In this paper the relative advantages of using square wave adsorptive stripping voltammetry in combination with a mercury film electrode as the working electrode were assessed. it was found that the resulting technique is fast, sensitive, offers excellent discrimination against the background current and can be used without deoxygenation of the sample; the analytical applications of the technique are demonstrated for the determination of Ni(II) with a limit of detection of 0.85 nmol l-1 and a linear range of 3 orders of magnitude (for 60 s preconcentration) and for the determination of Cu(II) in the nmol l-1 concentration level in the presence of dissolved oxygen.