Fullerene Separation Columns

Column Image

Separation of fullerenes, especially preparative scale separation, on conventional HPLC columns are always problematic due to the low solubility and low recovery rate of fullerenes. COSMOSIL offers a variety of columns designed for preparative scale separation of fullerenes including higher fullerenes, metallofullerenes and fullerene derivatives.


Packing material Buckyprep Buckyprep-M PBB PYE NPE
Silica gel High Purity Porous Spherical Silica
Average particle size 5 µm
Average pore size approx. 120
Specific surface area approx. 300 m2/g
Stationary phase Buckyprep
Bonding type Monomeric
End capping treatment Near-perfect None Near-perfect
Carbon content approx. 17% approx. 13% approx. 8% approx. 18% approx. 9%
Features Standard column for fullerenes separation. Designed to separate metallofullerenes. Designed for preparative separation of C60, C70. Separation of fullerene and structural isomers. Separation of fullerene derivatives

Product Informations

Comparison of retention in toluene

The figure below shows the retention time of C60 and C70 in toluene. Buckyprep, Buckyprep-M and PBB, and PYE nicely separate C60 and C70. On the other hand, C18 with alkyl group and NPE can not separate them in toluene.

retention in toluene

Column size 4.6 mm I.D. x 150 mm Column k' C60 k' C70 αC70/C60
Mobile phase Toluene PBB 2.22 5.43 2.44
Flow rate 1.0 ml/min Buckyprep 1.54 3.09 2.00
Temperature 30°C Buckyprep-M 1.12 1.79 1.59
Detection UV 312 nm PYE 0.71 1.46 2.06
Sample 1. C60 NPE 0.07 0.09 1.40
2. C70 5C18-MS-II 0.00 0.00 1.00

Solubility and boiling point of each solvent for C60

Solvent mg/ml b.p. (°C)
Methanol 0.001 64.5
Acetonitrile 0.018 81.8
n-Hexane 0.046 68.7
Toluene 3.2 111
Chlorobenzene 7.0 132
Carbon Disulfide 12 46.3
o-Dichlorobenzene 27 180
1,2,4-Trichlorobenzene 21.3 213

R. S. Ruoff, et al., J. Phy. Chem., 97, 3379 (1993)

The table above shows solubility and boiling point of each solvent for C60. Toluene is the most suitable solvent for due to its high solubility, appropriate boiling point, low cost and low corrosivity. Although C18 columns with alkyl groups can not separate C60 and C70 in toluene, by mixing acetonitrile and toluene, they can be separated as shown in the figure below. However, increasing injection volume in preparative purification triggers tailing that results in a practical injection volume limit of only 70 µl (175 µg). On the other hand, Buckyprep can separate well in toluene with no tailing with a maximum injection volume of 2,500 µl (6.25 mg).

Comparison with C18

Comparison with C18

Column size 4.6 mm I.D. x 250 mm
Mobile phase [5C18-MS-II] Toluene : acetonitrile = 55 : 45
[Buckyprep] Toluene
Flow rate 1.0 ml/min
Temperature 30°C
Detection UV 285 nm
Sample Fullerene toluene extract (2.5 mg/ml)

Suggested solvents

Solvents usable with Buckyprep series
Solvent Features C60 Solubility (mg/ml)
Toluene General-use solvent for fullerenes. 3.2
n-Hexane Weaker eluent than toluene. 0.046
n-Heptane **
Methanol 0.001
2-Propanol **
Acetonitrile Weaker eluent than toluene.
Chlorobenzene Stronger eluent than toluene. 7
o-Dichlorobenzene Stronger eluent than chlorobenzene. 27
1,2,4-Trichlorobenzene Strongest commonly-used eluent. Can be used to flush higher fullerenes. 21.3

Note: Use after filtration or distillation, if they are not HPLC grade.

Except for alkali aqueous and strong acid solutions, other solvents can be used (e.g., water-free pyridine and others). Depending on solvents, pay attention to high pressure caused by high solvent viscosity.


Fullerene Chromatogram Index

Fullerene Chromatogram Index includes more than 100 chromatograms is available at the website of The Fullerenes, Nanotubes and Graphene Research Society. (Click here to download)

Fullerene Chromatogram Index

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