Premium
Voltammetric Detection of Lead(II) Using Amide‐Cyclam‐ Functionalized Silica‐Modified Carbon Paste Electrodes
Author(s) -
GoubertRenaudin Stéphanie,
Moreau Mathieu,
Despas Christelle,
Meyer Michel,
Denat Franck,
Lebeau Bénédicte,
Walcarius Alain
Publication year - 2009
Publication title -
electroanalysis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.574
H-Index - 128
eISSN - 1521-4109
pISSN - 1040-0397
DOI - 10.1002/elan.200904661
Subject(s) - detection limit , cyclam , amide , mesoporous silica , adsorption , chemistry , calibration curve , carbon paste electrode , acetamide , analyte , electrode , inorganic chemistry , mesoporous material , electrochemistry , materials science , chromatography , organic chemistry , cyclic voltammetry , catalysis , metal
Abstract 2‐(4,8,11‐Triscarbamoylmethyl‐1,4,8,11‐tetraazacyclotetradec‐1‐yl)acetamide (TETAM) derivatives bearing 1, 2, or 4 silylated arms have been synthesized and grafted to the surface of silica gel and ordered mesoporous silica samples. The resulting organic‐inorganic hybrids have been incorporated into carbon paste electrodes and applied to the preconcentration electroanalysis of Pb(II). The attractive recognition properties of these cyclam derivatives functionalized with amide pendent groups toward Pb(II) species and the highly porous structure of the adsorbents can be exploited for the selective and sensitive detection of the target analyte. Various parameters affecting the preconcentration and detection steps have been discussed with respect to the composition and pH of both accumulation and detection media, the nature of the adsorbent (number of silylated groups linking the macrocycle to silica, texture of materials), the accumulation time, and the presence of interfering cations. Under optimal conditions and for 2 min accumulation at open‐circuit, the voltammetric response increased linearly with the Pb(II) concentration in a range extending from 2×10 −7 to 10 −5 M, while a longer accumulation time of 15 min afforded a linear calibration curve between 10 −8 and 10 −7 M with a detection limit of 2.7×10 −9 M which is well below the European regulatory limit of lead in consumption water.