NACALAI TESQUE COSMOSIL HPLC User manual

Contact us [ Japan ] [ International ]
Email ： [email protected] Email ： [email protected]
TEL ： [phone] TEL ： [phone]
FAX ： [phone] FAX ： [phone]
498 Higashitamaya-cho, Nijo Karasuma,
Nakagyo-ku, Kyoto 604-0855, Japan
For information on COSMOSIL HPLC columns and our database, the COSMOSIL Application,
an incredible source of application data, please visit our web site :
http://www.nacalai.com
C019-1212-1
1 / 2
For High Performance Liquid Chromatography
COSMOSIL®PACKED COLUMNS for fullerenes
Thank you for purchasing our COSMOSIL Packed Columns for fullerenes. Please read this manual carefully before use to ensure maximum
efficiency and a long column life.
COSMOSIL Packed Columns for fullerenes are packed with the silica gel that bonded specially designed stationary phase. Our columns are
shown in Table 1. Please choose the column suitable for your samples.
Table 1. Types of stationary phases and their characteristics
Packing material Buckyprep Buckyprep-M Buckyprep-D PBB
Silica gel High purity porous spherial silica
Average particle size 5μm
Average pore size approx. 120Å
specific surface area approx. 300m2/g
Stationary phase
Pyrenypropyl group Phenothiazinyl group Nitrocarbazolyl group Pentabromobenzyl group
End capping treatment Treatment None Treatment Treatment
Feature
Standard column for
fullerene separation.
Designed to separate
metallofullerenes.
Designed to separate
fullerenes derivatives.
Designed for
preparative separation
of C60, C70.
Table 2. Suggested solvents
Solvent Feature Solubility for C60 (mg/ml)
Toluene It is generally used to separation of fullerenes. 3.2
n-Hexane
Weak eluent than toluene.
0.046
n-Heptane **
Methanol* 0.001
2-Propanol* **
Acetonitrile* Weak eluent than toluene.
It is used for washing solvent before analysis with Buckyprep-D. 0.018
Chlorobenzene Stronger eluent than toluene. 7.0
o-Dichlorobenzene Stronger eluent than chlorobenzene. 27
1,2,4-Trichlorobenzene Strongest eluent. It can be used as a washing solvent for higher
fullerenes. 21.3
* In Buckyprep-D, they are stronger eluent than toluene.
(Note) Use them after filtration or distillation, if they are not for HPLC
1. INTRODUCTION
2. TYPES OF STATIONARY PHASES AND THEIR CHARACTERISTICS
Si
CH3
H3C
O
Br
Br
B
r
Br
Br
N
S
Si
H3CCH
3
N
Si
H
3
CCH
3
NO
2
O
2
N
Si
CH3
H3C
3. TROUBLESHOOTING

Contact us [ Japan ] [ International ]
Email ： [email protected] Email ： [email protected]
TEL ： [phone] TEL ： [phone]
FAX ： [phone] FAX ： [phone]
498 Higashitamaya-cho, Nijo Karasuma,
Nakagyo-ku, Kyoto 604-0855, Japan
For information on COSMOSIL HPLC columns and our database, the COSMOSIL Application,
an incredible source of application data, please visit our web site :
http://www.nacalai.com
C019-1212-1
2 / 2
1. Buckyprep-D has the fault of being hard to stabilize the baseline compared with other columns. In order to stabilize the baseline, it is
effective to wash acetonitrile about 10 minutes before analysis.
2. Avoid mechanical shocks to the column.
3. Connect the column according to the flow direction indicated on the label.
4. Keep pressure under 20MPa (15MPa in case of more than 10mmI.D). Take special care when using highly viscous mobile phase.
5. Elute the column with 20-30 ml mobile phase before connecting to the detector.
6. Use scrupulously degassed mobile phase. Air bubbles generate detection noise and accelerate column deterioration.
7. After analysis, wash the column with acid free, alkaline free and halogen free solvent. Store it tightly plugged.
8. Filter the sample before injection. Avoid precipitation at injection.
9. Removal of the end filters or change of the end-fittings will result in low performance of the column.
10. Do not tighten nuts more firmly than necessary.
11. Establish perfect chromatography conditions by experimenting with an analytical column of the same packing material before employing
a preparative column. Pay attention to impurities with longer retention time than your sample.
12. In order to maximize column performance, minimize the dead volume of mobile phase in the equipment by shortening and/or narrowing
the width of tubing.
13. Maintain constantly column and tubing temperature.
14. Avoid injecting air, changing flow rate rapidly and changing mobile phase at high flow rate.
15. Insoluble matters from the pumping system, mobile phase, or samples trapped in the filter at the inlet of the column may increase the
pressure.
16. We recommend using guard column to protect from irreversible adsorption on the packing material, clogging of the end filter by insoluble
matters, or rapid pressure increase.
17. We recommend keeping the chromatography conditions constant because frequent changes of mobile phases shorten column life.
Problem Possible Cause Solution
Increase of pressure Clogging of the end filter
Clogging of the packing material
Precipitation in the column
(1)
(2)
(2)
Poor resolution Contamination of packing material
Disorder of packing material
(2)(3)
Unregenerable
Split peak Void in the column Unregenerable
Unstable baseline Contamination of packing material
Contamination of mobile phase
(2)(3)
(4)
(1) Disconnect column from the detector. Wash with mobile phase through the column in reverse direction at half flow rate for 30 minutes.
(2) Wash the column with high solubility solvent.
(3) Wash the column with stronger eluent (ex.1,2,4-trichlorobenzene).
(4) Use the new solvent.
Nacalai Tesque will replace defective columns reported within 2 weeks of receipt. Nacalai Tesque approves return in case of:
(1) Damage during transportation caused by our incomplete packing.
(2) Theoretical plate number measured according to the test method specified in the Inspection Report is significantly lower than guaranteed.
(Please note that the plate number decreases when using apparatus with large dead volume or injecting big amount of sample.)
We cannot accept claims for deterioration of column performance caused by taking off the end filters or end-fittings or long shelf life.
Return shipment is unacceptable unless we have given prior permission and shipping instructions.
4. WARRANTY
4. CARE AND USE
5. TROUBLESHOOTING