Buckyprep-D offers improved separation for C₆₀ indene, a derivatized fullerenes, that has received much attention as the n-type semiconductor material of organic thin-film solar cell.

Buckyprep	Buckyprep-D
Data courtesy of Yusuke Tajima, Dr. Sci. Organic Optoelectronics Laboratory, RIKEN (Institute of Physics and Chemistry)

Buckyprep-D retains derivatized fullerenes longer than C₆₀. Therefore it is more suitable for preparative separation of derivatized fullerenes than conventional Buckyprep column.

5C18-MS-II	Buckyprep	Buckyprep-D

Buckyprep-D offers improved separation in toluene, a solvent with strong solubility for fullerenes (see Comparison with Conventional Type Columns above). It is necessary to mix in hexane with toluene when using the NPE column. (See table below.).

NPE

Column size:	4.6 mm I.D. x 250 mm
Mobile phase:	Toluene/Hexane = 25/75
Flow rate:	1.0 ml/min
Temperature:	30°C
Detection:	UV 325 nm
Sample:	1. [6,6]-Phenyl-C61 Butyric Acid Methyl Ester (1.5 µg) 2. [6,6]-Phenyl-C61 Butyric Acid Butyl Ester (1.5 µg) 3. C60 (1.5 µg)

Table: Solubility and Boiling Point of C₆₀ in Each Solvent

Condition	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
1,2,4-Trichlorobenzene	21.3	213
o-Dichlorobenzene*	27	180

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

Fullerene di-adduct

Buckyprep	Buckyprep-D

Azafulleroid

Buckyprep	Buckyprep-D

Fullerene Oxid

Buckyprep	Buckyprep-D

If the retention of derivatized fullerens on Buckyprep-D is too strong, shorten column length or add additives in toluene to decrease retention.

Using 50 mm Length Column

Buckyprep-D

Column size:	4.6 mm I.D. x 50 mm
Mobile phase:	Toluene
Flow rate:	1.0 ml/min
Temperature:	30°C
Detection:	UV 325 nm
Sample:	[6,6]-Diphenyl-C62 Bis (Butyric Acid Methyl Ester) [Bis[60]PCBM] (0.50mg/ml)
Inj. Vol:	10 µl

Adding Methanol

Buckyprep-D

Comparison of Each Solvent
Adding hexane or heptane to toluene increases retention on Buckyprep-D, while adding methanol or acetonitrile decreases retention. The effect of solvents on retention is the opposite to the conventional Buckyprep column.

Table. Comparison of percentage of retention ratio of each solvent on Buckyprep-D

Y-axis: Percentage of capacity factor k' when it is 100% toluene
X-axis: 10% of each solvent added into toluene

Adding Methanol Decreases Retention
Retention may decrease when a polar solvent is added on Buckyprep-D. For example, by increasing the methanol concentration to 1%, the retention dramatically decreases.

Buckyprep-D

Column size:	4.6 mm I.D. x 250 mm
Flow rate:	1.0 ml/min
Temperature:	30°C
Detection:	UV 325 nm
Sample:	[6,6]-Diphenyl-C62 Bis(Butyric Acid Methyl Ester) (0.5mg/ml)
Inj. Vol:	5.0 µl

Standard column for fullerenes → COSMOSIL Buckyprep
For separation of metallofullerenes → COSMOSIL Buckyprep-M
For separation of derivatized fullerenes → COSMOSIL Buckyprep-D

Solvent	Feature	Solubility of C60 (mg/ml)
Toluene	The most commonly used solvent	3.2
n-hexane		0.046
n-heptane	Weaker eluent than toluene	-
Methanol*		0.001
2-propanol*		-
Acetonitrile*	Weaker eluent than toluene. Recommended as a wash solvent for Buckyprep-D	0.018
Chlorobenzene	Stronger eluent than toluene	7.0
o-dichlorobenzene	Stronger eluent than chlorobenzene	27
1,2,4-trichlorobenzene	The strongest eluent. Recommended as a wash solvent	21.3

* These are stronger eluent on Buckyprep-D, opposite to Buckyprep.

Attenion:
Use HPLC Grade solvent or solvents after filtration or distillation. Except for alkali aqueous and strong acidic solutions, other solvents can be used (water-free pyridine and others). Depending on solvents, pay attention to high pressure caused by high solvent viscosity.

Note:
Baseline of Bukyprep-D is less stable relative to other fullerene columns. To stabilize baseline, let acetonitrile run through for 10 minutes before analysis.

Column	5 µm Buckprep-D
I.D. (mm)	2.0	4.6	10.0	20.0
Washing method	Wash with 1,2,4,-trichlorobenzene or other strong solvent to remove adsorbed contaminants.
Storage conditions	Wash column, then replace solvent with toluene. Plug tightly and store in a cool, dry place.
Max. pressure	20MPa		15MPa
Temperature range	The maximum usable temperature is 60°C. However. for regular use, please use at a constant temperature between 20°C and 50°C.

 

 

 

 

 

 

 

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. Used to wash Buckyprep-D before analysis.	0.018
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* When used with Buckyprep-D, they are stronger eluents than toluene.

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