Evaluation of in situelectrodeposition technique in electrothermal atomic absorption spectrometry

Abstract

Conventional electrothermal atomic absorption spectrometric (ETAAS) equipment was extensively modified to enable automated in situ electrodeposition. The original autosampler injection Teflon capillary was replaced by a composite Pt/Teflon capillary which served as an anode in the electrodeposition circuit. Incorporation of a peristaltic pump and of a three-way solenoid under computer control into the sample dispenser circuit provided all necessary steps for automated electrodeposition-ETAAS determination. The automated sequence controlled addition of Pd modifier and of the analyte, electrolysis, withdrawal of spent electrolyte, rinsing, drying and atomization. Performance of the system was evaluated by analyzing Pb in 3% m/v NaCl. Optimization using factorial design yielded 3σ detection limit of 20 pg Pb and reproducibility of 1.0–1.4% (for constant current electrodeposition), these values being superior to the results of conventional ETAAS of Pb in 0.5% m/v NaCl. Sensitivity of Pb determination is not affected by NaCl, NaOH, NaNO₃ and NH₄H₂PO₄, up to 4.6% m/v, demonstrating efficient matrix removal in the electrodeposition step.