Three-Elfmode, Two-Compartment QuartzCell for Recording EPR Spectra During In Situ Electrolysis
The standard aqueous EPR (flat) sample Wildman eell (WG-812) has been modified for recording EPR spectra of short-lived radicals during in situ electrolysis, as shown in the figure. A is the platinum mesh working electrode, located in the flat section of the cell, which is filled with the solution containing the supporting eledrolyte and the electroactive substance. B is the platinum strip auxiliary electrode, separated from the working electrode via a medium glass frit (porosity, 31, immersed in the solution containing only the supporting electrolyte. C is the reference electrode (home-madeaqueous SCE), and D is a -pas bubbler with 1and 2, gas inlets; and 3, a pas outlet. The eell.. olaced in the ESR cavitv.. is filled with the previourly degassed solutims and the cyclic roltamrnetry is recorded {gas inlet, I ) , then the potentiostatically contn,llrd elecrrolysii is performed wasinlet. ?). This cell has several advantages over the electrolytic, one-compartment, Wildman cell (WG-810):
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The appearance of the EPR signal is quicker, because the working electrode is large and well-located. The radicals survive loneer in the s e ~ a r a t e dworkine" compartment. The stopcock E makes the complete filling of the cell easier. Nbola Poll lstituto di Teoria, Smmura Eleltmnica e CornparamentoSpnrochimim dei Cornpasti di Cwrdinazione dei C.N.R. Area della Ricerca di Rome P.O. Box 10 00016 Monterotondo Starlone (Rorna). Italy
970
Journal of Chemical Education
