Single column purification of grain quantities of C[sub 70]

Journal Article · Wed Jul 27 04:00:00 EDT 1994 · Journal of the American Chemical Society; (United States)

DOI:https://doi.org/10.1021/ja00094a060· OSTI ID:6840938

Scrivens, W A; Cassell, A M; North, B L; Tour, J M ^[1]

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1. Univ. of South Carolina, Columbia, SC (United States)

Outlined here is a method for the purification of gram quantities of C[sub 70] from a crude fullerene mixture using activated charcoal (Norit A) and silica gel as a stationary phase in a flash chromatography column, after a single column pass, with toluene and o-dichlorobenzene (ODCB) as the mobile phases. During the solvent removal of the C[sub 70] enriched fractions, it was noticed that, if one carefully removes most of the ODCB via rotary evaporation at 85[degree]C, saturated solutions of C[sub 70] are made. These saturated solutions indicate a much higher solubility of C[sub 70] in hot ODCB than the known value of 24 mg/mL for C[sub 60] at room temperature. Initial observations indicate that solubilities of > 50 mg/mL may be obtained using hot ODCB. These solutions, if allowed to sit overnight, produce an abundance of long C[sub 70] crystals with 99.5% purity by HPLC analysis. 15 refs.

• OSTI ID: 6840938
• Journal Information: Journal of the American Chemical Society; (United States), Journal Name: Journal of the American Chemical Society; (United States) Vol. 116:15; ISSN JACSAT; ISSN 0002-7863
• Country of Publication: United States
• Language: English

Related Subjects

37 INORGANIC, ORGANIC, PHYSICAL, AND ANALYTICAL CHEMISTRY
400105 -- Separation Procedures
400201* -- Chemical & Physicochemical Properties
ACTIVATED CARBON
ADSORBENTS
ALKYLATED AROMATICS
AROMATICS
CARBON
CHLORINATED AROMATIC HYDROCARBONS
CHROMATOGRAPHY
ELEMENTS
FULLERENES
HALOGENATED AROMATIC HYDROCARBONS
HYDROCARBONS
NONMETALS
ORGANIC CHLORINE COMPOUNDS
ORGANIC COMPOUNDS
ORGANIC HALOGEN COMPOUNDS
PURIFICATION
SEPARATION PROCESSES
SILICA GEL
SOLUBILITY
TOLUENE