Non-HPLC Rapid Separation of Metallofullerenes and Empty Cages with TiCl₄ Lewis Acid

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.

Bottom-up formation of endohedral mono-metallofullerenes is directed by charge transfer

“…Two metalencapsulated carbon cages are isolated from the resulting soot by chemical separation 19 , and then isomerically purified by multistep high-performance liquid chromatography (HPLC). The recovered species Pr@C 82 (I) and Pr@C 82 (II) 20 , labelled based on HPLC elution order, exhibit cages C 2v (9)-C 82 and C s (6)-C 82 .…”

Therapeutic applications of low-toxicity spherical nanocarbon materials

“…Currently, people are developing large-scale production methods and facile separation processes to obtain high-purity fullerenes at low cost so that Gd@C 82 (OH) 22 nanoparticles can be used in clinical applications. [74][75][76] CARBON NANOHORNS FOR DRUG DELIVERY Single-wall carbon nanohorns (SWNHs) are another type of nanocarbon material that has the potential to be useful in nano-medicine. SWNH has a horn-tipped, tubular single-walled graphite structure and is between 2 and 5 nm in diameter and between 40 and 50 nm in length.…”

Isolation and Crystallographic Characterization of Gd3N@D2(35)-C88 through Non-Chromatographic Methods

“…Stage 1 utilizes selective fractionation of Gd endohedrals by successive precipitation with two Lewis acids, namely, CaCl 2 and ZnCl 2 . 10,15,23,24 Stage 2 provides further selectivity by manipulating chemical reactivity differences of the various fullerenes and endohedral fullerenes with nucleophilic amines immobilized onto a solid support (stir and filter approach or SAFA). 9,11,12,25 By combining the selectivity of two different types of reagents (i.e., electron-poor and electron-rich), Gd 3 N@C 88 can now be isolated using simple solution chemistry, as opposed to the conventional method of HPLC as the sole separation method.…”