In this work, a bismuth–antimony film electrode (Bi–SbFE) is reported for the first time as a possible alternative
for electrochemical stripping analysis of trace heavy metals. The Bi–SbFE was prepared in situ on
a glassy carbon electrode and employed in combination with square wave anodic stripping voltammetry
in hydrochloric acid solution (pH 2.0). Several key operational parameters influencing the electroanalytical
response of Bi–SbFE were optimized, such as the different proportions of Sb(III) and Bi(III), pH
value of the measure solution, deposition potential and deposition time. Compared with the bismuthfilm
electrode (BiFE) and antimony-film electrode (SbFE), the Bi–SbFE displayed higher stripping current
response. Under the optimum conditions, the sensor revealed highly linear behavior in the examined concentration
range from 1.0 to 220.0 g L−1, with the detection limit of 0.15 g L−1 for Cd(II), offering good
reproducibility. The method was applied to the analysis of Cd(II) in tap water sample with satisfactory
results.