Amperometric and fast scan-rate cyclic voltammetry detection at a microelectrode for gel permeation high-performance liquid chromatography of fullerenes

A study utilized amperometry and fast scan-rate cyclic voltammetry (CV) for detection and identification of fullerenes, which were separated by gel permeation high-performance liquid chromatography. The technique allows a rapid and feasible means for electrochemical characterization.

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Published inAnalytical chemistry (Washington) Vol. 65; no. 6; pp. 669 - 672
Main Authors Soucaze-Guillous, Benoit, Kutner, Wlodzimierz, Kadish, Karl M
Format Journal Article
LanguageEnglish
Published Washington, DC American Chemical Society 01.03.1993
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Abstract A study utilized amperometry and fast scan-rate cyclic voltammetry (CV) for detection and identification of fullerenes, which were separated by gel permeation high-performance liquid chromatography. The technique allows a rapid and feasible means for electrochemical characterization.
AbstractList Amperometry and fast scan-rate cyclic voltammetry (CV) at a 10-[mu]m-diameter platinum microelectrode were utilized for detection and in situ identification of fullerenes which were separated by gel permeation high-performance liquid chromatography. The microelectrode and inlet capillary nozzle were arranged perpendicularly. The limiting currents were virtually independent of the mobile phase flow rate in the range 0.1--2.0 mL min[sup [minus]1] for a distance between the microelectrode and inlet capillary nozzle [le] 0.10 mm. A toluene extract of the laser-vaporized soot containing low molecular mass fullerenes was resolved on two gel permeation columns which were connected in series. The mobile phase was dichloromethane/cyclohexane, 90/10 (v/v), 0.01 M tetra-n-butylammonium perchlorate. C[sub 60] and C[sub 70] were the major components of the extract and were present in a 3:1 mass ratio. Other higher fullerenes were also present in a 3:1 major concentration. The number and shapes of the peaks in chromatograms obtained with amperometric detection at [minus]1.3 V vs SCE were the same as those obtained with UV-visible spectroscopic detection at 366 nm, thus indicating that all of the detected compounds both absorb UV-visible light and are electrochemically active. Extracolumn peak broadenings due to detection and detectability (83.8 ng for C[sub 60]) were also the same in both detection techniques. In situ fast scan-rate voltammograms of C[sub 60] and C[sub 70] were obtained during elution, and the reversible E[sub 1/2] values of the third and fourth electroreductions could be used for their identification. 40 refs., 4 figs., 1 tab.
A study utilized amperometry and fast scan-rate cyclic voltammetry (CV) for detection and identification of fullerenes, which were separated by gel permeation high-performance liquid chromatography. The technique allows a rapid and feasible means for electrochemical characterization.
Author Kutner, Wlodzimierz
Soucaze-Guillous, Benoit
Kadish, Karl M
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  surname: Kadish
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Issue 6
Keywords Cyclic voltammetry
Amperometry
HPLC chromatography
Microelectrode
Fullerenes
Atomic cluster
Qualitative analysis
Gel permeation chromatography
Electrochemical detector
Language English
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Snippet A study utilized amperometry and fast scan-rate cyclic voltammetry (CV) for detection and identification of fullerenes, which were separated by gel permeation...
Amperometry and fast scan-rate cyclic voltammetry (CV) at a 10-[mu]m-diameter platinum microelectrode were utilized for detection and in situ identification of...
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SubjectTerms 360600 - Other Materials
400201 - Chemical & Physicochemical Properties
AMPEROMETRY
Analytical chemistry
Biochemistry
CARBON
CHEMICAL ANALYSIS
Chemistry
Chromatographic methods and physical methods associated with chromatography
CHROMATOGRAPHY
DETECTION
ELEMENTS
Exact sciences and technology
FULLERENES
GEL PERMEATION CHROMATOGRAPHY
INORGANIC, ORGANIC, PHYSICAL AND ANALYTICAL CHEMISTRY
LIQUID COLUMN CHROMATOGRAPHY
MATERIALS SCIENCE
NONMETALS
Other chromatographic methods
QUANTITATIVE CHEMICAL ANALYSIS
Scientific imaging
SEPARATION PROCESSES
TITRATION
VOLTAMETRY
Title Amperometric and fast scan-rate cyclic voltammetry detection at a microelectrode for gel permeation high-performance liquid chromatography of fullerenes
URI http://dx.doi.org/10.1021/ac00054a003
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