Synthesis and structural characterization of new macrocyclic ester. study as an immobilization agent for determination of lead by anodic stripping voltammetry

Juan F. Torres, Andreas Reiber, Mario Macías, Olimpo García-Beltran, Edgar Nagles, John Hurtado

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1 Scopus citations

Abstract

New macrocyclic ester (L) was yielded through reaction of catechol with isophthaloylchloride and isolated as white solid, air stable at room temperature. L was characterized by melting point, mass spectra, FTIR and NMR (1H, 13C) spectroscopy. The molecular structure was determined by single-crystal X-ray diffraction. The macrocyclic compound was evaluated to determine ultra-trace concentrations of Pb (II) by anodic stripping voltammetry in the presence of Cd(II). The method is based on the formation of a complex between lead and the macrocyclic ester, immobilized on a vitreous carbon electrode, allowing the oxidation of lead by voltammetric scan, using square wave modulation method. Anodic peak current was observed at -0.20 V for Pb(II). Under the best experimental conditions (pH 4.0; L concentration 10.0 mmol L-1; accumulative potential (Eacc) -0.8 V and accumulative time (tacc) of 60 s) anodic peak current was proportional to the Pb (II) concentration up to 80.0 μg L-1, with a detection limit (3σ) of 0.33 μg L-1. The proposed method was validated by determining Pb(II) in model solution with ultra-pure water with satisfactory results.

Original languageEnglish
Pages (from-to)3109-3119
Number of pages11
JournalInternational Journal of Electrochemical Science
Volume12
Issue number4
DOIs
StatePublished - 1 Apr 2017

Bibliographical note

Publisher Copyright:
© 2017 The Authors.

Copyright:
Copyright 2017 Elsevier B.V., All rights reserved.

Keywords

  • Anodic stripping voltammetry
  • Lead
  • Macrocyclic ester
  • Modified electrode

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