A novel nanostructured composite formed by interaction of copper octa(3-aminopropyl)octasilsesquioxane with azide ligands: Preparation, characterization and a voltammetric application

Author(s)

do Carmo, Devaney Ribeiro ^[1] ; Paim, Leonardo Lataro ^[2] ; Metzker, Gustavo ^[3] ; Dias Filho, Newton Luiz ^[1] ; Stradiotto, Nelson Ramos ^[2]

Affiliation

^[1] UNESP, Fac Engn Ilha Solteira, Dept Quim & Fis, BR-15385000 Ilha Solteira, SP - Brazil

^[2] UNESP, Inst Quim Araraquara, BR-14801970 Araraquara, SP - Brazil

^[3] Univ Sao Paulo, Inst Quim Sao Carlos, BR-13566590 Sao Carlos, SP - Brazil

• Document type: Journal article
• Source: Materials Research Bulletin; v. 45, n. 9, p. 1263-1270, SEP 2010.
• Web of Science Citations: 9

Abstract

This study presents the preparation, characterization and application of copper octa(3-aminopropyl)octasilsesquioxane following its subsequent reaction with azide ions (ASCA). The precursor (AC) and the novel compound (ASCA) were characterized by Fourier transform infrared spectra (FTIR), nuclear magnetic resonance (NMR), electron paramagnetic resonance (EPR), scanning electronic microscopy (SEM), X-ray diffraction (XRD), Thermogravimetric analyses and voltammetric technique. The cyclic voltammogram of the modified graphite paste electrode with ASCA (GPE-ASCA), showed one redox couple with formal potential (E(1/2)(ox)) = 0.30 V and an irreversible process at 1.1 V (vs. Ag/AgCl; NaCl 1.0 M; v = 20 mV s(-1)). The material is very sensitive to nitrite concentrations. The modified graphite paste electrode (GPE-ASCA) gives a linear range from 1.0 x 10(-4) to 4.0 x 10(-3) mol L(-1) for the determination of nitrite, with a detection limit of 2.1 x 10(-4) mol L(-1) and the amperometric sensitivity of 8.04 mA/mol L(-1). (C) 2010 Elsevier Ltd. All rights reserved. (AU)