Abstract
Atomic layers of antimony were electrodeposited onto glassy carbon electrode in overpotential region. The antimony deposition was characterized by chronocoulometry and scanning electron microscopy. Based on the excellent electrochemical properties of the glassy carbon/antimony system, a simple method was developed for rapid and reliable determination of ultra-trace Sb(V) by square-wave anodic stripping voltammetry. The key operational parameters of influencing the electroanalytical response of Sb, such as deposition potential, deposition time, and composition of the measurement solution, were investigated. Under the optimized condition, the method provided a linear calibration ranging from 1 to 16pgL−1 with a respective correlation coefficient of 0.9906. The detection limit was 1.64fmolL−1, which is the lowest ever reported for an electroanalytical technique and one of the lowest analytical methods for Sb(V) determination. The relative standard deviation for a Sb(V) solution (5pgL−1) was 3.2% for eight successive assays. Finally, the method was applied to the determination of antimony in tap water and compared with inductively coupled plasma mass spectrometry technique.
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