Preconcentration of cyanide from dilute solutions was carried out by co-deposition of Ag2S and AgCN on the surface of a rotating silver electrode. In the absence of sulphide in the sample, no deposition of AgCN appears to take place. Subsequent cathodic stripping was performed with both differential pulse voltammetry and square-wave voltammetry. Detection limits for cyanide of 0.35 and 1.2 mu M were found for these two methods, respectively. (C)2000 Elsevier Science B.V. All rights reserved.