The pyrolysis of nitrosamines in a modified Hall microelectrolytic conductivity system provides the basis for a highly selective and sensitive determination method. Under the conditions specified, the response of this detector system to nitrosamines is at least 10(7) times greater than that for n-hexane. The influence of several operational parameters on the response of the detector to nitrosamines was studied. For open-chain nitrosamines, the detection limit is 50 pg and the response is linear up to at least 200 ng.