Voltammetric Behavior of a Chemically Modified Silsesquioxane with 4-Amino-5-Phenyl-4h-[1,2,4]-Triazole-3-Thiol and its Application for Detection of L-Dopamine

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Silsesquioxane organofunctionalized with 4-amino-3-hydrazino-5-mercapto-1,2,4-triazole: preparation and subsequent reaction with silver and potassium hexacyanoferrate(III) for detection of l-cysteine

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Nanoparticles of octakis [3-(3-amino-1,2,4-triazole)propyl] octasilsesquioxane as ligands for Cu(II), Ni(II), Cd(II), Zn(II), and Fe(III) in aqueous solution

Nanoparticles of octakis[3-(3-amino-1,2,4-triazole)propyl]octasilsesquioxane (ATZ-SSQ) were tested as ligands, for transition-metal ions in aqueous solution with a special attention to sorption isotherms, ligand-metal interaction, and determination of metal ions in natural waters. The adsorption potential of the material ATZ-SSQ was compared with related [3(3-amino-1,2,4-triazole)propyl]silica gel (ATZ-SG). The adsorption was performed using a batchwise process and both organofunctionalized surfaces showed the ability to adsorb the metal ions from aqueous solution. The Langmuir model was used to simulate the sorption isotherms. The results suggest that the sorption of these metals on ATZ-SSQ and ATZ-SG occurs mainly by surface complexation. The equilibrium condition is reached at time lower than 3 min for ATZ-SSQ, while for ATZ-SG is only reached at time of 25 min. The maximum metal ion uptake values for ATZ-SSQ were higher than the corresponding values achieved with the ATZ-SG. In order to obtain more information on the ligand-metal interaction of the complexes on the surface of the ATZ-SSQ nanomaterial, ESR study with various degrees of copper loadings was carried out. The ATZ-SSQ was tested for the determination (in flow using a column technique) of the metal ions present in natural waters. (C) 2007 Elsevier B.V. All rights reserved.

Determination of copper in different ethanolic matrices using a chloropropyl silica gel modified with a nanostructured cubic octa(3-aminopropyl)octasilsesquioxane

The chloropropyl silica gel was modified with octa(3-aminopropyl) octasilsesquioxane and characterized by Fourier transform infrared (FTIR) spectroscopy, nuclear magnetic resonance (NMR), spectroscopies, and surface and area porosity. The specific sorption capacity of metallic ions (Cu2+ and Ni2+) increases in the following solvent order: water < ethanol 42% < ethanol < ketone. The high values of the constant (K) in the order of 103 L mol-1 suggested the high adsorbent capacity of the modified silica (SGAPC) for Cu2+ and Ni2+. SGAPC was applied to a separation column and shows recoveries of around 100% of copper in samples of sugar cane spirit, vodka, ginger brandy, and ethanol fuel. © 2013 Devaney Ribeiro Do Carmo et al.

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

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.

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

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Voltammetric Behavior of a Modified Electrode With Azide Copper Octa(3-Aminopropyl)Octasilsesquioxane Composite in the Oxidation of Ascorbic Acid

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

A new hybrid polyhedral cubic silsesquioxane chemically modified with 4-amino-5-(4-pyridyl)-4H-1,2,4-triazole-3-thiol (APTT) and copper hexacyanoferrate(III) for voltammetric determination of nitrite

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

A Silsesquioxane Organically Modified with 4-Amino-5-(4-pyridyl)-4H-1,2,4-triazole-3-thiol: Thermal Behavior and Its Electrochemical Detection of Sulfhydryl Compounds

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Voltammetric behaviour of a modified electrode with azide copper octa(3-aminopropyl)octasilsesquioxane composite in the oxidation of ascorbic acid

A novel nanostructured composite, azide copper octa (3-aminopropyl)octasilsesquioxane (ASCA) was incorporated into a graphite paste electrode and the electrochemical studies were conducted with cyclic voltammetry. The cyclic voltammogram of the modified graphite paste electrode with ASCA (GPE-ASCA), showed one redox couple with formal potential (E  ) = 0.30 V and an irreversible process at 1.1 V (vs Ag/AgCl; NaCl 1.0 mol L-1 ; v = 20 mV s-1 ). The redox couple with (E  ) = 0.30V presents an electrocatalytic response for determination of ascorbic acid. The modified electrode gives a linear range from 1.010-4 – 1.010-3 mol L-1 (r = 0.998) for the determination of ascorbic acid with detection limit of 6.910-5 mol L-1 and standard deviation of 2.3% for n = 3 . The amperometric sensitivity was 122.1 mA/mol L-1 for ascorbic acid. The application this electrode was tested and ascorbic acid in three commercial pharmaceutical product (Cebion, Cewin and Redoxon) have been determined.

Voltammetric Study of a Cubic Silsesquioxane Organically Modified with Imidazole and their Subsequent Reaction with Cadmium and Hexacyanoferrate (III)

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

A cubic silsesquioxane modified with purpald®: Preparation, characterization and a voltammetric application for determination of sulfite

A novel composite formed by interaction of a octa(3-chloropropyl)octasilsesquioxane modified with Purpald®, and its subsequent reaction with silver and hexacyanoferrate (III) (AgHSP), was synthesized and initially characterized by Fourier transform infrared spectra (FTIR) and cyclic voltammetry. The cyclic voltammogram of the modified graphite paste electrode with AgHSP, showed one redox couple with formal potential Eθ'=0.64V (vs Ag/AgCl, KNO3, 1.0 mol L-1; v = 20 mV s-1), attributed to the Fe2+(CN)6/ Fe3+(CN)6 process. The redox couple presents an electrocatalytic response for determination of sulfite. The modified electrode showed a linear response from 7.0×10-5 to 1.0×10-3 mol L-1 with the corresponding equation Y(μA) = 18.05 + 29.983×103 [sulfite], and a correlation coefficient of r=0.999. The method showed a detection limit of 0.115×10-4 mol L-1 with a relative standard deviation of ± 4% (n = 3) and amperometric sensitivity of 29.983×10-3A mol L-1. The modified electrode showed a excellent stability and good reproducibility during experiments. © 2013 by ESG.

A cubic silsesquioxane modified with purpald (r) : preparation, characterization and a voltammetric application for determination of sulfite

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Quantificação eletroquímica de analitos de interesse ambiental e biológico, empregando novos materiais preparados a partir de silsesquioxanos funcionalizados

Pós-graduação em Ciência dos Materiais - FEIS

Organic-inorganic poly(methyl methacrylate) hybrids with confined polyhedral oligosilsesquioxane macromonomers

We herein report the synthesis of organic-inorganic hybrid poly(methyl methacrylate) containing 1 polyhedral oligosilsesquioxanes. Octakis(3-hydroxypropyldimethylsiloxy)octasilsesquioxane (OHPS) was synthesized from octakis(hydridodimethylsiloxy)octasilsesquioxane [Si8O12(OSiMe2H)(8), Q(8)M(8)(H)] following literature procedures. Octakis(tnethacryloxypropyldimethylsiloxy) octasilsesquioxane (OMPS) was synthesized via the reaction of methacryloyl chloride or methacrylic acid anhydride with OHPS, with the latter giving improved purity. Polymerization of OMPS with methyl inethacrylate using a dibenzoylperoxide initiator gave a highly cross-linked polymer. Characterization of the polymer was performed using Fourier transform IR spectroscopy, Si-29 NMR, differential scanning calorimetry, thermogravimetric analysis, atomic force microscopy, and transmission electron microscopy with energy-dispersive X-ray analysis. The polymer was found to be largely homogeneous. Increasing the OMPS concentration in the polymer gave increased decomposition and glass transition temperatures.