Abstract
This paper describes the interaction of a octa (3-chloropropyl)octasilsesquioxane (SS) functionalized with imidazole (SSI) groups, and its subsequent reaction with silver (AgSSI) and hexacyanoferrate (III) (AgHSSI). The materials SS, SSI were characterized by infrared (FTIR); solid state 13C and 29Si nuclear magnetic resonance (NMR). The AgSSI and AgHSSI were characterized by electronic (Uv-Vis) and infrared spectroscopy (FTIR). The AgHSSI was incorporated into a graphite paste electrode and the electrochemical studies were conducted with cyclic voltammetry. The AgSSI system was studied first, followed by the AgHSSI. The spectroscopic studies reveals that preparation was conducted with success. The cyclic voltammogram of AgSSI obtained from a graphite paste electrode modified (50% m/m) exhibited a redox couple with average potential (E?’) of 0.01 V (vs Ag/AgCl(s), KNO3, 1.0 mol L-1; v = 20 mV s-1), attributed to the Ag0/Ag+ redox process. The cyclic voltammogram of AgHSSI with AgHSSI (50% m/m) exhibited a single redox couple, much wider with E?’= 0.14 V, (vs Ag/AgCl(s), KNO3, 1.0 mol L-1, v = 20 mV s-1) attributed to the Fe2+(CN)6/ Fe3+(CN)6 process.
Highlights
Polyhedral oligosilsesquioxanes (POSS) refer to all structures that have the empirical formula (RSiO1,5)n, where R can be a hydrogen or any organic group such as alkyl, methyl, aryl, vinyl, phenyl, arylene, or any organofunctional derivative thereof, n can vary between 4 and 30, but it is usually 6, 8, 10 and 12 (Cordes, Lickiss, & Rataboul, 2010; Lickiss & Rataboul, 2008; Voronkov & Lavrent'yev, 1982)
The AgHSSI was incorporated into a graphite paste electrode and the electrochemical studies were conducted with cyclic voltammetry
The cyclic voltammogram of AgSSI obtained from a graphite paste electrode modified (50% m/m) exhibited a redox couple with average potential (Eθ’) of 0.01 V (vs Ag/AgCl(s), KNO3, 1.0 mol L-1; v = 20 mV s-1), attributed to the Ag0/Ag+ redox process
Summary
Polyhedral oligosilsesquioxanes (POSS) refer to all structures that have the empirical formula (RSiO1,5)n, where R can be a hydrogen or any organic group such as alkyl, methyl, aryl, vinyl, phenyl, arylene, or any organofunctional derivative thereof, n can vary between 4 and 30, but it is usually 6, 8, 10 and 12 (Cordes, Lickiss, & Rataboul, 2010; Lickiss & Rataboul, 2008; Voronkov & Lavrent'yev, 1982). When compared with silica gel, the advantage of using silsesquioxanes modified by covalent attachment of organofunctional groups regards their easy preparation, high sorption capacity and fast adsorption kinetics, in addition to their good chemical stability (Rajec & Hanzel, 2003; Silveira, 2012). Within this context, our interest in the silsesquioxane chemistry is to prepare multifunctional nanostructured materials that can be used as electrochemical sensors. The electrochemical behavior of AgHSSI provide additional information about different species formed during their preparation
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