Middlesex) are reported. Six selected low molecular weight aromatic hydrocarbons namely benzene, toluene, ethyl benzene and m-, p- and o-xylene are investigated in detail. The concentrations of these compounds were measured and results related to traffic flow rates and meteorological conditions to establish the fact that vehicle exhaust emissions are the main sources of the volatile organic compounds (VOCs) pollution at the collection sites. A study of volatile organic compounds (VOCs) levels in ambient air in Tehran (Iran) in which 55 hydrocarbons are identified is reported. A detailed study is made of the concentrations of the six hydrocarbons benzene, toluene, ethyl benzene and m-, p- and o-xylene because high concentrations of these pollutants can produce potential health problems. It is shown that the nature of the geographical location and the day time temperature play an important part in determining the composition of the mixture of pollutants in Tehran. Samples obtained directly from internal combustion engines with and without catalytic converters are also analysed using the method developed and the results show that there is a large depletion in aromatic hydrocarbons when toluene is reduced to a greater extent than benzene. The analytical method is also used to compare vehicle emissions from engines under cold start and hot start conditions.