COSMOSIL HPLC Columns
Special Columns for Fullerenes
Separation of fullerenes, especially preparative-scale separation, on conventional HPLC columns is always problematic due to the low solubility and small recovery of fullerenes. COSMOSIL offers a variety of columns designed for preparative-scale separation of fullerenes including higher fullerenes, metallofullerenes and fullerene derivatives.
Material characteristics
| Packing material | Buckyprep | Buckyprep-M | PBB | PYE | NPE |
|---|---|---|---|---|---|
| Silica gel | high purity porous spherical silica | ||||
| Average particle size | 5 m | ||||
| Average pore size | approx. 120 | ||||
| Specific surface area | approx. 300 m2/g | ||||
| Stationary phase |  pyrenylpropyl group |
 phenothiazinyl group |
 pentabromobenzyl group |
 pyrenylethyl group |
 nitrophenylethyl group |
| Bonding type | monomeric | ||||
| End capping treatment | near-perfect | none | near-perfect | near-perfect | near-perfect |
| Carbon content | approx. 17% | approx. 13% | approx. 8% | approx. 18% | approx. 9% |
| Feature | 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 |
Comparison of retention in toluene
| Condition | |||||
|---|---|---|---|---|---|
| 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
Toluene is the most commonly used solvent for fullerene separation.
| Solvent | mg/ml | b.p. ( oC) |
|---|---|---|
| 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)
Comparison with C18
| Condition | |
|---|---|
| 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
| Chlorobenzene | Stronger eluent than toluene. Recommended for higher fullerenes. |
|---|---|
| o-Dichlorobenzene | Stronger eluent than chlorobenzene. |
| 1,2,4-richlorobenzene | Strongest eluent. It can be used as a washing solvent for higher fullerenes. To wash a column, inject 3 ml of1,2,4-trichlorobenzene to a 4.6 mm I.D. x 250 mm column and 50 ml to a 20 mm I.D. × 250 mm column after every operation. |
| n-Hexane | Weak eluent. Recommended for weakly retained fullerenes. |
| Acetonitrile | Weak eluent. Recommended for weakly retained fullerenes. |
Fullerene Chromatogram Index
Fullerene Chromatogram Index includes more than 100 chromatograms. If you are interested in this index, please feel free to e-mail us.
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