Voltammetric methods are very suitable, versatile and rapid techniques for simultaneous determination of metals in complex matrices. The present work, determination of Cu(II), Sn(II), Sb(III), Tl(I), and Pb(II) by square-wave anodic-stripping voltammetry and Cr(VI) by square-wave adsorptive-stripping voltammetry, is an interesting example of the possibility of simultaneous determination of each single element in food and environmental samples, even in the presence of reciprocal interference. Dibasic ammonium citrate, pH 6.3 or 8.2, was employed as supporting electrolyte. The voltammetric measurements were carried out using a stationary hanging mercury drop electrode as working electrode and a platinum electrode and an Ag|AgCl|KCl(sat) electrode as auxiliary and reference electrodes, respectively. The analytical procedure was verified by analysis of standard reference materials--wholemeal BCR-CRM 189, wheat flour NIST-SRM 1567a, rice flour NIST-SRM 1568a, estuarine sediment BCR-CRM 277, river sediment BCR-CRM 320, and Montana soil with moderately elevated traces NIST-SRM 2711. Precision and accuracy, expressed as relative standard deviation and relative error, respectively, were generally below 6% whereas limits of detection for each element were below 0.069 microg g(-1). In the presence of reciprocal interference the standard addition method considerably improved the resolution of the voltammetric technique, even for very high element concentration ratios. After being set up on the standard reference materials the analytical procedure was transferred and applied to commercial samples of meal and soil samples taken from sites devoted to agricultural practice. A critical comparison with graphite furnace atomic-absorption spectroscopy is also discussed.