Synthesis and preliminary characterization of octakis (chloropropyldimethylsiloxy) octasilsesquioxane

Carmo, Devaney Ribeiro do; Filho, Newton Luiz Dias; Stradiotto, Nelson Ramos

doi:10.1590/s1516-14392004000300020

Cited by 16 publications

(11 citation statements)

References 15 publications

(12 reference statements)

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“…The thermogram of SS ( Figure 5(a)) showed three mass loss phases. In the first step at 100 ∘ C (1%) attributed to physically adsorbed water loss, confirmed by the endothermic event in the DTA curve; the other two mass loss stages were observed at 220 ∘ C (15%) and 320 ∘ C (33%) attributed to the oxidation of organic matter [50] and the decomposition of residual groups SiO 2 [16,51,52] in the sample, also confirmed by the exothermic events in the DTA curve in the corresponding temperatures. It should be noted that as SS has chlorine in its composition, it was subjected to the programmed temperature increase up to the maximum temperature of 700 ∘ C, because at high temperatures the chlorine gas released can react with the platinum crucible used in the measurements.…”

Section: Thermogravimetric Analysis (Tga)mentioning

confidence: 53%

“…The thermogram of SA ( Figure 5(c)) showed two mass loss stages, the first at 100 ∘ C (5%) attributed to the physically adsorbed water loss and confirmed by the endothermic event in the DTA curve at the corresponding temperature. It was observed that the anhydrous compound is stable up to temperatures close to 200 ∘ C. At temperatures above 200 ∘ C the second mass loss stage was observed (65%), attributed to oxidation of the organic matter in the sample and confirmed by the exothermic event in the DTA curve [50]; it was also observed that at temperatures above 800 ∘ C no further mass loss (total mass loss of 70%) can be attributed to the formation of SiO 2 formed by the oxidation of SA [16,51,52].…”

Section: Thermogravimetric Analysis (Tga)mentioning

confidence: 64%

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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

Carmo

Silvestrini

Barud

et al. 2014

Journal of Nanomaterials

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The octakis(3-chloropropyl)silsesquioxane (SS) was organofunctionalized with 4-amino-5-4(pyridyl)-4H-1,2,4-triazole-3-thiol. The product formed (SA) was undergo another reactions in two steps, first with copper and so hexacyanoferrate (III) to form CuHSA. The organofunctionalized silsesquioxane was characterized by the following techniques: scanning electron microscopy (SEM), Fourier transform infrared (FTIR), nuclear magnetic resonance (NMR) in solid state, and thermogravimetric analysis in air and nitrogen atmosphere. The composite CuHSA was incorporated into a graphite paste electrode and the electrochemical behavior studies were conducted with cyclic voltammetry. The cyclic voltammogram of the modified graphite paste electrode with CuHSA showed one redox couple with formal potentialEθ′=0.75 V versus Ag/AgCl(sat)(KCl 1.0 mol L−1;v= 20 mV s−1) attributed to the redox process Fe(II)(CN)6/Fe(III)(CN)6of the binuclear complex formed. The redox couple presents an electrocatalytic response of sulfhydryl compounds such as n-acetylcysteine and l-cysteine. For determination of n-acetylcysteine and l-cysteine the modified graphite paste electrode showed a linear region in the concentration range of 2 to 20 mmol L−1. The modified electrode was chemically and electrochemically stable and showed good reproducibility.

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Section: Thermogravimetric Analysis (Tga)mentioning

confidence: 53%

Section: Thermogravimetric Analysis (Tga)mentioning

confidence: 64%

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

Carmo

Silvestrini

Barud

et al. 2014

Journal of Nanomaterials

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“…The CAC and ACCoN scanning electron microscopy analyses at a 20.000X increases are presented in Figure 4(A) and (B). Concerning CAC (Figure 4(A)), microparticles presenting mostly cubic structural shapes and average size of 252 nm were observed, characteristic of octameric cubic silsesquioxanes [64]. Regarding ACCoN (Figure 4(B)), a cluster of cubic and cylindrical particles with an average size of approximately 670 nm was detected.…”

Section: Resultsmentioning

confidence: 97%

Isoniazid‐sensing Behavior of a Hybrid Silsesquioxane and Cobalt Pentacyanonitrosylferrate‐based Nanocomposite

Magossi

Filho

et al. 2021

Electroanalysis

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A novel silsesquioxane and cobalt nitroprusside compound was prepared from octa(aminopropyl)silsesquioxane, resulting in a nanocomposite (ACCoN), which was then characterized by different spectroscopic techniques. The cyclic voltammograms of the ACCoN‐modified graphite paste electrode indicated a redox pair with a formal potential (Eθ′)=0.38 V, assigned to the Co(II)Fe(II)(CN)5NO/Co(II)Fe(III)(CN)5NO redox couple. The ACCoN‐modified graphite paste electrode was sensitive to isoniazid concentrations, presenting a linear response at a concentration range from 6.0×10−7 to 1.0×10−5 mol L−1, with limit of detection and amperometric sensitivity of 5.53×10−7 mol L−1 and 0.17 A/mol L−1, respectively.

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“…8a) showed two mass loss phases. The first stage was from 350 to 450 • C (68%) and the second was from 450 to 650 • C (7%) attributed to the oxidation of organic matter [48,49] and the decomposition of residual groups SiCH 2 [50][51][52] in the sample. The residue was 25% and based mainly on silica.…”

Section: Thermogravimetric Analysis Tg -Dtamentioning

confidence: 99%

Reactivity of a Silsesquioxane Organofunctionalized with 4-Amino-5-Phenyl-4H-[1,2,4]-Triazole-3-thiol: Complementary Characterization and an Application to Chronoamperometric Detection of L-Dopamine

Fernandes

Maraldi

Filho

et al. 2018

Silicon

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This work describes the organofunctionalization and a complementary characterization and application of an octakis(3-chloropropyl)octasilsesquioxane (1) with 4-Amino-5-Phenyl-4H-[1,2,4]-Triazole-3-Thiol (2). The functionalized silsesquioxane (3) was characterized by nuclear magnetic resonance, X-ray diffraction, transmission electron microscopy and thermogravimetric analysis. After functionalized, the silsesquioxane can interact with copper chloride and subsequently with potassium hexacyanoferrate (III) (4). The hybrid composite formed (4) was characterized by FT-IR and diffuse reflectance. The compound 4 included into a work graphite paste electrode (20% w/w) was examined for chronoamperometric determination of L-Dopamine. The modified graphite paste electrode with compound 4 showed a linear response from 2.5×10 −5 at 4.0×10 −4 mol L −1 . The modified graphite paste electrode with 4 showed a detection limit of 2.08× 10 −4 mol L −1 with a relative standard deviation of ±2% (n = 3) and amperometric sensitivity of 0.136 A mol L −1 .

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Synthesis and preliminary characterization of octakis (chloropropyldimethylsiloxy) octasilsesquioxane

Cited by 16 publications

References 15 publications

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

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

Isoniazid‐sensing Behavior of a Hybrid Silsesquioxane and Cobalt Pentacyanonitrosylferrate‐based Nanocomposite

Reactivity of a Silsesquioxane Organofunctionalized with 4-Amino-5-Phenyl-4H-[1,2,4]-Triazole-3-thiol: Complementary Characterization and an Application to Chronoamperometric Detection of L-Dopamine

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