Bismuth film electrode prepared in situ on glassy carbon disk surface (abbreviated to BiFE in situ) wasused as working electorode for square-wave adsorption stripping voltammetry (SqW-AdSV) for thedetermination of cadmium (Cd) and lead (Pb) in HEPES buffer (pH = 7.3) and the presence of calceiblue (CB) as a complexing ligand. The influence of the factors on Cd and Pb stripping peak curent (Ip)such as: BiIII concentration, HEPES and CB concentrations, deposition potential and deposition time,adsorptive potential and adsorptive time, the electrode rotating speed, interferents... wereinvestigated. At the deposition potential of -1500 mV, the deposition time of 90 s and the adsorptivepotential of -400 mV, the adsorbent time of 1 s, the method gained high sensitivity (116 ± 6 and 105 ± 5nA/ppb for Cd and Pb, respectively), good reproducibility of the Ip : RSD = 9% and 2% (n = 9) for Cdand Pb, respectively, low detection limit (3s) (1.4 - 1.6 ppb for each metal)
linear correlation bewteenthe Ip and the metal concentration was good in the range of 2 - 50 ppb (R ≥ 0,99).