The development of surface NMR-electrochemistry: A new in situ analytical probe to examine electrochemical interfaces
Slezak, Philip John
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https://hdl.handle.net/2142/22277
Description
Title
The development of surface NMR-electrochemistry: A new in situ analytical probe to examine electrochemical interfaces
Author(s)
Slezak, Philip John
Issue Date
1992
Doctoral Committee Chair(s)
Wieckowski, Andrzej
Department of Study
Chemistry
Discipline
Chemistry
Degree Granting Institution
University of Illinois at Urbana-Champaign
Degree Name
Ph.D.
Degree Level
Dissertation
Keyword(s)
Chemistry, Analytical
Language
eng
Abstract
Electrode potential-dependent NMR measurements of a $\sp{13}$C adsorbate on platinum were conducted for the first time. The method that I have developed has the capability of becoming a viable analytical technique in surface and solid-state electrochemistry. Using this method, carbon monoxide obtained from the decomposition of methanol was found to be bonded to a polycrystalline platinum electrode through linear and bridge configurations. Spin-spin and spin-lattice relaxation measurements were conducted to confirm the identification. Work completed previously by spectroelectrochemistry and gas-derived surface NMR measurements have been used for the data interpretation.
My thesis discusses the challenges of developing the surface NMR-electrochemistry method, as well as the solutions obtained to overcome them. Digitizing overload, RF penetration, vibrations, and the interfacing of electrochemistry to NMR are examined. Several second-generation probes, as well as computer simulations, were designed to expand the capabilities of this method. Analyses of a broad range of NMR spectra and cyclic voltammetry profiles of methanol-derived $\sp{13}$CO bonded to platinum are presented and discussed.
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