Nonchromatographic “Stir and Filter Approach” (SAFA) for Isolating Sc₃N@C₈₀ Metallofullerenes

Authors

Steven Stevenson, University of Southern MississippiFollow
Kim Harich, Virginia Polytechnic Institute and state University
Hua Yu, University of Southern MississippiFollow
Ryan R. Stephen, University of Southern Mississippi
David Heaps, University of Southern Mississippi
Curtis Coumbe, University of Southern Mississippi
J. Paige Phillips, University of Southern MississippiFollow

Document Type

Article

Publication Date

7-12-2006

Department

Chemistry and Biochemistry

School

Mathematics and Natural Sciences

Abstract

Separation difficulties have led to a paucity of purified metallic nitride fullerenes (MNFs). Fundamental research and application development has been hampered with limited sample availability. Separation techniques designed to remove contaminant empty-cage fullerenes (e.g., C₆₀, C₇₀...C_2n) and classical metallofullerenes (e.g., non-MNFs) traditionally require expensive and tedious chromatographic methods. Our motivation is an alternative purification approach to minimize dependence on HPLC. Herein we report the use of cyclopentadienyl (CPD) and amino functionalized silica to selectively bind contaminant fullerenes. This “Stir and Filter Approach” (SAFA) provides purified MNF samples at ambient and reflux conditions. Under reflux conditions, purified MNFs (80% recovery, 41 h) are obtained using CPD silica. However, at room temperature, there is an equilibrium established between fullerenes and CPD silica, and no purified MNF samples are obtained using SAFA. In contrast, purified MNF samples (99+%) are readily obtained at room temperature using amino, diamino, and triamino silica at recoveries of 93% (11 h), 76% (9 h), and 50% (6 h), respectively.

Publication Title

Journal of the American Chemical Society

Volume

128

Issue

27

First Page

8829

Last Page

8835

Recommended Citation

Stevenson, S., Harich, K., Yu, H., Stephen, R. R., Heaps, D., Coumbe, C., Phillips, J. P. (2006). Nonchromatographic “Stir and Filter Approach” (SAFA) for Isolating Sc₃N@C₈₀ Metallofullerenes. Journal of the American Chemical Society, 128(27), 8829-8835.
Available at: https://aquila.usm.edu/fac_pubs/9050