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Fullerene separation

Separation of fullerenes by HPLC

Fullerene separation by multi-step HPLC


First-step HPLC


The most efficient procedure for the separation of fullerenes is the HPLC (High Performance Liquid Chromatography). For instance, the separation of the fullerene mixture from C60 to C94 is made in two steps.

The following figure shows a preparative HPLC setup. This setup is used for the first separation step. After this first step the resulting fractions are: C60, C70, C76, C78, C80, C84, C86, C88, C90(I), C90(II), C92 and C94.

Preparative HPLC setup
preparative hplc system

The next figure shows a typical HPLC-chromatogramm. The separation was done on a praparative Buckyprep (Cosmosil, Japan) column with toluene being the mobile phase (flow rate: 10 ml/min).

HPLC chromatogramm of fullerene fractions
empty fullerenes HPLC chromatogramm

The main subject in fullerene research of our group are endohedral fullerenes. After the first HPLC-step the endohedral fullerenes are found in the fractions of higher empty fullerenes, for instance La@C82 is found in the C88 fraction. To clarify the composition of the fractions after the fitst HPLC-step, the fraction are investigated by mass spectrometry.

Second-step HPLC


After the mass spectrometric analysis the fractions are subject to the second-step HPLC separation.

In the left figure an analytical HPLC-System from Hewlett Packard (Series 1050) is shown. Furthermore a system from Abimed/Glison (right figure) is used for the separation of endohedral fullerenes.

Anlytical
HPLC setup
HPLC 1050HPLC Abimed

The following chromatogramms show the analytical separation of Sm@C74. In the end we reach a purity of 99 % by the separation.


Sepearation of Sm@C74 by HPLC
 Separation of Sm@C74


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Contact

Prof. Lothar Dunsch

Address: IFW Dresden

Helmholtzstraße 20
01069 Dresden

Germany
Phone: +49 351 4659 660
Fax: +49 351 4659 811
Email: L.Dunsch@ifw-dresden.de