Analysis of experimental constraints and variables for time resolved detection of Fourier transform electrochemical impedance spectra

By using the Fourier transform (FT) technique, it is possible to perform electrochemical impedance spectroscopy in real time during the occurrence of DC voltage controlled surface reactions. The data obtained in this approach, a series of Nyquist plots as functions of DC control variables, can provide a wealth of time resolved information about surface kinetics. We discuss in detail the theoretical and experimental considerations for such time resolved experiments. We focus primarily on the constraints and criteria of measurements in the context of new data acquisition electronics that became available during the last few years. We also present sample experimental results for a gold electrode.

[1]  David J. Gavaghan,et al.  A complete numerical simulation of the techniques of alternating current linear sweep and cyclic voltammetry: analysis of a reversible process by conventional and fast Fourier transform methods , 2000 .

[2]  Allen J. Bard,et al.  Electrochemical Methods: Fundamentals and Applications , 1980 .

[3]  S. C. Creason,et al.  Fourier transform faradaic admittance measurements II. Ultra-rapid, high precision acquisition of the frequency response profile , 1972 .

[4]  C. M. Pettit,et al.  Electrodeposition of indium on molybdenum studied with optical second harmonic generation and electrochemical impedance spectroscopy , 2002 .

[5]  A full analytic treatment of reversible linear-scan voltammetry with square-wave modulation , 2002 .

[6]  J. Macdonald.  Some new directions in impedance spectroscopy data analysis , 1993 .

[7]  E. Brigham,et al.  The fast Fourier transform and its applications , 1988 .

[8]  Magnus Rosvall,et al.  A complete system for electrochemical impedance spectroscopy which combines FFT methods and staircase voltammetry , 2000 .

[9]  S. Ottow,et al.  In situ impedance spectroscopy of silicon electrodes during the first stages of porous silicon formation , 1997 .

[10]  D. Macdonald.  Review of mechanistic analysis by electrochemical impedance spectroscopy , 1990 .

[11]  R. N. Schindler,et al.  In-situ time resolved impedance spectroscopy of processes in the solid/liquid interface : electropolymerization of bithiophene , 1993 .

[12]  C. M. Pettit,et al.  Capacitance of a metal/liquid interface during anion adsorption: phase-selective measurement in the presence of d.c. voltage sweep and finite solution resistance , 1999 .

[13]  H. Takenouti,et al.  A specific aspect of impedance measurements in low conductivity media. Artefacts and their interpretations , 1990 .

[14]  R. N. Schindler,et al.  Effect of sample nonlinearity on the performance of time domain electrochemical impedance spectroscopy , 1995 .

[15]  C. M. Pettit,et al.  Analysis of potentiostatic current transients at metal/liquid interfaces: resolving the effects of a finite step interval , 2001 .

[16]  G. Popkirov,et al.  Fast time-resolved electrochemical impedance spectroscopy for investigations under nonstationary conditions , 1996 .

[17]  R. N. Schindler,et al.  A new approach to the problem of good and bad impedance data in electrochemical impedance spectroscopy , 1994 .

[18]  R. N. Schindler,et al.  A new impedance spectrometer for the investigation of electrochemical systems , 1992 .

[19]  J. Taylor.  An Introduction to Error Analysis , 1982 .

[20]  Minimal measurement time in electrochemical impedance identification , 1994 .

[21]  P. Griffiths.  Applications of the FFT in Electrochemistry , 1978 .

[22]  K. B. Oldham,et al.  Must ac voltammetry employ small signals , 2000 .

[23]  R. J. Loyd,et al.  High speed synchronous data generation and sampler system: application to on-line fast Fourier transform faradaic admittance measurements , 1977 .

[24]  R. N. Schindler,et al.  Optimization of the perturbation signal for electrochemical impedance spectroscopy in the time domain , 1993 .

[25]  B. Boukamp.  A Nonlinear Least Squares Fit procedure for analysis of immittance data of electrochemical systems , 1986 .

[26]  A. Bond,et al.  Numerical simulation of Fourier transform alternating current linear sweep voltammetry of surface bound molecules , 2002 .

[27]  R. N. Schindler,et al.  Validation of experimental data in electrochemical impedance spectroscopy , 1993 .

[28]  A. Bond,et al.  A unified approach to trace analysis and evaluation of electrode kinetics with fast Fourier transform electrochemical instrumentation , 1998 .

[29]  Ralph E. White,et al.  Comprehensive Treatise of Electrochemistry , 1981 .

[30]  C. M. Pettit,et al.  Surface kinetics of electrodeposited silver on gold probed with potential step and optical second harmonic generation techniques , 2001 .

[31]  R. N. Schindler,et al.  Time evolution of the active silver electrode area after immersion in cyanide containing solutions , 1997 .

[32]  C. M. Pettit,et al.  Kinetic analysis of electrosorption using fast Fourier transform electrochemical impedance spectroscopy: underpotential deposition of Bi3+ in the presence of coadsorbing ClO4− on gold , 2002 .