Antimony powder-modified carbon paste electrodes for electrochemical stripping determination of trace heavy metals

Highlights: → New antimony powder-modified carbon paste electrode. → Combination of specific properties of carbon paste substrate and metallic antimony. → No requirement of using toxic antimony(III) salts. → Electrochemical stripping determination of trace heavy metals at ppb levels. → Anodic stripping voltammetric and stripping chronopotentiometric measurements. - Abstract: A new type of the antimony electrode based on a carbon paste bulk-modified with antimony powder (Sb-CPE) is presented for the determination of cadmium(II) and lead(II) ions at the microgram-per-liter concentration level, when using square-wave anodic stripping voltammetric or stripping chronopotentiometric protocol. The Sb-CPE was prepared by mixing fine antimony powder, carbon powder, and silicon oil, thus combining typical features of the carbon paste material with specific electrochemical properties of antimony. Key-operational parameters, including the amount of antimony powder in the carbon paste mixture, effect of the deposition potential and deposition time, were optimized and electroanalytical performance of the Sb-CPE in nondeaerated solution of 0.01 M hydrochloric acid (pH 2) was compared with related bismuth powder-modified carbon paste electrode (Bi-CPE) and with in situ prepared antimony film carbon paste electrode (SbF-CPE). The electrode of interest exhibited well-developed signals and highly linear calibration plots for both metal ions tested. In addition, favorable limits of detection were achieved; namely: 1.4 μg L-1 for Cd(II) and 0.9 μg L-1 for Pb(II). The applicability of the new electrode was demonstrated on the analysis of tap water (spiked sample). Besides voltammetric measurements, the Sb-CPE was preliminary tested also under chronopotentiometric stripping mode in deoxygenated solutions, revealing also an excellent electroanalytical performance.