Application of solid-state electrochemistry techniques to polyfunctional organic–inorganic hybrid materials: The Maya Blue problem

Doménech, Antonio; Doménech‐Carbó, María Teresa; Osete-Cortina, Laura; Montoya, Noemí

doi:10.1016/j.micromeso.2012.04.031

Cited by 25 publications

(16 citation statements)

References 59 publications

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“…The above data are consistent with a description of MB in terms of successive isomerization and redox tuning processes as schematized in Figure . Generically, this view is consistent with the description of isomerization of methyl red plus palygorskite hybrids reported by Giustetto et al, and the isomerization and redox tuning previously studied for lapachol attached to palygorskite, and are also consistent with the two-step kinetics observed from spectral data in the preparation of MB specimens . This model is also consistent with thermochemical data that can be estimated from electrochemical, Raman, and visible spectroscopic data.…”

Section: Resultssupporting

confidence: 91%

Isomerization and Redox Tuning: Reorganizing the Maya Blue Puzzle from Synthetic, Spectral, and Electrochemical Issues

Doménech‐Carbó

Costero²,

Gil³

et al. 2021

J. Phys. Chem. C

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A new approach to describe the composition of Maya blue (MB), an ancient organic− inorganic hybrid material, is presented. It is based on the analysis of attenuated total reflection-Fourier transform infrared (ATR-FTIR), Raman spectroscopy, UV−visible (vis) spectroscopic, and electrochemical data for indigo and dehydroindigo plus palygorskite hybrids, including a novel methodology using electrocatalytic effects on the oxygen reduction reaction. As a result, it is concluded that MB results from the tautomerization of indigo-to-indigo hemienol and the subsequent oxidation of these isomeric forms to dehydroindigo, all associated with the palygorskite clay framework, at temperatures above 100 °C. This model is also consistent with 13 C NMR data on indigo plus sepiolite hybrids. A consistent set of thermochemical parameters is obtained from ATR-FTIR, solid-state electrochemistry, and UV−vis diffuse reflectance spectra for the successive isomerization and redox tuning processes experienced by palygorskiteassociated indigo.

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Section: Resultssupporting

confidence: 91%

Isomerization and Redox Tuning: Reorganizing the Maya Blue Puzzle from Synthetic, Spectral, and Electrochemical Issues

Doménech‐Carbó

Costero²,

Gil³

et al. 2021

J. Phys. Chem. C

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“…In this context, application of VMP, further confirmed by application of a multi-technique methodology that included UV-Vis spectrophotometry, FTIR and Raman spectroscopy, MNR, SEM-EDX, TEM, AFM, GC-MS, Py-GC-MS, UTLC-MS, and HPLC-DAD, has provided experimental evidences of the existence of redox tuning in Maya blue-type materials and, in particular, of the presence not only of indigo but also of dehydroindigo attached to palygorskite [101][102][103][104][105][106]. The co-existence of different organic molecules attached to the palygorskite in variable concentration depending on the thermal treatment applied during the preparation of the pigment justify the different hue found in Maya wall paintings, which ranges from yellow to blue and green.…”

Section: Examination Of Paint Samplesmentioning

confidence: 99%

Another beauty of analytical chemistry: chemical analysis of inorganic pigments of art and archaeological objects

Doménech‐Carbó

Osete-Cortina

2016

ChemTexts

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“…Moreover, this approach allows the selective transformation of specific groups in a ligand or in a complex under very mild conditions. In the last several decades, contributions of electrochemical technique are of interest not only to inorganic [1][2][3][4][5][6][7] Direct anodic dissolution of nickel metal and cathodic reduction of carboxylic acids (RCOOH) in acetonitrile has proved to be a simple and efficient one-step route to synthesize unique polymeric nickel(II) carboxylate complexes, {Ni(OOCR)2}n in H-type glass Pyrex cell. When the oxidation was carried out in the presence of neutral ligands (L) such as 2,2'-bipyridyl or 1,10-phenanthroline, the complexes of type {Ni(OOCR)2.L}n were obtained.…”

Section: Introductionmentioning

confidence: 99%

Synthesis and Characterization of Unique Nickel(II) Carboxylates and Their Coordination Complexes

Shavina¹,

Singh²

2018

Asian J. Chem.

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INTRODUCTIONElectrochemical technique in inorganic synthesis is highly selective in terms of potential, current density, electrode material and electrolyte composition for controlling the reaction rate. Electro synthesis is not only the oldest but also the simplest method for the synthesis of coordination compounds starting from the zero-valent metal. Electrochemical methods employ simple machinery and pure starting materials. The fact that the metal is employed rather than one of its salts avoids the occurrence of competitive reactions between the anion salts and the ligand to coordinate to the metal ion. Moreover, this approach allows the selective transformation of specific groups in a ligand or in a complex under very mild conditions. In the last several decades, contributions of electrochemical technique are of interest not only to inorganic [1][2][3][4][5][6][7] Direct anodic dissolution of nickel metal and cathodic reduction of carboxylic acids (RCOOH) in acetonitrile has proved to be a simple and efficient one-step route to synthesize unique polymeric nickel(II) carboxylate complexes, {Ni(OOCR)2}n in H-type glass Pyrex cell. When the oxidation was carried out in the presence of neutral ligands (L) such as 2,2'-bipyridyl or 1,10-phenanthroline, the complexes of type {Ni(OOCR)2.L}n were obtained. Tetrabutylammonium chloride has been used as a supporting electrolyte in order to increase the electrolytic conductivity of the electrochemical system which in turn affects the current efficiency, cell voltage and energy consumption in the electrolytic cell. The complexes have been characterized by vibrational spectra, CHN elemental analysis, solubility and melting points shows a good agreement with the structure. The result also shows that the direct electrochemical synthetic technique has high current efficiency, extra purity and yield.

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Application of solid-state electrochemistry techniques to polyfunctional organic–inorganic hybrid materials: The Maya Blue problem

Cited by 25 publications

References 59 publications

Isomerization and Redox Tuning: Reorganizing the Maya Blue Puzzle from Synthetic, Spectral, and Electrochemical Issues

Isomerization and Redox Tuning: Reorganizing the Maya Blue Puzzle from Synthetic, Spectral, and Electrochemical Issues

Another beauty of analytical chemistry: chemical analysis of inorganic pigments of art and archaeological objects

Synthesis and Characterization of Unique Nickel(II) Carboxylates and Their Coordination Complexes

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