Elucidation of interference mechanisms caused by iron on stibine electrochemical generation by differential pulse anodic stripping voltametry. A case study

The interference effect caused by the presence of iron – both (II) and (III) oxidation states – on the electrochemical generation of SbH3 has been characterized. Interference from Fe(III) was more severe than for Fe(II). Total signal suppression was obtained for a Fe(III) : Sb(III) concentration ratio of 5 : 1, whereas a 40% suppression was obtained for Fe(II). A mechanism is proposed based on the results obtained by differential pulse anodic stripping voltametry. The standard conditions used for the hydride electrochemical generation were simulated in the differential pulse anodic stripping voltametry measurements in order to achieve valid conclusions. The reduction of Fe(II) onto the cathode surface prevents the formation of stibine avoiding the recombination of Sb0 with the hydrogen atoms adsorbed on the surface. The mechanism by which the Fe(III) interferes on the stibine formation is related to the co-deposition of the iron and antimony that also avoid the further recombination of the Sb0. The formation of a specie of stoichiometry not determined (probably 1 : 1) on the cathode surface may justify the larger interference effect observed for the Fe(III).