Operation Manual
®
Cartridger
C�670
096946
en
BÜCHI CartridgerTM C-670
Table of contents
Table of contents
1 Delivery package 2
2 Safety 3
3 Function 6
3.1 Principle of the packing process 6
3.2 Area of usage 6
4 Putting into operation 7
4.1 Location 7
4.2 Connecting to the vacuum tube to 7
the cartridge holder
4.3 Connecting the Cartridger to a vacuum source 8
4.4 Connecting the Cartridger to a compressed air or 8
gas supply
5 Operation 9
5.1 Checking the suction output 9
5.2 Overview of packing process 9
5.2.1 Selecting the stationary phase 11
5.2.2 Filling the stationary phase 11
5.2.3 Fluidization of the stationary phase 11
5.2.4 Inserting the first (lower) frit 12
5.2.5 Screwing in the cartridge 13
5.2.6 Packing the cartridge 13
5.2.7 Inserting the second (upper) frit 14
5.2.8 Removing the packed cartridge 14
5.3 Storing cartridges 14
5.4 Changing the stationary phase 14
5.5 After finishing work 15
Please be sure to read these operating instructions thoroughly before using the BÜCHI
CartridgerTM C-670. Keep these instructions
in the immediate proximity of the device so
that it is accessible at all times.
Chapter 2 contains important safety
instructions. Their observance is absolutely
necessary for safe operation of the device.
Technical changes may be carried out without prior notice. No
part of these operating instructions may be reproduced in any
form or processed, multiplied or distributed using electronic or
optical systems without the written permission of Büchi Labortechnik AG. All rights reserved.
Copyright © Büchi Labortechnik AG 2003
6 Maintenance 16
6.1 Cleaning the device 16
6.2 Replacing the safety frits 16
6.3 Customer service 17
7 Taking out of operation 18
7.1 Storage/transport 18
7.2 Disposal 18
8 Replacement parts and accessories 19
8.1 Replacement parts and accessories 19
8.2 Cartridges 20
9 Appendix 21
9.1 Technical data 21
9.2 Materials used 21
9.3 EU declaration of conformity 22
en, Version C (22 pages) Order no.
C-670 Operating instructions 96946
1
1 Delivery package
BÜCHI CartridgerTM C-670
1 Delivery package
Description Order no.
Büchi Cartridger C-670 44500
Included in delivery package
Cartridger module
Vacuum tube 17631
Cartridge holder 44530
Protective lid 44505
Test tube 44587
1 Operating instructions:
German 96945
English 96946
French 96947
Italian 96948
Spanish 96949
Table: Delivery package
Figure 1.1: BÜCHI Cartridger C-670
Figure 1.2: Cartridges C-675
2
BÜCHI CartridgerTM C-670
2 Safety
2 Safety
The device has been built according to the most up to date
technical standards and recognized safety regulations. However, use of the device still presents risks and hazards:
• when the device is not used according to the instructions.
• when the device is operated by inadequately trained
personnel
2.1 Symbols
Stop
Information concerning hazards that could result in significant
property damage or to life-threatening injuries.
Warning
Information concerning hazards that could result in damage
to health or property.
Note
Information pointing out technical requirements. Failure to
observe may result in malfunctions, inefficiency and reduced
productivity.
2.2 Requirements of the operator
The device may only be used by lab personnel and other persons
having an overview, on the basis of training or practical
experience, of the hazards involved in the operation of the device.
Personnel lacking this training or persons currently in training
require thorough instruction. The operating instructions form
the foundation for this purpose.
2.3 Correct usage
The device has been conceived of and constructed as a lab
device. Its correct usage is for the packing of Büchi Cartridges
C-675 with fluidized separation materials for liquid chromatography with the assistance of a vacuum.
Humidity and oil free compressed air or non-combustible gases
such as nitrogen or argon with 1 bar (15 psi) can be used for
fluidization. Never use combustible, explosive or reactive gases
for fluidization.
We do not recommend operating the Cartridger together with
a distillation apparatus for the packing process with vacuum.
The very rapid change of the vacuum during the packing process can lead to malfunctions.
3
2 Safety
BÜCHI CartridgerTM C-670
2.4 Incorrect usage
Any other usage than that mentioned in the above or any
usage not corresponding to the technical data is considered
to be incorrect usage. The operator bears exclusive
responsibility for any damages resulting from such usage.
2.5 Basic hazards
Basic hazards arise from:
• the evacuated tubes under vacuum conditions
• condensed gases
• fine grained separation materials: the inhalation of fine dust
with a particle size of < 10 µm can damage your health.
Do not use stationary phases with a high percentile of fine
dusts and observe the safety instructions of the stationary
phase intended for use. For safety reasons, the Cartridger
C-670 should be operated with an exhaust system or a
protective mask should be worn when packing cartridges
if there is no data sheet for the stationary phase.
The removal of lids with the assistance of a commercially
available tool is not permitted, with the exception of authorized
maintenance and repair personnel. The device may not be
operated with damaged glassware.
2.6 Instrument specific hazards
none
4
BÜCHI CartridgerTM C-670
3 Function
2 Safety
2.7 Safety measures
The wearing of personal protective gear such as safety glasses
and lab coat is obligatory.
These operating instructions must be available to the operators
at the location of the device at all times as a component of
the Cartridger C-670. Translations of these operating instructions Are available in English, German, French, Italian, Spanish
and Japanese.
Modifications
Modification of the device or of its replacement parts or accessories or usage of replacement parts or accessories other than
those mentioned in these operating instructions is only allowed
with the written permission of BÜCHI Labortechnik AG.
Responsibility of the operator
The operator is responsible for the instruction of his personnel.
These operating instructions can be ordered in other languages
to this purpose.
The operator must inform the manufacturer immediately of
any incidents occurring when using the device that are relevant to matters of safety.
5
3 Function
BÜCHI CartridgerTM C-670
3 Function
The function of the Cartridger is the packing of Büchi Cartridges
C-675 with separation materials for liquid chromatography.
3.1 Principle of the packing process
The packing process consists of two phases. In the first phase,
the stationary phase is fluidized by the flowing through of gas
or compressed air. Silica gel, for example, is thereby homogenized, and the friction of the particles against one another
is considerably reduced.
In the second phase the cartridge is packed using vacuum
and sealed with two frits.
3.2 Area of usage
The Cartridger is suitable for the dry packing of all Büchi
Cartridges C-675. The stationary phases to be packed must
be dry and have an identical particle size. Clumped starting
material is not suitable.
The permitted grain sizes for packing are between 30 and
200 µm. Smaller particles can not be packed dry. Larger particles are almost never used in chromatography. Silica gel with a
grain size of 40-63 µm is most often used in preparative
chromatography and is the most suitable.
6
BÜCHI CartridgerTM C-670
4 Putting into operation
4 Putting into operation
Inspect for damages after unpacking. It is important that
possible transport damage is immediately recognized upon
unpacking. It may be necessary to report transport damages
to your supplier.
The original packaging should be kept for possible later
transport or storage.
4.1 Location
The Cartridger can be used anywhere in the lab. The space
should be level, dry and free of vibration. Büchi recommends
operation in a clean exhaust system.
Operation in explosion-proof rooms is not permitted. Although
the Cartridger is not an electric device, the build-up of a static
charge during the packing process is not impossible.
Operation in refrigerated rooms, bathrooms, next to water
baths and in storerooms is not recommended. The large
surface of the stationary phases and the hygroscopic properties of many stationary phases (e.g. silica gel) can result in
contamination and changed chromatographic characteristics.
4.2 Connecting the vacuum tube to
the cartridge holder
The supplied tubes are designed for use with both vacuum and
compressed air up to 2bar. Connect the cartridge holder and
the Cartridger housing with the shorter tube (see Fig. 4.1).
Figure 4.1: Cartridge holder and Cartridger
7
4 Putting into operation
Figure 4.2: Cartridge holder
BÜCHI CartridgerTM C-670
Now fasten the other end of the tube to the cartridge holder
(see Fig. 4.2).
4.3 Connecting the Cartridger to a
vacuum source
Figure 4.3: Vacuum Indicator
The Cartridger has two connections on the back side (Figure
4.4). The upper connection is for the vacuum. The vacuum
pump should reach a final vacuum of 20mbar and have a
suction output greater than 1m3/min. The display panel on
the left side (Figure 4.3) is for easily ascertaining whether a
sufficient vacuum is present. If the display panel is red, either
the vacuum is not sufficient, the Cartridger is not vacuum
sealed or the vacuum valve on the front side of the device is
open.
4.4 Connecting the Cartridger to a
compressed air or gas supply
The lower connection on the rear side of the device is
connected to the compressed air or gas supply. The inlet
pressure should be between 1 bar (15psi) and 2 bar (30 psi)
and should not exceed this range. In-house compressed air
must be free of water and oil in order to prevent contamination
of the stationary phase and to avoid changing the water
content of the stationary phase.
Figure 4.4: Rear view
8
The use of in-house compressed air should be avoided if there
are doubts as to its quality.
All common inert lab gases can be used as an alternative to
compressed air (nitrogen, technical air, argon, helium).
BÜCHI CartridgerTM C-670
Figure 5.1 a/b: Checking the suction output
5 Operation
5 Operation
5.1 Checking the suction output
Check the suction output of the Cartridger at the cartridge
holder prior to each packing process. This is quite easy and
fast using the supplied cartridge with the glass ball. Screw in
the cartridge and open the vacuum valve. The ball should
quickly rise to the top and remain there. Cartridges cannot be
packed if it doesn’t rise, rises very slowly or falls to the bottom
again. Check the vacuum seal of the system, inspect and
replace the safety frits if necessary (see 6.2 Replacing the
safety frits). If the suction output is adequate following these
checks you can now begin to pack cartridges.
5.2 Overview of packing process
Selecting the stationary phase Preparing the filling process
Fluidization of the stationary
phase
Ready for packing
Filling the stationary phase
Inserting the first (lower) frit
Filling the stationary phase
Screwing in the cartridge
Dip into the stationary phase
Close the vacuum valve
9
5 Operation
BÜCHI CartridgerTM C-670
empty
Packing the cartridge Open the vacuum valve
full
Scratching out excess material
of stationary phase
Inserting the second (upper) frit
Vacuum valve still open
Inserting the second (upper) frit
Vacuum valve still open
Closing the vacuum valve
Removing the packed cartridge
After finishing work
10
BÜCHI CartridgerTM C-670
5 Operation
5.2.1 Selecting the stationary phase
The stationary phases to be packed must be dry and must
have a very uniform particle size range, e.g. clumped starting
material is unsuitable. The permissible particle sizes for packing
lie between 30 and 200µm. Modified phases can also be used
in this particle size range (C18, C8, C4, ...). Smaller particles
cannot be reliably packed.
Do not use phases containing fine dust particles that can
penetrate the lungs (particle size <10µm). These can endanger
your health.
Use DC plates to test which stationary phases are best suited
for your separation. Modified silica gels can also be packed
with the Cartridger (C18, C8, C4, NH2...).
Figure 5.1: Glass vessel with level indicator
5.2.2 Filling the stationary phase
Remove the black function lid and slowly empty your stationary
phase into the glass container. Please be sure not to overfill
the vessel (see the marking on the glass).
5.2.3 Fluidization of the stationary phase
The fluidization is based on a flow of gas (or air) through the
stationary phase. A frit is integrated into the bottom of the
glass vessel. The optimal gas flow is dependent upon the
grain size of the silica gel and can be set very precisely on the
right side using a needle valve. Be sure to close the needle
valve completely when using the Cartridger for the first time.
Fill the glass vessel and open the air supply to the Cartridger.
Next, slowly open the needle valve until the first air bubbles
appear on the surface of the gel. Inspect the fluidization with
a spatula. It should be possible to move the spatula through
the fluidized gel without resistance. However, the gel shouldn’t
bubble, meaning that the gel should have an even, calm
surface.
Figure 5.1: Needle valve for fine regulation of gas flow
Once the needle valve has been set, it need no longer be
adjusted as long as the admission pressure and the stationary
phase remain the same. At the end of the packing process
you need only shut off the main gas flow. Please turn on the
gas supply slowly prior to the next packing procedure.
11
5 Operation
Figure 5.3: Insertion device
BÜCHI CartridgerTM C-670
5.2.4 Inserting the first (lower) frit
Lay the first frit with a diameter of 12mm level in the recession
of the insertion device and insert the frit into the cartridge.
The insertion device is conceived of in such a way that the frit
is inserted in the correct insertion depth.
If you forget the first frit, the Cartridger is protected from contamination by a safety frit in the cartridge holder. In such a case
always be sure to replace the safety frit prior to continuing
packing (see 6.2 Replacing the safety frit).
12
BÜCHI CartridgerTM C-670
5 Operation
5.2.5 Screwing in the cartridge
Now screw the cartridge with the side of the frit into the
cartridge holder until the stop. Movement of the frit is prevented
by the stop.For short cartridges of 75 mm length use the
elongation.
5.2.6 Packing the cartridge
Submerge the cartridge into the fluidized gel. Open the valve
On the front side of the cartridger. The cartridge is filled all at
once. Leave the valve open and carefully withdraw the
cartridge from the glass vessel.
Adherent gel is cleaned from the cartridge by the brushes in
the lid. You should thereby directly clean off the gel projecting
beyond the length of the cartridge.
See also video of cartridge packing at the Buchi synthesis
homepage http://synthesis.buchi.com
Figure 5.6: Submerged cartridge with vacuum valve
13
5 Operation
BÜCHI CartridgerTM C-670
5.2.7 Inserting the second (upper) frit
햵
햴
Figure 5.7: Tools
햳
햶
햲
햷
Before inserting the second frit you must first use the appropriate tool (knife 햲 or 햳) in the lid to free the column start of
gel. The scraper knives have a stop that determines the depth.
Now insert the appropriate frit with 12 mm or 40 mm into the
insertion tool and insert the second frit.
햲 Knife Ø 12 mm
햳 Knife Ø 40 mm
햴 Punch Ø 40 mm
햵 Punch Ø 12 mm
햶 Brush set Ø 40 mm complete
햷 Stop sleeve
5.2.8 Removing the packed cartridge
Close the vacuum valve and unscrew the cartridge from the
cartridge holder. Finished. You can now use the cartridge for
chromatography.
Avoid jarring or blows. These can damage the column bed,
which unavoidably leads to worse separation performance.
5.3 Storing the cartridges
Büchi recommends packing the cartridges immediately prior
to use. If you intend to store supplies of filled cartridges, be
sure that the cartridge ends are properly sealed and that they
are stored protected from jarring and vibration. Most gels are
hygroscopic and have a bonding affinity with volatile chemicals.
Both effects have a negative influence on the separation
performance.
5.4 Changing the stationary phase
When changing the stationary phase it is particularly important
to thoroughly clean the glass vessel and the lid. This is best
undertaken with a vacuum cleaner and a dry, lint-free cloth.
Never use solvents or water!
14
BÜCHI CartridgerTM C-670
5 Operation
5.5 After finishing work
At the end of the packing process, shut off the vacuum source
and the gas supply. Where longer interruptions are intended
(app. 2 weeks, depending upon the ambient conditions), we
recommend transferring the remaining gel into a vessel that
can be tightly sealed and using this for storage purposes.
The glass vessel can also be separated from the Cartridger.
For daily usage it is usually sufficient to tightly press on the
white plastic lid.
Figure 5.8: Removal of the glass vessel
15
6 Maintenance
BÜCHI CartridgerTM C-670
6 Maintenance
6.1 Cleaning the device
No special cleaning is normally required when the device is
used correctly.
The housing can be wiped off with a damp cloth. Fine dust
from the gel can also be vacuumed.
6.1.1 Replacing the safety frit
The safety frit in the cartridge holder should be inspected from
time to time and be replaced as necessary. Use the small
cartridge with the glass ball to test the permeability of the frit.
If after opening the vacuum valve the ball rises quickly upwards
and remains there, the suction output is optimum and the
safety frit need not be exchanged.
To exchange the frit you need only unscrew the holder, replace
the frit and screw it tight again. Never try to blow out an
already used safety frit with compressed air or to clean it
„chemically“ or in an ultrasonic bath.
Incorrect operation of the Cartridger without a safety frit
shortens the useful life of the vacuum valve and the vacuum
pump. Such usage makes any guarantee claim null and void.
Figure 6.1: Procedure for replacing the safety frit
16
BÜCHI CartridgerTM C-670
6 Maintenance
6.2 Customer service
Only authorised service personnel can perform work on or in
the apparatus. These persons have a comprehensive technical
training and knowledge about hazards, resulting when safety
stipulations are not complied with. BÜCHI Customer Service
Office have apparatus specific Service Manual, which can
only be obtained by authorised personnel.
The addresses of the official BÜCHI Customer Service offices
are given on the last cover page of these operating instructions.
Please direct technical questions and application problems to
these offices in case of malfunction.
BÜCHI Customer Service is equipped to supply the following
services:
• replacement part service
• repair service
• maintenance service
• technical consultation
• Serviceve contracts
17
7 Taking out of operation
BÜCHI CartridgerTM C-670
7 Taking out of operation
7.1 Storage/transport
The device should be thoroughly cleaned. Chemical residue
must be removed without exception and the glass parts
washed. The device should be stored and transported in its
original packaging.
7.2 Disposal
We have provided a list of the materials used in the Appendix,
Chapter 9, in order to enable the disposal of the device in an
environmentally-friendly manner. In this way it can be ensured
that the parts are separated and can be reused. Please observe valid regional and local laws.
18
BÜCHI CartridgerTM C-670
8 Replacement parts and accessories
8 Replacement parts and
accessories
Only Büchi original accessories and replacement parts
guarantee safe usage and functionality of the device. The use
of replacement parts and accessories other than those from
Büchi is only allowed with the permission of the manufacturer.
The replacement parts catalog may only be used in connection
with the corresponding chapters 5 and 7 of the operating
instructions for assembly or disassembly purposes. Perusal
by and transfer to third parties as well as production according
to this handbook is not permitted. Büchi Labortechnik AG
maintains the copyright.
A
D
C
B
8.1 Replacement parts and accessories
Description Order no.
A 1 Safety frit set 44802
B 1 Fluidization vessel cpl. with tools 44800
C 1 Bottom frit and seal set 44801
D 1 Glass part of Fluidization vessel 44559
E 1 Brush set Ø 40 mm complete 44555
F 1 Stamp Ø 12 mm 44545
G 1 Stamp Ø 40 mm 44550
H 1 Knife Ø 40 mm 44540
I 1 Knife Ø 12 mm 44537
J 1 Pneumatic tube 5 m 44803
See next page for K - P
K 1 O-Ring for brush Ø 63 x 2,5 mm 44551
L 1 O-Ring Ø 38 x 2,5 mm 44538
M 1 O-Ring Ø 28 x 2,5 mm 44535
N 1 O-Ring string Ø 176 mm 44532
O 1 O-Ring string Ø 184 mm 44533
P 1 Elongation 44598
1 Operating instructions:
E
F
G
H
J
I
German 96945
English 96946
French 96947
Italian 96948
Spanish 96949
Table: Replacement parts and accessories
19
8 Replacement parts and accessories
N
Ø 176 mm
O
Ø 184 mm
BÜCHI CartridgerTM C-670
K
LM
P
8.2 Empty Cartridges
High transparent, chemical resistant polypropylene cartridges
including porous HD-polyethylene frits for packing with the
Büchi CartridgerTM C-670.
Figure 8.1: Empty Cartridges C-675
20
Cartridge inner
diameter (ID)
Cartridge length
Used for sample
range
Resulting
packing weight
with Si60
(40-63 µm)
cartridges incl. frits 50 50 50 50
Order No. 44880 44881 44882 44883
Table: Büchi Cartridges C-675
12 mm 12 mm 40 mm 40 mm
75 mm 150 mm 75 mm 150 mm
up to
200 mg
4 g 8 g 40 g 90 g
up to
400 mg
up to
1 g
up to
5 g
BÜCHI CartridgerTM C-670
9 Appendix
9.1 Technical data
BÜCHI CartridgerTM C-670
Device dimensions (W x H x D) 220 x 315 x 450 mm
Weight (empty) 7.5 kg
Power consumption none
Voltage none
Compatible cartridge sizes all Büchi Cartridges C-675
Prerequisites Gas/air and vacuum → oil-free and dry
Vacuum source: Vacuum flow ≥ 1 m3/h
Vacuum ≤ 20 mbar
Tube connections ID 6 mm for pressurized gas/air and vacuum
Table: Technical data
9 Appendix
9.2 Materials used
Description Materials Material code
Housing PUR
Glass parts Borosilicate glass 3.3
Plastic parts POM
Frits HD-PE
Seals NBR
Table: Materials used
21
9 Appendix
9.3 Declaration of conformity
We BÜCHI Labortechnik AG
Postfach, CH-9230 Flawil
Switzerland
declares, as exclusively responsible party, that the product:
BÜCHI CartridgerTM C-670
with which this declaration is concerned, conforms to the following norms:
EN 292-1:1991
Safety of machines; basic concepts, general principles of design
Part 1: Basic terminology, methodology
EN 292-2:1991 + A1:1995
Safety of machines – basic concepts, general principles of design
Part 2: Technical basic principles and specifications
BÜCHI CartridgerTM C-670
According to the determinations of the EU guideline:
89/392/EEC (Machine guideline)
Flawil, 11.06.2003
BÜCHI Labortechnik AG
Meierseggstrasse 40
9230 Flawil
Switzerland
Tel +41 (0)71 394 63 63 Guido Worch
Fax +41 (0)71 394 65 65 Quality manager
buchi@buchi.com
www.buchi.com
22
BÜCHI Labortechnik AG
CH- 9230
T +41 71 394 63 63
F +41 71 394 65 65
Flawil 1 / Switzerland
www.buchi.com Quality in your hands
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