in this project, ultra trace amounts of Cu(II), Pb(II), Cd(II) and Zn(II) were determined by differential pulse adsorptive cathodic stripping voltammetry (DPAdCSV). In addition, the assisted transfer of proton and Cd 2+ were studied at a micro interface of two immiscible electrolyte solutions (ITIES) by cyclic voltammetry. Cadmium and zinc ions were determined by DPAdCSV. This method is based on the selective accumulation of the complexes of Cd(II)-XO and Zn(II)-XO on a HMDE. At the optimized conditions the relationship between peak currents for cadmium(II) and zinc(II) concentration were linear up to 580 and 260 ng/ml, respectively. The detection limits for Cd(II) and Zn(II) were 1.7 ng/ml and 1.8 ng/ml, respectively. In another work, a selective method was presented for the determination of copper(II) based on DPAdCSV on HMDE. The experimental factors were optimized using artificial neural network (ANN). At the optimized conditions, a linear calibration curve was obtained for the concentration of Cu(II) in the range of 1.0-50.0 ng/ml with a detection limit of 0.3 ng/ml Cu(II). A wavelet neural network (WNN) model was proposed for extending the dynamic range of Cu(II). The WNN model consisted of three layers ( 2-8-1 ) with the Morlet mother wavelet transfer function in the hidden layer. The model was able to extend the dynamic range of Cu(II) by 1.8 orders of magnitude. Comparing of WNN and ANN results was demonstrated the superiority of the WNN model relative to ANN model. In the other work the simultaneous determination of two different systems containing Pb-Cd and Cu-Pb-Cd using AdDPCSV were also described. The effect of various parameters on the peak currents was investigated using ANN. The relationship between peak currents for cadmium and lead concentrations were linear over the range of 4.0 -150.0 and 5.0 -150.0 ng/ml, respectively. The limits of detection were 0.98 and 1.18 ng/ml for lead and cadmium, respectively. In the Cu(II)-Pb(II)-Cd(II) system there was intermetallic interaction. Therefore, ANN was utilized to solve this problem. The ANN model was trained for simultaneously determination of concentrations of Cu(II), Pb(II), and Cd(II) ions in the ranges of 1-50, 5-200 and 10-200 ng/ml respectively. The proposed methods were applied to the determination of the above mentioned ions in several real samples.