Determination of trace mercury(II) in 0.1 M perchloric acid by differential pulse stripping voltammetry at a rotating gold disc electrode

Andrews, Richard W.; Larochelle, John H.; Johnson, Dennis C.

doi:10.1021/ac60365a025

Cited by 52 publications

(15 citation statements)

References 21 publications

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“…The Hg UPD process is particularly important because of the technical significance of Hg amalgams and Hg surfaces in electrochemical and other processes. Underpotential deposition of Hg has been studied extensively with standard electrochemical techniques [9][10][11][12][13][14][15], but fundamental insight has been elusive because of the lack of microscopic surface structural information. In addition, the sensitivity of this process to different electrolytes is unknown.…”

Section: Department Of Chemistry University Of Illinois 505 S Mathmentioning

confidence: 99%

In situobservation of monolayer structures of underpotentially deposited Hg on Au(111) with the atomic force microscope

Chen

Gewirth

1992

Phys. Rev. Lett.

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The structures of monolayers of Hg atoms underpotentially deposited on Au(l 11) were resolved with the atomic force microscope. In sulfate, nitrate, and perchlorate electrolytes, a hexagonal overlayer with a 0.58 ±0.02-nm spacing was seen. In acetate, a hexagonal lattice exhibiting a 0.74±0.05-nm spacing was observed positive of the underpotential-deposition potential, a rhombic lattice with a 0.43 ± 0.02-nm spacing was seen at intermediate potentials, and another hexagonal lattice with a 0.30±0.03-nm spacing was found just positive of bulk deposition. PACS numbers: 68.55.-a, 82.45.+Z Development of a detailed understanding of the structure of the electrified solid-liquid interface is a central step in understanding electrochemical reactivity. A fundamental example of this reactivity is the deposition of a monolayer of one metal onto another. This phenomenon, known as underpotential deposition (UPD) [1], occurs when metal ions are electrodeposited onto a (different) metal surface at potentials positive from the reversible (Nernst) potential. In this process, only a monolayer or submonolayer of the metal forms on the electrode surface. The structure of these monolayers has attracted considerable attention because of their importance in electrodeposition and electrocatalytic [2] processes. In UHV environments, monolayers of foreign metal adatoms evaporated onto (ill) surfaces exhibit closepacked incommensurate structures [3,4]. These closepacked structures arise from net attractive forces between the adatoms. The demonstration that UPD monolayers of Cu [5,6] and Ag [7] form open adlattice structures in the electrochemical environment has been taken to imply that the force between adatoms has become repulsive, possibly deriving from coadsorption of electrolyte with the metal. Alternatively, other effects could also serve to open the adlattice. In particular, retention of a partial charge on the adatom, complex formation with the electrolyte, or deposition of a non-fcc element onto a (111) surface of an fee material could all lead to open lattices.In this Letter, we report an atomic force microscope ( AFM) [8] structural study of UPD of Hg onto Au(l 11) surfaces in four different electrolytes. The Hg UPD process is particularly important because of the technical significance of Hg amalgams and Hg surfaces in electrochemical and other processes. Underpotential deposition of Hg has been studied extensively with standard electrochemical techniques [9-15], but fundamental insight has been elusive because of the lack of microscopic surface structural information. In addition, the sensitivity of this process to different electrolytes is unknown. This latter point is important because UPD lattices of Cu [5,6] andAg [7] on Au(lll) surfaces exhibit strong electrolyte sensitivity. AFM images were obtained with a Nanoscope II AFM [16] operating in constant force mode. The force, optimized for each image, was nominally 1 x 10"^ N. A cell made from glass held the electrolyte. Au(l 11) electrodes were prepared by evaporation onto ...

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Section: Department Of Chemistry University Of Illinois 505 S Mathmentioning

confidence: 99%

In situobservation of monolayer structures of underpotentially deposited Hg on Au(111) with the atomic force microscope

Chen

Gewirth

1992

Phys. Rev. Lett.

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“…Gold was found to be superior to platinum as a working electrode. Andrews et al (107) used ASPV with a rotating gold disc electrode to determine the trace amounts of mercury (II) in 0.1M perchloric acid. Anderson and Tallmann (108) used a graphite epoxy TFME as working electrode.…”

Section: Stripping Methodsmentioning

confidence: 99%

Pulse polarography - theory and application.

Osteryoung

Hasebe

1976

Review of Polarography

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“…Compared to AAS, the main advantage of the electrochemical technique is the lower cost of the studies carried out; aside from that, there is its versatility, where several electrodes can be chosen to work with sequentially. Expectedly, this is considered an added bonus, because the electrodes chosen may have their surfaces modified, as is the case for gold (Au) [3 -5], glassy carbon (GCE), [3,6], graphite powder mixed with wax [7] and carbon paste electrodes (CPE) [8 -9]: the latter have been instrumental in attaining significant increments of their analytic response in terms of sensitivity and selectivity.…”

Section: Introductionmentioning

confidence: 99%

“…To improve the determination of Hg(II) with ASV, the GCE and CPE have been modified with poly(4-vinylpyridine) [3] and tetraphenyl borate [9] for salts such as HgCl 2 , or with a chelating resin Sumichelate Q10R [10], where deposition takes place during 2 to 30 minutes to determine concentrations of the order of pM.…”

Section: Introductionmentioning

confidence: 99%

Electrochemical Characterization and Determination of Mercury Using Carbon Paste Electrodes Modified with Cyclodextrins

et al. 2005

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In this work the characterization and determination of mercury in HClO 4 media using carbon paste electrodes modified with a-and b-cyclodextrins (CPE a-CD and CPE b-CD ) at E d ¼À 0.7 V with a t d ¼ 20 s and a potential scan v ¼ 20 mV s À1 is studied.. The statistical results obtained indicate that the modified electrodes displayed a better analytical performance as compared to that obtained with the unmodified CPE. The detection limits for the CPE a-CD and for the CPE b-CD were 0.05 and 0.09 mM, respectively, while for the CPE it was 0.41 mM. The CPE b-CD exhibited greater sensitivity as compared to that of the CPE a-CD .

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Determination of trace mercury(II) in 0.1 M perchloric acid by differential pulse stripping voltammetry at a rotating gold disc electrode

Cited by 52 publications

References 21 publications

In situobservation of monolayer structures of underpotentially deposited Hg on Au(111) with the atomic force microscope

In situobservation of monolayer structures of underpotentially deposited Hg on Au(111) with the atomic force microscope

Pulse polarography - theory and application.

Electrochemical Characterization and Determination of Mercury Using Carbon Paste Electrodes Modified with Cyclodextrins

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