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  • Non-HPLC rapid separation of metallofullerenes and empty cages with TiCl4 Lewis acid.

Non-HPLC rapid separation of metallofullerenes and empty cages with TiCl4 Lewis acid.

Journal of the American Chemical Society (2012-05-18)
Kazuhiko Akiyama, Tatsuyuki Hamano, Yusuke Nakanishi, Erina Takeuchi, Shoko Noda, Zhiyong Wang, Shiro Kubuki, Hisanori Shinohara
ABSTRACT

Rapid and efficient separation/purification of pure metallofullerenes M(x)@C(n) (M = metal; x = 1, 2; n > 70) and carbide metallofullerenes of the type M(y)C(2)@C(n-2) (y = 2, 3, 4; n - 2 > 68) has been reported. The present method utilizes rapid and almost perfect preferential formation of TiCl(4) (generally known as a Lewis acid)-metallofullerene complexes, which easily decompose to provide pure metallofullerene powders by a simple water treatment. The present method enables one to separate the metallofullerenes up to >99% purity within 10 min without using any type of high-performance liquid chromatography (HPLC). It is found that the oxidation potentials of the metallofullerenes are crucial factors for efficient purification. The current separation/purification technique may open a brand-new era for inducing further applications and commercialization of endohedral metallofullerenes.

MATERIALS
Product Number
Brand
Product Description

Sigma-Aldrich
Titanium tetrachloride, packaged for use in deposition systems
Sigma-Aldrich
Titanium(IV) chloride solution, 0.09 M in 20% HCl
Sigma-Aldrich
Titanium(IV) chloride solution, 1.0 M in methylene chloride
Sigma-Aldrich
Titanium(IV) chloride, ReagentPlus®, 99.9% trace metals basis