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Ladder diagrams are useful for evaluating equilibria involving metal-ligand complexes. The vertical scale of the ladder diagram represents the concentration of unreacted or free ligand, pL. The horizontal lines on the scale depict the log of stepwise formation constants for metal-ligand complexes and indicate the dominant species in all the regions.
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EDTA titrations are usually carried out in highly basic conditions, where the fully deprotonated form of EDTA, Y4−, actively complexes with the free metal ions in the solution. Several metal ions precipitate as hydrous oxide (hydroxides, oxides, or oxyhydroxides) under these conditions, lowering the concentration of free metal ions in the solution. For this reason, auxiliary complexing agents or ligands such as ammonia, tartrate, citrate, or triethanolamine are used in EDTA titrations to...
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Electrodeposition is a technique used to separate an analyte from interferents by electrochemical processes. Here, the analyte is a metal ion that can be deposited on an electrode immersed in the sample solution. The electrochemical setup consists of an anode and a cathode. When an electric current is applied to the setup, oxidation occurs at the anode. At the cathode, which consists of a large metal surface, metal ions undergo reduction and deposit onto the surface.
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Electrocatalytic Ammonia Oxidation by a Low-Coordinate Copper Complex.

Md Estak Ahmed1,2, Mahdi Raghibi Boroujeni2, Pokhraj Ghosh1,2

  • 1Department of Chemistry, Michigan State University, East Lansing, Michigan 48824, United States.

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|November 9, 2022
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A novel copper catalyst efficiently oxidizes ammonia to dinitrogen, a key step for using ammonia as a sustainable fuel and hydrogen source. This robust electrocatalyst demonstrates stability and a viable mechanism for N-N bond formation.

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Area of Science:

  • Electrochemistry
  • Catalysis
  • Inorganic Chemistry

Background:

  • Ammonia oxidation to dinitrogen is crucial for utilizing ammonia as a fuel and hydrogen source.
  • This process requires breaking strong N-H bonds and forming N-N bonds, presenting significant catalytic challenges.

Purpose of the Study:

  • To report a novel β-diketiminato copper complex as a robust electrocatalyst for ammonia oxidation.
  • To investigate the mechanism of ammonia oxidation mediated by the copper catalyst.

Main Methods:

  • Electrochemical characterization including cyclic voltammetry (CV) and controlled potential electrolysis (CPE).
  • Synthesis and characterization of a novel β-diketiminato copper complex.
  • Density Functional Theory (DFT) analysis to elucidate reaction pathways and thermodynamic barriers.

Main Results:

  • The synthesized copper complex ([Pr2NNF6]CuI-NH3) efficiently catalyzes ammonia oxidation at a moderate overpotential (700 mV) with a high turnover frequency (TOFmax = 940 h-1).
  • The catalyst demonstrated excellent stability during prolonged electrolysis (>5 h).
  • Mechanistic studies revealed the formation of a reactive copper(II)-amide intermediate, crucial for N-N bond formation, and identified electrocatalytically inactive species at high ammonia concentrations.

Conclusions:

  • The reported copper complex is a robust and efficient electrocatalyst for ammonia oxidation to dinitrogen.
  • Understanding the mechanistic pathway, including the role of copper-amide intermediates and the deactivation pathway at high ammonia concentrations, is key for catalyst design.
  • This work provides a promising avenue for the development of catalysts for ammonia-based energy applications.