A new analytical method for determination of TMLead and TELead in air is suggested. A simple system for preconcentration and collection of the alkyllead vapours on iodized glass fibre carbon filters is described. Experimental evidence for the use of MIBK as solvent for the alkyllead iodides formed in the collector and their extraction by diluted hydrochloric acid is given. Additionally, optimal conditions for sampling, sample treatment and storage are presented, based on model experiments with model samples. Finally, real samples from the working environment of an oil refinery are analysed.