In this work, the applicability of H-point standard addition method (HPSAM) to the kinetic voltammetry
data is verified. For this purpose, a procedure is described for the determination of Sb(III) and Sb(V) by
adsorptive linear sweep voltammetry using pyrogallol as a complexing agent. The method is based on the
differences between the rate of complexation of pyrogallol with Sb(V) and Sb(III) at pH 1.2. The results
show that the H-point standard addition method is suitable for the speciation of antimony. Sb(III) and
Sb(V) can be determined in the ranges of 0.003–0.120 and 0.010–0.240 g mL−1, respectively. Moreover,
the solution is analyzed for any possible effects of foreign ions. The obtained results show that the HPSAM
in combination to electroanalytical techniques is a powerful method with high sensitivity and selectivity.
The procedure is successfully applied to the speciation of antimony in water samples.