Anodic stripping voltammetry (ASV) performed in a twin-electrode thin-layer cell eliminates Cu-Zn and Cu-Cd Intermetallic interferences that are often encountered in ASV. Cu is first exhaustively deposited on one electrode, and then the second electrode is used to complete the Zn and/or Cd determination. Intermetallic interferences are circumvented since the interfering constituents are deposited on different working electrodes. Effects of increasing Cu concentration on the Cd and Zn stripping peaks are shown. Linear calibration curves for Cd and Zn (13 to 130 ppm) are obtained from standard solutions in which Cu2+ concentrations vary from 16 to 76 ppm. The feasibility of determining Pb, Cd, Zn, and Cu simultaneously by anodic stripping voltammetry with no intermetallic interferences is enhanced with the twin-electrode thin-layer cell. © 1979, American Chemical Society. All rights reserved.