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The construction of a column‐shaped, thin‐layer ESR spectroelectrochemical cell for use at both ambient and low temperatures in nonaqueous solvents
Author(s) -
Mu X. H.,
Kadish K. M.
Publication year - 1990
Publication title -
electroanalysis
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.574
H-Index - 128
eISSN - 1521-4109
pISSN - 1040-0397
DOI - 10.1002/elan.1140020105
Subject(s) - chloride , platinum , analytical chemistry (journal) , perchlorate , layer (electronics) , electrode , materials science , electrochemistry , volume (thermodynamics) , thin film , methylene , electrochemical cell , spectral line , chemistry , chromatography , catalysis , composite material , ion , organic chemistry , nanotechnology , metallurgy , physics , quantum mechanics , astronomy
The construction and utilization of a column‐shaped in situ thin‐layer ESR spectroelectrochemical cell for both ambient and low temperature operation is reported. The working electrode is a columnshaped expanded platinum sheet of 9.4 × 4.0 mm that is placed in a 0.25 mm thick column‐shaped, thin‐layer chamber. The solution volume in the thin‐layer chamber is 12 μL, and the total solution volume in the cell ranges between 1 and 3 mL. The application of this cell is demonstrated by time‐resolved ESR spectra for electrooxidized porphyrins in methylene chloride solutions containing 0.3 M tetrabutylammonium perchlorate. The electrochemical behavior of this cell is also demonstrated by the oxidation of ferrocene under the same solution conditions at temperatures between 23 and −75°C. Well‐defined ESR spectra are obtained in as short as 5–10 seconds without data manipulation.