University of North Florida
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Stuart Chalk, Ph.D.
Department of Chemistry
University of North Florida
Phone: 1-904-620-1938
Fax: 1-904-620-3535
Email: schalk@unf.edu
Website: @unf

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Journal of the Electrochemical Society

  • Publisher: The Electrochemical Society
  • FAD Code: JELS
  • CODEN: JESOAN
  • ISSN: 0013-4651
  • Abbreviation: J. Electrochem. Soc.
  • DOI Prefix: 10.1149/
  • Language: English
  • Comments: Fulltext available from 1930 v57

Citations 12

"Electrochemical Analysis Of Nitrofurans Based On Flow Injection Analysis On Pretreated Commercial Carbon Nanofiber Screen Printed Electrodes: Determination In Chicken Muscle Samples"
J. Electrochem. Soc. 2013 Volume 160, Issue 9 Pages H553-H559
P. Salgado-figueroa,P. Jara-ulloa,A. Alvarez-lueje,L. J. Nunez-vergara,J. A. Squella

"Hybrid Electrochemical Treatment For Persistent Metal Complex At Conductive Diamond Electrodes And Clarification Of Its Reaction Route"
J. Electrochem. Soc. 2006 Volume 153, Issue 12 Pages J123-J132
Yoko Yamaguchi, Yuki Yamanaka, Mayumi Miyamoto, Akira Fujishima, and Kensuke Honda

Abstract: The hybrid electrochemical treatment for persistent organometallic complexes [Cu-ethylenediaminetetraacetic acid (EDTA)] that was a combination of the reduction recovery of the center metal as nanoparticles and the oxidative decomposition of the organic ligand was attempted using the potential cycling at the oxygen-terminated boron-doped diamond (BDD) electrode. In the step of the recovery of the center metal of the organo-metal complex in the potential cycling from the reduction potential for Cu2+, by stepping up the anodic potential limit to the potential region for oxygen evolution reaction, the reionization of electrodeposited Cu could be suppressed in the presence of the dissolved oxygen. Moreover, separation of the electrodeposited Cu as nanoparticles from the electrode surface could be achieved by introducing the oxygen-containing functional groups on the diamond surface. The oxidation of the particle surface by the dissolved oxygen might induce the formation of the insulating layer and accelerate the separation by the electrostatic repulsive force between the oxygen-terminated surface and the insulating layer on the Cu particles. The reaction pathway of the Cu-EDTA treatment was analyzed using the long-term potential cycling at the potential region between the reduction potential of Cu and the oxidation potential of the EDTA. In flow injection analysis with the UV detector, the formation of the Cu particles by the reduction reaction of the Cu2+ ion from Cu-EDTA was clarified to mainly occur in the initial stage of the electrolysis. Moreover, in high-performance liquid chromatography analysis with the electrogenerated chemiluminescence detector for the treated solution, ethylenediaminetriacetic acid (ED3A) and ethylenediaminediacetic acid (EDDA) were observed. Therefore, it was confirmed that the liberated EDTA was oxidized to ED3A and EDDA through sequential removal of the acetate groups. An unidentified product (supposed to be the small size of a hydrocarbon) appeared after 100 h during the electrolysis. Although the concentration of this unidentified product was not decreased in the electrolysis with anodic potential limit of 2.3 V, the concentration decay for this product was observed for the potential cycling up to 3.0 V, suggesting that for the full oxidation of EDTA to CO2, it might be effective for the electrochemical oxidation by the OH radical available over 2.6 V at BDD.The Electrochemical Society © 2006 The Electrochemical Society.

"Design Of A Flow-Through Cell For Analysis Of Thiosulfate In Solutions Containing Copper And Ammonia"
J. Electrochem. Soc. 2004 Volume 151, Issue 7 Pages D51-D54
P. L. Breuer, M. I. Jeffrey, E. H. K. Tan, and A. W. Bott

Abstract: Thiosulfate is a potential alternative to cyanide in the recovery of gold. However, in the presence of copper and ammonia the solution chemistry is complex, and the thiosulfate concentration continually decreases due to its oxidation. The determination of the thiosulfate concentration by traditional techniques is difficult in leach solutions due to the interference from copper and other polythionates. A flow injection analysis method for thiosulfate has been developed which utilizes an electrochemical cell containing platinum and silver electrodes. The basis of the analysis is that the silver electrode measures the formation of the silver thiosulfate complex plus the oxidation/reduction of copper(I)/copper(II). In order to correct for copper, the charge for copper(I)/copper(II) is measured on the platinum electrode, and this is subtracted from the silver charge measured on the silver electrode. This provides a simple and robust analytical method for the analysis of thiosulfate in solutions used for gold leaching. ©2004 The Electrochemical Society. All rights reserved.

"Electrochemical Oxidation Of Alkylphenols On ECR-sputtered Carbon Film Electrodes With Flat Sub-nanometer Surfaces"
J. Electrochem. Soc. 2002 Volume 149, Issue 12 Pages E479-E484
Tianyan You, Osamu Niwa, Masato Tomita, Toshihiro Ichino, and Shigeru Hirono

Abstract: We prepared a new carbon film electrode by the electron-cyclotron-resonance (ECR) plasma sputtering method. The film is amorphous-like and different from the glassy carbon (GC), highly oriented pyrolytic graphite and diamond films that have previously been studied for use as electrode materials. We used cyclic voltammetry (CV) and flow injection analysis (FIA) with amperometric detection to compare the electrochemical properties of an ECR-sputtered carbon (SC) film electrode with those of a GC electrode and carbon film deposited by thermal chemical vapor deposition (T-CVD). The ECR-SC film electrode exhibited better electrochemical properties than the GC and T-CVD carbon electrodes, namely, a lower background current, a wider working potential window, and better reproducibility. CV with the ECR-SC film electrode did not reveal any large reduction in rho-nonylphenol (NP) and other alkylphenol (AP) peaks. In contrast, we observed a clear reduction in the CV and FIA peaks when we measured NP with GC and T-CVD carbon electrodes, indicating that there was much less deactivation from the NP oxidation products on the ECR-SC electrode surfaces. The NP calibration curve at the ECR-SC electrode in a flow system showed a linear concentration range of 0.125-10 muM with a detection limit of 50 nM (S/N = 3). (C) 2002 The Electrochemical Society.
Derivatization

"Determination Of Nitrite And Nitrogen Oxides By Anodic Voltammetry At Conductive Diamond Electrodes"
J. Electrochem. Soc. 2001 Volume 148, Issue 3 Pages E112-E117
Nicolae Spãtaru, Tata N. Rao, Donald A. Tryk, and Akira Fujishima

Abstract: The oxidation of nitrite at boron-doped diamond (BDD) electrode was investigated by use of anodic voltammetry. The voltammetric curves exhibit well-defined anodic peaks, with response that is superior to that obtained with glassy carbon electrodes. The influence of pH, nitrite concentration: and potential sweep rare on the electrode response was thoroughly investigated. The results show that the measurement of the oxidation peak current can be used as the basis for a simple, accurate, rapid method for the determination of NO2-. within a concentration range of 0.002-1 mM. Flow injection analysis with amperometric detection was also examined and improved sensitivity was observed, with analytical useful signals being obtained at 50 nM. The possibility of using anodic voltammetry for the determination of nitrogen oxides (NO and NO2 was also assessed. It is shown that BDD is a very promising electrode material for the detection of nitrogen oxides (NO,NO2) in gases and the determination of NO in aqueous solution. (C) 2001 The Electrochemical Society.

"Anodic Dissolution Of 304 Stainless Steel Using Atomic Emission Spectroelectrochemistry"
J. Electrochem. Soc. 2000 Volume 147, Issue 5 Pages 1770-1780
K. Ogle and S. Weber

Abstract: In this work a new spectroelectrochemical method based on an inductively coupled plasma atomic emission spectrometry has been developed and used to measure the elementary dissolution rates of Fe, Cr, Ni, Mn, Mo, and Cu simultaneously during linear scan voltammetry of a 304 stainless steel in the active region. Simultaneous dissolution was observed For all elements with the exception of copper. which appeared in solution at a potential approximately 100 mV more positive. The Tafel slopes for Fc, Cr, Ni, and Mn partial dissolution rates were measured around the corrosion potential and found to be identical within experimental error, between 59 and 68 mV/decade. The anodic dissolution of copper in acidic chloride and sulfate solutions was used to establish the quantitative relationship between the concentration transients and the dissolution rate. The residence time distribution of the electrochemical flow cell was determined using galvanostatic pulses of copper or stainless steel dissolution. The experimental residence time distribution could be approximated to a high degree of accuracy at both long and short times by a log-normal distribution. The effect of the residence time distribution on the shape of partial elemental current transients during linear scan voltammetry was investigated by numerical simulation.

"High Sensitivity Flow Injection Analysis Of Urea Using Composite Electropolymerized Polypyrrole-polyion Complex Film"
J. Electrochem. Soc. 1999 Volume 146, Issue 2 Pages 615-619
Tetsuya Osaka, Shinichi Komaba, Yusuke Fujino, Tomoka Matsuda, and Ikuo Satoh

Abstract: A highly sensitive and rapid flow injection system for urea analysis was constructed with a composite film of electropolymerized inactive polypyrrole (PPy) and a polyion complex incorporating urease. This system shows a sensitivity of 120 mV decade-1 and a lifetime of more than 80 assays. The origin of the high sensitivity of this system is attributed to an additional potential response of inactive PPy to ammonia or ammonium ion superimposed on the response to pH change. By injecting a concentrated buffer solution immediately after the sample injection, this system is capable of assaying more than 15 samples per hour.

"Characterizations Of Iron-containing Clay Modified Electrodes And Their Applications For Glucose Sensing"
J. Electrochem. Soc. 1998 Volume 145, Issue 1 Pages 154-158
Suh-Ching Shyu and Chong Mou Wang

Abstract: An amperometric biosensor was constructed on the basis of ruthenium purple-containing clay and glucose oxidase for the direct assay of glucose. These clay-modified electrodes were characterized by cyclic voltammetry and flow injection analysis techniques. The electrodes were very sensitive to the presence of glucose. Linear calibration curves between 10 µM and 15 mM with an electrode sensitivity of 3.88 µA/M and a detection limit of 10 µM were registered in aerated solutions (pH 5.1). Uric acid, ascorbic acid, and oxygen interfere very little with the detection of glucose. Long-term tests showed these clay electrodes were quite durable, e.g., the electrode sensitivity only decreases by ~25% over a period of six weeks.
Glucose Amperometry Sensor Electrode Electrode Interferences Apparatus Detector

"Characterization Of Iron-Containing Clay Modified Electrodes And Their Applications For The Detection Of Hydrogen Peroxide And Ascorbic Acid"
J. Electrochem. Soc. 1997 Volume 144, Issue 10 Pages 3419-3425
Suh-Ching Shyu and Chong Mou Wang

Abstract: Clays containing ruthenium purple (denoted clay/RP) were prepared and characterized by diffuse-reflectance ultraviolet-visible absorption spectroscopic and electrochemical methods. The characteristics of the clay-modified electrodes with or without RP were obtained and compared. The clay/RP electrodes displayed a remarkable ability for detection of hydrogen peroxide and ascorbate. When H2O2 or ascorbic acid was present, the current response was dramatically enhanced and tended to a limiting value, leading to a linear relationship with the bulk activity of the substrate. The rate constants (pseudo-first-order) were determined from Deltai/io vs. v^-1 plots and calculated to be 530 M^-1 s^-1 (pH 3.3) for H2O2, and 150 M^-1 s^-1 (pH 4) for ascorbic acid. Flow injection analysis showed that the detection limits for both substances were about 1 ppm at pH 5. Oxygen reduction causes little interference with the detection of H2O2, and this was tentatively ascribed to unfavorable electron transfer between oxygen and clay/RP particles.

"Platinization Of Shapable Electroconductive Polymer Film For An Improved Glucose Sensor"
J. Electrochem. Soc. 1996 Volume 143, Issue 10 Pages 3336-3342
Golam Faruque Khan; Wolfgang Wernet

Abstract: This paper describes a novel electrode material for the preparation of a first generation amperometric biosensor. The material consists of a flexible conductive polymer film of polypyrrole doped with polyanions and a layer of microporous Pt black, prepared electrochemically on the polymer film. Sensors fabricated with this material produce a comparatively higher H2O2 oxidation current at a lower applied potential. Glucose sensors were prepared by adsorbing glucose oxidase at the porous Pt black structure, covering with gelatin, and finally cross-linking with glutaraldehyde at dry condition. The developed sensors showed significantly improved performance over similar reported sensor systems. The performance of the glucose sensor was evaluated by a specially designed flow injection analysis (FIA) system. The sensors were continuously polarized at 25°C and glucose samples were automatically injected at 30 min intervals. The sensors worked at 0.3 to 0.4 V and produced a huge current response (>1 mA/cm2 with a wide linear range of detection (0 to 100 mM). The system effectively recycles oxygen, thus, the response current was not affected by a variation of oxygen concentration of the buffer. The interference of ascorbic acid, uric acid, bilirubin, etc. (at a physiological level) produced a current within the experimental error level. The sensor showed an extended working and shelf life.

"Measurement Of Trace Metallic Contaminants On Silicon Wafer Surfaces In Native And Dielectric Silicon Oxides By Vapor Phase Decomposition Flow Injection Inductively Coupled Plasma Mass Spectrometry"
J. Electrochem. Soc. 1993 Volume 140, Issue 4 Pages 1105-1109
J. Fucsko, S. S. Tan, M. K. Balazs

Abstract: The concentration of trace metals on silicon wafer surfaces was measured using a novel highly sensitive multi-element analytical method, called vapor phase decomposition flow injection inductively coupled plasma-mass spectrometry (ICP-MS). Metallic contaminants result in a deterioration in the performance and yield of semiconductor devices. ICP-MS uses hydrogen fluoride vapor to decompose and release metal contaminants from surface oxides. The metals are collected by scanning a small drop of dilute acid solution throughout the surface of the wafer and are measured by ICP-MS using flow injection sample introduction. As many as 60 elements can be determined with detection limits ranging from 108 to 1011 atom/cm2. ICP-MS has the potential to serve as a reference technique for the calibration of surface analytical methods, as well as offering an improved technique for measuring trace metals. One or more Si wafers were loaded into a specially constructed vapor-phase decomposition box containing a reservoir of HF solution The exposure time depends on the thickness of the oxide layer, 20 min for 15-30 .angstrom., 3-12 h for 2000-10 000 .angstrom.. A single drop of HF was then placed on the wafer surface and carefully rolled over the surface to extract the trace metals. The drop was transferred to a small sample tube and injected into the Ar ICP torch assembley with a cross-flow pneumatic nebulizer. Calibration was performed using multi-element standard solution For solution containing either 0.8 or 4.0 ppb of Mg, Cu, and Ni, and Cu the precision (n = 10) was ± 15% and ± 8%, respectively. The recovery of trace metals spiked on to bare Si wafers varied from 90-110% for Al, Cr, Fe, Ni and Na at surface concentration. of 5.67 x 1010-63.5 x 1010 atom/cm2. The recovery of Cu was 8.3% with the experimental conditions used. The detection limits were 108-109 atom/cm2 for Cr, Co, Fe, Pb, Mg, Mn, Ni, K, V, Zr, 2 x 1010 for Al and Fe and 1 x 1010 for Na. The procedure was applied to the determination of metal contaminants on bare Si wafers from different sources. Aluminum, Fe and Na are the most common metal contaminants.
Metals, trace Chromium Cobalt Iron Lead Magnesium Manganese Nickel Potassium Vanadium Zirconium Metal Inorganic compound Mass spectrometry Multielement

"Double-layer Perturbation For Ion Sensing In Liquid Chromatography"
J. Electrochem. Soc. 1988 Volume 135, Issue 9 Pages 2389-2390
TUNULI MS

Abstract: The increase in capacitive current that occurs upon contact adsorption at an electrode is free from interference by non-adsorbable species. Detection limits for I-, Br-, Cl- and SO42- at a AuCl electrode at 0.15 V are 0.1, 2 and 120 pmol and 2 nmol, respectively. Flow injection traces of 0.66 nmol of Br- at Au and AuCl electrodes show better sensitivity at the latter.
Bromine Chloride Iodide Sulfate Capacitance Electrode Electrode Interferences Sensitivity