Effects of Oxygen Reduction on Nickel Deposition from Unbuffered Aqueous Solutions: II . Characterization of the Electrode Interface in Electrodeposition

1995 ◽  
Vol 142 (4) ◽  
pp. 1132-1138 ◽  
Author(s):  
C. Q. Cui ◽  
Jim Y. Lee ◽  
J. Lin ◽  
K. L. Tana
Keyword(s):  
Aqueous Solutions ◽  
Oxygen Reduction ◽  
Nickel Deposition ◽  
Electrode Interface

A Pyridinic Fe-N4 Macrocycle Effectively Models the Active Sites in Fe/N-Doped Carbon Electrocatalysts

2020 ◽  
Author(s):  
Travis Marshall-Roth ◽  
Nicole J. Libretto ◽  
Alexandra T. Wrobel ◽  
Kevin Anderton ◽  
Nathan D. Ricke ◽  
...  
Keyword(s):  
Oxygen Reduction ◽  
Active Sites ◽  
Catalytic Properties ◽  
Reduction Reaction ◽  
Iron Phthalocyanine ◽  
Electrochemical Studies ◽  
Onset Potential ◽  
Nitrogen Doped Carbon ◽  
Iron Active Sites

Iron- and nitrogen-doped carbon (Fe-N-C) materials are leading candidates to replace platinum in fuel cells, but their active site structures are poorly understood. A leading postulate is that iron active sites in this class of materials exist in an Fe-N<sub>4</sub> pyridinic ligation environment. Yet, molecular Fe-based catalysts for the oxygen reduction reaction (ORR) generally feature pyrrolic coordination and pyridinic Fe-N<sub>4</sub> catalysts are, to the best of our knowledge, non-existent. We report the synthesis and characterization of a molecular pyridinic hexaazacyclophane macrocycle, (phen<sub>2</sub>N<sub>2</sub>)Fe, and compare its spectroscopic, electrochemical, and catalytic properties for oxygen reduction to a prototypical Fe-N-C material, as well as iron phthalocyanine, (Pc)Fe, and iron octaethylporphyrin, (OEP)Fe, prototypical pyrrolic iron macrocycles. N 1s XPS signatures for coordinated N atoms in (phen<sub>2</sub>N<sub>2</sub>)Fe are positively shifted relative to (Pc)Fe and (OEP)Fe, and overlay with those of Fe-N-C. Likewise, spectroscopic XAS signatures of (phen<sub>2</sub>N<sub>2</sub>)Fe are distinct from those of both (Pc)Fe and (OEP)Fe, and are remarkably similar to those of Fe-N-C with compressed Fe–N bond lengths of 1.97 Å in (phen<sub>2</sub>N<sub>2</sub>)Fe that are close to the average 1.94 Å length in Fe-N-C. Electrochemical studies establish that both (Pc)Fe and (phen<sub>2</sub>N<sub>2</sub>)Fe have relatively high Fe(III/II) potentials at ~0.6 V, ~300 mV positive of (OEP)Fe. The ORR onset potential is found to directly correlate with the Fe(III/II) potential leading to a ~300 mV positive shift in the onset of ORR for (Pc)Fe and (phen<sub>2</sub>N<sub>2</sub>)Fe relative to (OEP)Fe. Consequently, the ORR onset for (phen<sub>2</sub>N<sub>2</sub>)Fe and (Pc)Fe is within 150 mV of Fe-N-C. Unlike (OEP)Fe and (Pc)Fe, (phen<sub>2</sub>N<sub>2</sub>)Fe displays excellent selectivity for 4-electron ORR with <4% maximum H<sub>2</sub>O<sub>2</sub> production, comparable to Fe-N-C materials. The aggregate spectroscopic and electrochemical data establish (phen<sub>2</sub>N<sub>2</sub>)Fe as a pyridinic iron macrocycle that effectively models Fe-N-C active sites, thereby providing a rich molecular platform for understanding this important class of catalytic materials.<p><b></b></p>

scholarly journals Preparation and Characterization of the Sulfur-Impregnated Natural Zeolite Clinoptilolite for Hg(II) Removal from Aqueous Solutions

Processes ◽  
2021 ◽  
Vol 9 (2) ◽  
pp. 217
Author(s):  
Marin Ugrina ◽  
Martin Gaberšek ◽  
Aleksandra Daković ◽  
Ivona Nuić
Keyword(s):  
Chemical Modification ◽  
Aqueous Solutions ◽  
Specific Surface ◽  
Surface Area ◽  
Natural Zeolite ◽  
Contact Time ◽  
Liquid Ratio ◽  
X Ray ◽  
Solid Liquid

Sulfur-impregnated zeolite has been obtained from the natural zeolite clinoptilolite by chemical modification with Na2S at 150 °C. The purpose of zeolite impregnation was to enhance the sorption of Hg(II) from aqueous solutions. Chemical analysis, acid and basic properties determined by Bohem’s method, chemical behavior at different pHo values, zeta potential, cation-exchange capacity (CEC), specific surface area, X-ray powder diffraction (XRPD), scanning electron microscopy with energy-dispersive X-ray analysis (SEM-EDS), Fourier transform infrared spectroscopy (FTIR), as well as thermogravimetry with derivative thermogravimetry (TG-DTG) were used for detailed comparative mineralogical and physico-chemical characterization of natural and sulfur-impregnated zeolites. Results revealed that the surface of the natural zeolite was successfully impregnated with sulfur species in the form of FeS and CaS. Chemical modification caused an increase in basicity and the net negative surface charge due to an increase in oxygen-containing functional groups as well as a decrease in specific surface area and crystallinity due to the formation of sulfur-containing clusters at the zeolite surface. The sorption of Hg(II) species onto the sulfur-impregnated zeolite was affected by the pH, solid/liquid ratio, initial Hg(II) concentration, and contact time. The optimal sorption conditions were determined as pH 2, a solid/liquid ratio of 10 g/L, and a contact time of 800 min. The maximum obtained sorption capacity of the sulfur-impregnated zeolite toward Hg(II) was 1.02 mmol/g. The sorption mechanism of Hg(II) onto the sulfur-impregnated zeolite involves electrostatic attraction, ion exchange, and surface complexation, accompanied by co-precipitation of Hg(II) in the form of HgS. It was found that sulfur-impregnation enhanced the sorption of Hg(II) by 3.6 times compared to the natural zeolite. The leaching test indicated the retention of Hg(II) in the zeolite structure over a wide pH range, making this sulfur-impregnated sorbent a promising material for the remediation of a mercury-polluted environment.

Synthesis and Characterization of Chitosan/Fluorapatite Composites for the Removal of Cr (VI) from Aqueous Solutions and Optimized Parameters

2020 ◽  
Vol 231 (4) ◽  
Author(s):  
Rachid El Kaim Billah ◽  
Youness Abdellaoui ◽  
Zakaria Anfar ◽  
Germán Giácoman-Vallejos ◽  
Mahfoud Agunaou ◽  
...  
Keyword(s):  
Aqueous Solutions ◽  
Synthesis And Characterization

Preparation and Characterization of Carbon Supported Nano-Nickel and its Sorption Behavior for Zinc from Aqueous Solutions

2012 ◽  
Vol 510-511 ◽  
pp. 271-276 ◽  
Author(s):  
Tayyaba Asim ◽  
R. Ahmed ◽  
M.S. Ansari
Keyword(s):  
Morphological Study ◽  
Aqueous System ◽  
Effect Of Temperature ◽  
Vacuum Drying ◽  
Sorption Behavior ◽  
Nickel Deposition ◽  
Adsorption Data ◽  
Nano Nickel ◽  
The Mean

Nickel deposited on carbon has been used as adsorbent to recover Zn (II) from aqueous system. The adsorbent was synthesized by depositing nickel nitrate on carbon under inert conditions and decomposing it to nickel by raising the temperature, washing and vacuum drying. Various techniques including XRD, FTIR, and SEM were employed for its characterization. FTIR showed that the nickel deposition enhanced the carbon functionalization due to presence of OH, C=O and C-O groups.Average crystallite size ofabout 9 nm was determined from XRD. Nickel deposition resulted in further division particles as indicated from the morphological study. Zn (II) was subjected to adsorptionon the synthesized adsorbent. It was observed that the rate of adsorption increased significantly on the nickel deposited carbon than the carbon alone. Morris-Weber, Lagergren and Reichenberg models were applied to find out the type and rate of adsorption employingfirst and second order rate equations.The adsorption data were applied toLangmuir, Freundlich and D-R isotherms and values of isotherm constants were calculated and were higher for Ni/C than carbon alone. The mean free energy of zinc sorption on carbon and Ni/C are 16.67 and 18.26 kJmol-1 which shows chemisorption. Thermodynamic studies were done to find out the effect of temperature on sorption. Positive values of ΔH and negative values of ΔG show endothermic and spontaneous type of sorption.

Characterization of Structural Changes of Poly(vinyl methyl ether) γ-Irradiated in Diluted Aqueous Solutions

Langmuir ◽  
2004 ◽  
Vol 20 (7) ◽  
pp. 2883-2889 ◽  
Author(s):  
Claudia Querner ◽  
Thomas Schmidt ◽  
Karl-Friedrich Arndt
Keyword(s):  
Aqueous Solutions ◽  
Methyl Ether ◽  
Structural Changes ◽  
Vinyl Methyl ◽  
Vinyl Methyl Ether
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