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 Title: The development of surface NMR-electrochemistry: A new in situ analytical probe to examine electrochemical interfaces Author(s): Slezak, Philip John Doctoral Committee Chair(s): Wieckowski, Andrzej Department / Program: Chemistry Discipline: Chemistry Degree Granting Institution: University of Illinois at Urbana-Champaign Degree: Ph.D. Genre: Dissertation Subject(s): Chemistry, Analytical 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. Issue Date: 1992 Type: Text Language: English URI: http://hdl.handle.net/2142/22277 Rights Information: Copyright 1992 Slezak, Philip John Date Available in IDEALS: 2011-05-07 Identifier in Online Catalog: AAI9305698 OCLC Identifier: (UMI)AAI9305698
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