In this thesis, stripping voltammetry method in conjunction with chemometrics methods was presented for individual or simultaneous determination of cations of Cu(II), Mo(VI), Bi(III), V(V). In the first part one reliable and sensitive procedure for the simultaneous determination of trace levels of copper and molybdenum is proposed. The effect of chemical and instrumental parameters on the sensitivity and selectivity were studied. A standard addition method was utilized for the analysis of voltammogram data, under the optimal conditions. The linear dynamic range was achieved over the range of 2.0 – 70.0 and 0.8 – 80.0 ng/ml and the detection limits of 0.3 and 0.1 ng/ml for Cu(II) and Mo(VI), respectively. In part two a reliable and very sensitive procedure for the determination of ultra trace of molybdenum is proposed. Under optimial conditions the relationship between the peak current and molybdenum concentration is linear in the range of 0.010 – 21.0 ng/ml. The limit of detection was found to be 0.006 ng/ml. The method was applied for the determination of molybdenum in some real samples include water samples, plant foodstuff, and certified steel reference materials. In part three a new method is proposed for the determination of bismuth and copper in the presence of each other based on adsorptive stripping voltammetry of complexes of Bi(III)-chromazorul-S and Cu(II)-chromazorul-S at a hanging mercury drop electrode. Copper is an interferent element for the determination of Bi(III) because, the voltammograms of Bi(III) and Cu(II) overlapped with each other. Continuous wavelet transform (CWT) was applied to separate the voltammograms. In this regards, wavelet filter, resolution of the peaks and the fitness were optimized to obtain minimum detection limit for the elements. It was realized that copper imposes a matrix effect on the determination of Bi(III) and the standard addition method was able to cope with this effect. In part four a procedure is presented for the simultaneous determination of ultra trace amounts of vanadium and molybdenum based on adsorptive cathodic stripping voltammetry. Under the optimized conditions linear dynamic range for V(V) and Mo(VI) are in the range of 0.3-24.0 and 0.1-30.0 ng/ml respectivly. Detection limits of 0.1 and 0.08 ng/ml were achieved for V(V) and Mo(VI), respectively.