Electrocatalysis of Nitrate Reduction at Copper‐Nickel Alloy Electrodes in Acidic Media

Simpson, Brett K.; Johnson, Dennis C.

doi:10.1002/elan.200302790

Cited by 65 publications

(54 citation statements)

References 31 publications

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“…The proposed mechanism is supported by previous works reported in the literature [36,38] and is consistent with the results on the dependence of the electrocatalytic process with the solution pH (see further discussion). Figure 3 demonstrates the influence of the activation step towards nitrite sensing using a copper electrode.…”

Section: Electrochemical Reduction Of Nitritesupporting

confidence: 91%

“…The cathodic reduction of nitrate and nitrite at copper surfaces depends strongly on the specific adsorption of these species from the solution bulk and H-atoms produced by reduction of protons [36]. Therefore, the increase in the surface area of copper electrodes explains the increase in sensitivity of analytical methods for nitrate and nitrite after the electrode activation procedure.…”

Section: Electrochemical Reduction Of Nitritementioning

confidence: 99%

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Activated Copper Cathodes as Sensors for Nitrite Analysis

et al. 2010

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The increased surface area of copper electrodes upon applying a suitable potential protocol was characterized by atomic force microscopy images. Scanning electrochemical microscopy was used to demonstrate the enhanced reactivity of the generated surface. The modified electrode showed excellent catalytic activity towards nitrite reduction in acidic medium (pH 2). This new platform was used in the development of a fast and simple voltammetric method for nitrite determination. Commercial and rainwater spiked samples were analyzed and the data showed an excellent agreement with those obtained with a reference spectrophotometric method (Griess reaction) at a confidence level of 95 % (Students t-test).

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Section: Electrochemical Reduction Of Nitritesupporting

confidence: 91%

Section: Electrochemical Reduction Of Nitritementioning

confidence: 99%

Activated Copper Cathodes as Sensors for Nitrite Analysis

et al. 2010

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“…After screening several cathode materials, various investigators have converged to identify copper [7][8][9][10][11][12][13] or its alloys, especially Cu-Ni [14,15], as the most suitable ones. To cope with the intrinsic tendency of Cu to become deactivated upon nitrate reduction, in most cases, Cu layers were formed in situ, just before the analyses, by reducing Cu ions deliberately added to the analytical samples.…”

Section: Introductionmentioning

confidence: 99%

Study of Cu, Cu-Ni and Rh-modified Cu porous layers as electrode materials for the electroanalysis of nitrate and nitrite ions

Comisso¹,

Cattarin²,

Guerriero³

et al. 2015

J Solid State Electrochem

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Three porous materials (Cu, a Cu-Ni alloy with 70 at.% Cu and Rh-modified Cu) have been tested as electrodes for the electroanalysis of nitrate and nitrite ions, in either neutral or basic media, using mainly a flow injection technique. Porous Cu and Cu-Ni were prepared by electrodeposition at high current density, exploiting the transient template action of hydrogen bubbles. Rh-modified Cu electrodes were obtained from porous Cu, through a galvanic displacement reaction. All materials had a linear response for both nitrates and nitrites, at concentrations up to 10 −3 M, at least. Sensitivities, detection limits and stability were determined. Compared with Cu, used as a benchmark, (i) Rh-modified Cu had higher sensitivity for nitrates, comparable sensitivity for nitrites, lower or comparable detection limits and overall better stability; (ii) Cu-Ni had lower sensitivity, but exhibited lower detection limits and more stable performance for most analyte/medium combinations.

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“…This open pore structure is attributable to the presence of pyramidal crystals and the possible adsorption of hydrogen bubbles on the electrode surface, which can explain the formation of the voids seen in Figure 3B. The evolution of hydrogen depends on the solution pH and this has been reported in the literature 11,12 to occur at negative potentials due to the interaction of H-atoms adsorbed in specific sites and diffusing protons, according to the following equation:…”

Section: Resultsmentioning

confidence: 67%

Morphology, microstructure and electrocatalytic properties of activated copper surfaces

Gamboa

Petri

Benedetti

et al. 2012

J. Braz. Chem. Soc.

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Alterações morfológicas em superfícies de cobre resultantes da aplicação de um protocolo definido de potencial foram examinadas por microscopia eletrônica de varredura (MEV) e microscopia de força atômica (AFM). Os resultados mostraram uma boa correlação entre o tempo empregado na ativação do eletrodo, microestrutura resultante e a atividade eletroquímica.Morphologic changes on copper surfaces upon applying an established potential protocol were examined by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The results showed a good correlation between the time employed in the electrode activation and the resulting microstructure and electrochemical activity.Keywords: nitrite, copper electrode, activation process, SEM, AFM IntroductionThe deliberate manipulation of electrodic surfaces consists of an area of continuing interest, because this approach leads to an improvement in the ability to recognize molecules and carry out electron transfer processes at higher rates. Hence, one of the dominant subjects in electrochemistry is the attempt to control the chemical composition and morphological structure of the electrode surface to gain advantages in electroanalytical determinations. It is well known that the electroactivity of copper surfaces depends strongly on their morphology, surface area and structure, which would in turn depend on the method employed to prepare the electrode prior to electrochemical measurements. Hence, several studies have been reported in the literature on the use of copper surfaces aiming for the quantification of different species such as glucose, 1 carbohydrates, 2 ethanol, 3 nitrate, 4, 5 nitrite, 5 and sufite. 6 The electrochemical determination of nitrate after deposition of copper from solutions containing Cu(II) has been reported by some authors, 7,8 who examined qualitatively the morphology of the copper deposit by scanning electron microscopy (SEM) and atomic force microscopy (AFM). The increased sensitivity for nitrate after the surface modification by deposition of the fresh copper layer was attributed to morphologic changes assessed through quantitative parameters such as roughness and porosity of the film. Our group reported a new procedure for the activation of copper surfaces using a potential protocol based on copper oxidation and subsequent reduction of generated copper ions. 9,10 Taking into account these findings and as an attempt to understand which surface parameters control the electrochemical activity, the present study aims to evaluate whether there is a quantitative correlation between the surface area of copper electrodes and their electrochemical properties. Accordingly, copper electrodes were activated for different periods of time to produce layers which were analyzed by SEM and AFM. Then, the electrochemical activity of each generated surface was evaluated towards the cathodic reduction of nitrite. To the best of our knowledge, this is the first time that such a quantitative approach is applied for copper electrodes. Experimental Chemicals a...

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Electrocatalysis of Nitrate Reduction at Copper‐Nickel Alloy Electrodes in Acidic Media

Cited by 65 publications

References 31 publications

Activated Copper Cathodes as Sensors for Nitrite Analysis

Activated Copper Cathodes as Sensors for Nitrite Analysis

Study of Cu, Cu-Ni and Rh-modified Cu porous layers as electrode materials for the electroanalysis of nitrate and nitrite ions

Morphology, microstructure and electrocatalytic properties of activated copper surfaces

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