In situ electrochemical impedance spectroscopy/synchrotron radiation grazing incidence X-ray diffraction—A powerful new technique for the characterization of electrochemical surfaces and interfaces

Jiang, Zhong Tao; Martizano, Jay; Lowe, A. D.; Pejcic, Bobby; Riessen, Arie van

doi:10.1016/j.electacta.2006.03.030

Cited by 20 publications

(16 citation statements)

References 31 publications

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“…Notwithstanding, a citric acid calibration buffer was able to yield the expected value of approximately 10 À19 M aFe 3þ [15] in UV photooxidized or organic-free seawater, as expected for the inorganic speciation of iron-(III) in seawater [2]. The thesis herein is that an appropriate blend of ligands possessing a range of functionalities that are representative of natural organic ligands in seawater may be able to simulate the effects of seawater ligands on the response of the iron(III) ISE, and a previous EIS/SR-GIXRD study of the surface chemistry of the iron(III) ISE in raw seawater as well as calibration ligands [18] has guided our choice regarding a blend ligands for use in this study.…”

Section: Resultsmentioning

confidence: 99%

“…The EIS/SR-GIXRD data [18] revealed a destruction of the surface layer of the ISE in organic-free or artificial seawater due to a complete removal of all surface crystalline phases, while raw seawater comprising natural organic ligands and a seawater ligand mimetic system containing EN, SA, EDTA along with millimolar and submillimolar amounts of iron and copper is capable of protecting the iron(III) ISEs surface against this destructive dissolution process. Consequently, it is likely that the seawater ligand interference effect is due to a mismatching between the level of protection offered by natural seawater ligands against the dissolution of surface crystalline phases on the iron(III) ISE, as compared to that offered by the ligands in an ISE calibration buffer medium, and this EN-SA-EDTA-Cu-Fe calibration ligand provides a possibility for simulating the effects of natural seawater ligands on the surface chemistry of the iron(III) ISE.…”

Section: Introductionmentioning

confidence: 98%

“…Recently, De Marco and co-workers [17,18] have developed a novel synchrotron radiation-grazing incidence X-ray diffraction (SR-GIXRD)/potentiometry/electrochemical impedance spectroscopy (EIS) capability to monitor in-situ the surface chemistry of the iron(III) ISE in artificial and real seawater showing that the surface crystalline phases of this sensor (i.e., metal selenides) are attacked aggressively by chloride and hydroxide in organicfree or artificial seawater, but this deleterious process is suppressed significantly by the natural organic ligands in seawater. The EIS/SR-GIXRD data [18] revealed a destruction of the surface layer of the ISE in organic-free or artificial seawater due to a complete removal of all surface crystalline phases, while raw seawater comprising natural organic ligands and a seawater ligand mimetic system containing EN, SA, EDTA along with millimolar and submillimolar amounts of iron and copper is capable of protecting the iron(III) ISEs surface against this destructive dissolution process.…”

Section: Introductionmentioning

confidence: 98%

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Response of the Iron Chalcogenide Glass Membrane Ion‐Selective Electrode in a Seawater Ligand Mimetic Calibration Buffer

Martizano

2007

Electroanalysis

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As a continuation of recent mechanistic studies into the influence of seawater ligands on the surface chemistry of the iron chalcogenide glass membrane ion-selective electrode (ISE), the present study has investigated the response of the iron(III) ISE in a seawater ligand mimetic system to examine its suitability as a calibration medium for the electroanalysis of raw or natural seawater. Significantly, dip method calibrations of the ISE in a mixture of salicylate, ethylene diamine tetraacetic acid (EDTA), ethylene diamine and minor amounts of dissolved iron(III) and copper(II) yielded the expected Nernstian response of 30 mV/decade according to the known ion-exchange/electron transfer response mechanism of this ISE. Furthermore, ideal Nernstian response of the electrode is also obtained in a continuous flow analysis (CFA) mode, noting that this provides scope for using a hydrodynamic flow regime to minimize the electrode release of iron and the concomitant detection limit of the ISE. Ultimately, repetitive CFA analyses of free iron(III) in raw or natural seawater yielded a free iron(III) level commensurate with the expected inorganic and organic speciation of iron(III) in seawater.

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Section: Resultsmentioning

confidence: 99%

Section: Introductionmentioning

confidence: 98%

Section: Introductionmentioning

confidence: 98%

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Response of the Iron Chalcogenide Glass Membrane Ion‐Selective Electrode in a Seawater Ligand Mimetic Calibration Buffer

Martizano

2007

Electroanalysis

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“…The EIS/SR-GIXRD data [110] illustrated that a destruction of the MSL in artificial seawater is due to a complete removal of all surface crystalline phases, and that raw seawater comprising natural organic ligands together with a mimetic seawater ligand system containing ethylenediamine, salicylic acid and EDTA is capable of protecting the MSL of the iron(III) ISE against this oxidative dissolution process. Unpublished data has shown that this mimetic seawater ligand calibration buffer provides meaningful aFe 3þ data in seawater, and this paper will be published soon.…”

Section: Iron(iii) In Seawatermentioning

confidence: 98%

“…In recent research, De Marco and co-workers [110,111] have developed a novel synchrotron radiation-grazing incidence X-ray diffraction (SR-GIXRD)/potentiometry/ EIS capability to monitor in-situ the so-called modified surface layer (MSL) of the iron(III) chalcogenide glass ISE in artificial and real seawater, and it was shown that the surface crystalline phases of this sensor (i.e., metal selenides) are attacked by chloride and hydroxide in artificial seawater, but are protected by the natural organic ligands in seawater. The EIS/SR-GIXRD data [110] illustrated that a destruction of the MSL in artificial seawater is due to a complete removal of all surface crystalline phases, and that raw seawater comprising natural organic ligands together with a mimetic seawater ligand system containing ethylenediamine, salicylic acid and EDTA is capable of protecting the MSL of the iron(III) ISE against this oxidative dissolution process.…”

Section: Iron(iii) In Seawatermentioning

confidence: 98%

Ion‐Selective Electrode Potentiometry in Environmental Analysis

2007

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This review will illustrate how it is possible to develop ion-selective electrode (ISE) methodologies that meet the stringent requirements (i.e., high selectivities and very low detection limits) for the analysis of important analytes in the environment, and will present a variety of examples on the application of ISEs in environmental analysis. Despite the experimental biases that have limited the analytical performance of ISEs through apparently high detection limits and modest selectivities, there has been a plethora of research in the application of ISEs in the monitoring of environmentally important trace metals and anions in natural waters and soils. Most popular has been the analysis of free metals in natural waters, as this parameter is known to be a master variable in the uptake and toxicology of trace metals on aquatic biota reflecting the bioavailability of trace metals in the environment. Furthermore, as copper is a major trace metal in coastal waters due to its extensive use in antifouling paints on sea vessels and structures, there are many reports in the literature on the use of the copper ISE in assays of either free copper or the copper complexing capacity of natural waters and soil peats. Moreover, there have been a variety of studies showing a strong correlation between free copper levels and the toxicity of copper on a variety of marine and fresh water organisms. Nevertheless, there are numerous reports in the literature that have used ISEs to monitor important anions such as fluoride, phosphate, sulfate, nitrate, nitrite, chloride, cyanide, etc., as well as other important cations such as ammonium and chromium(VI) in waste and natural waters. In conclusion, this review will present new and interesting perspectives on the application of ISEs in environmental analysis using approaches such as real-time remote monitoring of water quality, shipboard monitoring of environmentally important analytes using flow analysis instrumentation, the use of robust all-solid-state ISEs in submersible instruments for long-term deployment in the field, and innovative analytical approaches such as backside calibration and switchtrodes that avoid standard addition analysis and the concomitant perturbation in analyte speciation in natural samples.

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Response Mechanisms and New Approaches with Solid‐State Ion‐Selective Electrodes: A Powerful Multitechnique Materials Characterization Approach

et al. 2006

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In modern materials science, there is a plethora of characterization techniques of materials that can provide valuable insights into the fundamental chemical physics of solid-state devices such as chalcogenide glass ion-selective electrodes (ISEs). In this paper, electrochemical impedance spectroscopy (EIS), X-ray photoelectron spectrometry (XPS) and secondary ion mass spectrometry (SIMS) have been used in the elucidation of the mechanistic chemistry of the cadmium chalcogenide glass ISE. Furthermore, in situ synchrotron radiation-grazing incidence X-ray diffraction (SR-GIXRD), in situ EIS/SR-GIXRD, along with small angle neutron scattering (SANS), can be used to unravel the complex relationship between the nanostructure, bulk electrical conductivity and concomitant electrochemical reactivity of an iron chalcogenide glass ISE. Significantly, exciting preliminary modified atomic force microscopy (AFM) data -utilizing AFM cantilevers with attached microparticles of the copper sensing material jalpaitedemonstrate the tremendous potential of selective force ISE-AFM in the imaging of important molecular structures such as the copper ion channels of cell membranes in fish gills and/or phytoplankton.

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In situ electrochemical impedance spectroscopy/synchrotron radiation grazing incidence X-ray diffraction—A powerful new technique for the characterization of electrochemical surfaces and interfaces

Cited by 20 publications

References 31 publications

Response of the Iron Chalcogenide Glass Membrane Ion‐Selective Electrode in a Seawater Ligand Mimetic Calibration Buffer

Response of the Iron Chalcogenide Glass Membrane Ion‐Selective Electrode in a Seawater Ligand Mimetic Calibration Buffer

Ion‐Selective Electrode Potentiometry in Environmental Analysis

Response Mechanisms and New Approaches with Solid‐State Ion‐Selective Electrodes: A Powerful Multitechnique Materials Characterization Approach

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