A field experiment for the comparison of the efficiency of canisters and adsorption multibed tubes for sampling atmospheric highly volatile hydrocarbons at ppbv levels is described. The canister was passivated by the Summa process and the adsorption tubes were filled with Carbotrap C, Carbotrap B and Carbosieve S-III. The sampling with the adsorption tubes was performed at ambient temperature and at -10°C. The highest concentrations were generally obtained with canisters but these results are very similar to those obtained with refrigerated multibed adsorption tubes. Both methods appear to be equivalent for most of the highly volatile hydrocarbons encountered in moderately polluted urban areas. In contrast, sampling with ambient temperature tubes provides lower concentrations. This study has also shown that K2CO3 drying efficiently removes humidity from air samples allowing the obtention of reliable concentration data on highly volatile hydrocarbons at ppbv levels. These drying tubes can easily be re-conditioned and tested for blanks and memory effects, which greatly facilitates the control of external contamination and sample cross-contamination.