Teachware
Metrohm AG
CH-9100 Herisau
teachware@metrohm.com
This documentation is protected by copyright. All rights reserved.
Although all the information given in this documentation has been
checked with great care, errors cannot be entirely excluded. Should you
notice any mistakes please send us your comments using the address
given above.
Documentation in additional languages can be found on
The 930 Compact IC Flex is operated solely using the MagIC Net software.
A USB cable is used to connect the instrument to a computer with
MagIC Net installed. The intelligent software detects the instrument automatically and checks its functionality. The software controls and monitors
the instrument, evaluates the measured data and manages it in a database.
The 930 Compact IC Flex Oven/SeS/PP/Deg consists of the following modules:
Leak sensor
The leak sensor detects leaking liquid that collects in the instrument's base
tray. Liquid that leaks in the instrument is routed to the base tray using
drainage tubing and detected there.
Column oven
The column oven tempers the separation column and the eluent and
thereby provides stable measuring conditions. A column holder with a
chip reader is located in the column oven.
Eluent degasser
The eluent degasser removes gas bubbles and dissolved gases from the
eluent.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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1.1 Instrument description
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High-pressure pump
The intelligent and low-pulsation high-pressure pump pumps the eluent
through the system. It is equipped with a chip where its technical specifications and "life history" (operating hours, service data, etc.) are saved.
Inline filter
Inline filters protect the separation column reliably from potential contamination from the eluent. The small filter pads with 2 µm pore size can be
replaced quickly and easily. They remove particles from the solutions, such
as bacteria and algae.
Pulsation absorber
The pulsation absorber protects the separation column from damage
caused by pressure fluctuations when switching the injection valve, and
reduces interfering pulsations during highly sensitive measurements.
Injection valve
The injection valve connects the eluent path to the sample path. By a
quick and precise switching of the valve a quantity of sample solution
defined by the size of the sample loop is injected and flushed to the separation column with the eluent.
Suppressor
The suppressor consists of a suppressor drive, a rotor and, where applicable, an adapter. The suppressor drive gives you the flexibility to use different rotors according to the principle "one drive – many rotors". With
appropriate adapters, the rotor for the sample preparation module (SPM
Rotor) or suppressor rotors with different capacities and construction can
be easily exchanged. The rotors are not included in the instrument's scope
of delivery. A rotor suitable for the application must be ordered separately.
Peristaltic pump
The peristaltic pump is used for pumping sample and auxiliary solutions. It
can rotate in both directions.
Metrohm CO2 Suppressor (MCS)
The Metrohm CO2 Suppressor (MCS) removes the CO2 from the eluent
flow. This lowers the background conductivity, improves detection sensitivity and minimizes the injection peak and carbonate peak.
Detector
Metrohm offers a series of different detectors for various analysis tasks. A
suitable detector type must be ordered as a separate accessory.
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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Sample degasser
The sample degasser removes gas bubbles and dissolved gases from the
sample.
Separation column
The intelligent separation column separates different components according to their interactions with the column. Metrohm separation columns
are equipped with a chip where their technical specifications and history
(start-up, operating hours, etc) are stored.
1.2 Intended use
The 930 Compact IC Flex Oven/SeS/PP/Deg is used for the determination
of anions or polar substances with sequential suppression using ion chromatography.
Sequential suppression consists of:
1 Introduction
■Chemical suppression with a Metrohm Suppressor Module (MSM) and
subsequent
■CO2 suppression with the Metrohm CO2 Suppressor (MCS).
Background conductivity is reduced to a minimum with sequential suppression.
The instrument can also be used as needed for the determination of cations or anions without chemical suppression.
The present instrument is suitable for processing chemicals and flammable
samples. Usage of the 930 Compact IC Flex therefore requires the user to
have basic knowledge and experience in handling toxic and caustic substances. Knowledge with respect to the application of the fire prevention
measures prescribed for laboratories is also mandatory.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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1.3 Safety instructions
1.3 Safety instructions
1.3.1 General notes on safety
WARNING
This instrument may only be operated in accordance with the specifications in this documentation.
This instrument has left the factory in a flawless state in terms of technical
safety. To maintain this state and ensure non-hazardous operation of the
instrument, the following instructions must be observed carefully.
1.3.2 Electrical safety
The electrical safety when working with the instrument is ensured as part
of the international standard IEC 61010.
WARNING
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Only personnel qualified by Metrohm are authorized to carry out service
work on electronic components.
WARNING
Never open the housing of the instrument. The instrument could be
damaged by this. There is also a risk of serious injury if live components
are touched.
There are no parts inside the housing which can be serviced or replaced
by the user.
Mains voltage
WARNING
An incorrect mains voltage can damage the instrument.
Only operate this instrument with a mains voltage specified for it (see
rear panel of the instrument).
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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Protection against electrostatic charges
WARNING
Electronic components are sensitive to electrostatic charges and can be
destroyed by discharges.
Do not fail to pull the mains cable out of the mains connection socket
before you set up or disconnect electrical plug connections at the rear
of the instrument.
1.3.3 Tubing and capillary connections
CAUTION
Leaks in tubing and capillary connections are a safety risk. Tighten all
connections well by hand. Avoid applying excessive force to tubing
connections. Damaged tubing ends lead to leakage. Appropriate tools
can be used to loosen connections.
1 Introduction
Check the connections regularly for leakage. If the instrument is used
mainly in unattended operation, then weekly inspections are mandatory.
1.3.4 Flammable solvents and chemicals
WARNING
All relevant safety measures are to be observed when working with
flammable solvents and chemicals.
■Set up the instrument in a well-ventilated location (e.g. fume cup-
board).
■Keep all sources of flame far from the workplace.
■Clean up spilled liquids and solids immediately.
■Follow the safety instructions of the chemical manufacturer.
1.3.5 Recycling and disposal
This product is covered by European Directive 2002/96/EC, WEEE – Waste
from Electrical and Electronic Equipment.
The correct disposal of your old equipment will help to prevent negative
effects on the environment and public health.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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1.4 Symbols and conventions
More details about the disposal of your old equipment can be obtained
from your local authorities, from waste disposal companies or from your
local dealer.
1.4 Symbols and conventions
The following symbols and formatting may appear in this documentation:
Cross-reference to figure legend
The first number refers to the figure number, the second to the instrument part in the figure.
Instruction step
Carry out these steps in the sequence shown.
MethodDialog text, parameter in the software
File ▶ NewMenu or menu item
[Next]Button or key
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WARNING
This symbol draws attention to a possible life-threatening hazard or risk of injury.
WARNING
This symbol draws attention to a possible hazard due
to electrical current.
WARNING
This symbol draws attention to a possible hazard due
to heat or hot instrument parts.
WARNING
This symbol draws attention to a possible biological
hazard.
CAUTION
This symbol draws attention to possible damage to
instruments or instrument parts.
NOTE
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This symbol highlights additional information and
tips.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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2 Overview of the instrument
2.1 Front
2 Overview of the instrument
Figure 1Front
Bottle holder
1
Column oven
3
Sample degasser
5
Injection valve
7
Pulsation absorber
9
High-pressure pump
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
Column holder
2
Suppressor
4
Inline filter
6
Purge valve
8
Base tray
10
Eluent degasser
12
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7
2.2 Rear
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Peristaltic pump
13
Detector chamber
15
Room for the detector and the adsorption
cartridges for the MCS.
2.2 Rear
Metrohm CO2 Suppressor (MCS)
14
1
3
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8
Figure 2Rear
Bottle holder
Knurled screws
For fastening the removable back panel.
Drainage tubing connection
2
For connecting the drainage tubing, which
guides escaped fluids away from the bottle
holder.
Back panel
4
Removable. Enables access to the detector
chamber.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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2 Overview of the instrument
Drainage tubing connection
5
For connecting the drainage tubing, which
guides escaped fluids away from the detector chamber.
Exhaust opening
7
Labeled Exhaust. For extracting the air from
the vacuum chamber.
Service connection socket
9
For Metrohm service only.
Drainage tubing connections
11
For connecting two drainage tubings that
guide the escaped fluid to the leak sensor
and from there to the waste container.
Type plate
13
Leak sensor connection socket
15
Labeled Leak Sensor. For connecting the
leak sensor connection cable.
MSB connection sockets
17
Labeled MSB 1 and MSB 2. For connecting
MSB devices.
Transport locking screws
6
For securing the vacuum pump when transporting the instrument.
Auxiliary connection socket
8
For connecting an 891 Professional Analog
Out (2.891.0010).
Transport locking screws
10
For securing the high-pressure pump when
transporting the instrument.
Base tray
12
With leak sensor.
Serial number
14
Detector connection socket
16
Labeled Detector. For connecting Metrohm
detectors.
USB connection sockets
18
Labeled USB 1 and USB 2. For connecting
USB devices.
PC connection socket
19
For connecting the instrument to the computer with the USB cable (6.2151.020).
Power socket
21
Power socket for connecting the power
cable and power switch for switching the
instrument on and off.
Vacuum connection
20
Plugged with a stopper.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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2.3 Feed-throughs for capillaries and cables
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2.3 Feed-throughs for capillaries and cables
Multiple openings are available for leading capillaries into the instrument
and for leading capillaries and cables out of the instrument:
■Openings on the door
■Openings on the back panel
■Ducts between the instrument and the base tray as well as between
the instrument and the bottle holder (see Figure 5, page 12)
Openings on the door
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Figure 3
Luer connector
1
For connecting a capillary from inside and
for inserting a syringe (6.2816.020) from
outside. For manual sample injection.
An opening for up to 3 capillaries is located on the door of the instrument.
The two Luer connections above are not actually openings; the capillaries
are fastened to the Luer connection from within using PEEK pressure
screws. You can use a syringe to inject or draw out liquid from the outside.
Feed-throughs on the door
Opening for capillaries
2
For up to 3 capillaries.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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2 Overview of the instrument
Openings on the back panel
Openings for capillaries
1
Figure 4Openings for capillaries and cables
Openings for cables
2
The removable back panel is outfitted with openings through which capillaries and cables can be lead out of the detector chamber.
Ducts for capillaries
There are ducts for capillaries between the instrument and base tray as
well as between the instrument and the bottle holder. The capillaries can
be fed to the front of the instrument from both sides of the instrument
and from the front of the instrument to the back of the instrument.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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2.3 Feed-throughs for capillaries and cables
Figure 5Ducts for capillaries
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3 Installation
3.1 Setting up the instrument
3.1.1 Packaging
The instrument is supplied in highly protective special packaging together
with the separately packed accessories. Keep this packaging, as only this
ensures safe transportation of the instrument.
3.1.2 Checks
Immediately after receipt, check whether the shipment has arrived complete and without damage by comparing it with the delivery note.
3.1.3 Location
The instrument has been developed for operation indoors and may not be
used in explosive environments.
3 Installation
Place the instrument in a location of the laboratory which is suitable for
operation, free of vibrations, protected from corrosive atmosphere, and
contamination by chemicals.
The instrument should be protected against excessive temperature fluctuations and direct sunlight.
3.2 Capillary connections in the IC system
Generally speaking, capillary connections between two components of an
IC system are made up of one connection capillary and two pressure
screws used to connect the capillary to the respective components.
Pressure screws
Three types of pressure screws are used in the IC system:
Number
6.2744.010 / 6.2744.014Pressure screwOn the injection valve
Pressure screws are tightened and loosened by hand. A tool is not
needed.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3.2 Capillary connections in the IC system
Also see: PEEK pressure screws video on the Internet http://ic-
help.metrohm.com/maintenance.php?chapter=1_2.
Connection capillaries
PEEK capillaries and PTFE capillaries are used in the IC system.
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PEEK capillaries (polyetheretherketone)
PTFE capillaries
(poly(tetrafluoroethylene))
PEEK capillaries are temperature-resistant up to 100 °C, stable under pressure up to 400 bar (depending on the inner diameter), flexible, chemically
inert and have an extremely smooth surface. They can be readily cut down
to the desired length with the capillary cutter (6.2621.080).
Use:
■PEEK capillaries with an inner diameter of 0.25 mm (6.1831.010) for
the entire high-pressure section.
■PEEK capillaries with an inner diameter of 0.75 mm (6.1831.030) for
sample processing in the ultratrace range.
PTFE capillaries are transparent and enable visual tracing of the liquids to
be pumped. They are chemically inert, flexible and temperature-resistant
up to 80 °C. They can be readily cut down to the desired length with the
capillary cutter (6.2621.080).
Use:
PTFE capillaries (6.1803.0x0) are used for the low-pressure section.
■PTFE capillaries with an inner diameter of 0.5 mm for sample process-
ing.
■PTFE capillaries with an inner diameter of 0.97 mm for sample process-
ing and rinsing solutions (they are not necessarily included in the scope
of delivery of the instrument).
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Capillary connections
NOTE
If you work with an increased system pressure (> 15 MPa), capillaries
may slip out of the pressure screws.
To avoid this, we recommend degreasing the ends of the capillaries
before installing them.
Dampen a cloth with acetone and wipe off the ends of the capillaries
before connecting them with the pressure screws.
In order to achieve optimum analysis results, capillary connections in an IC
system must be absolutely tight and free of dead volume. Dead volume
occurs if two capillary ends connected to each other do not fit exactly,
thus allowing liquid to escape. There are two possible causes for this:
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3 Installation
■The capillary ends do not have exactly flat edges.
■The two capillary ends do not completely meet.
One prerequisite for dead-volume-free capillary connection is that both
capillary ends are cut exactly flat. Therefore we recommend cutting PEEK
capillaries only with a capillary cutter (6.2621.080).
Also see: Cutting capillaries video on the Internet http://ic-
help.metrohm.com/maintenance.php?chapter=1_1.
Creating dead-volume-free capillary connections
To create dead-volume-free capillary connections, proceed as follows:
Wipe off the end of the capillary with a cloth dampened with ace-
1
tone.
Slide the pressure screw over the capillary. Ensure that the capillary
2
protrudes 1 to 2 mm from the tip of the pressure screw.
Push the capillary into the connection or coupling as far as it will go
3
and hold it there.
Only then start turning the pressure screw.
4
Colored sleeves for PEEK capillaries
The enclosed set of varicolored sleeves for PEEK capillaries (6.2251.000)
serves to easily differentiate the various flows of liquid in the system
through color coding. Each capillary conveying a given liquid (e.g. eluent)
can be marked with sleeves of the same color.
Slide a sleeve of a selected color over a capillary and move it to an
1
easily visible position.
Heat the colored sleeve, such as with a hairdryer.
2
The colored sleeve shrinks and adapts to the shape of the capillary.
NOTE
In order to arrange capillaries more clearly, they can be bundled with
the spiral band (6.1815.010).
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3.3 Removing transport locking screws
3.3 Removing transport locking screws
To avoid damage to the drives for the high-pressure pump and the vacuum pump during transport, the pumps are secured with transport locking screws. These are located at the rear of the instrument and labeled
with Transport security screws.
Remove these transport locking screws before the initial start-up.
AccessoriesFor this step you need:
■Hex key 4 mm (6.2621.030)
Remove the transport locking screws
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Figure 6
Transport locking screws
1
For the vacuum pump. Only present if the
instrument has a degasser.
Remove all of the transport locking screws with the hex key.
1
Store the transport locking screws in a safe place. Reinsert the transport
locking screws each time you transport the instrument a significant distance.
Removing the transport locking screws
Transport locking screws
2
For the high-pressure pump.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3 Installation
CAUTION
The pumps may be damaged if you transport the instrument without
inserting the transport locking screws.
3.4 Connecting the drainage tubing and leak sensor
The leak sensor detects leaking liquid that collects in the instrument's base
tray. Liquid that leaks in the bottle holder or in the detector chamber is
routed to the base tray using drainage tubing and is detected there.
If the leak sensor detects a leak in the IC system, the IC instrument is
switched off and a warning is output in the software.
The leak sensor functions properly only if the following preconditions are
met:
■The drainage tubing is connected.
■The leak sensor connection cable is inserted into the leak sensor con-
nection socket.
■The 930 Compact IC Flex is switched on.
■The leak sensor is switched to active in the software.
3.4.1 Installing the drainage tubing
Liquid that leaks in the bottle holder or detector chamber flows to the rear
of the instrument and is drained through openings on the bottle holder
and in the detector chamber. The drainage tubing has to be mounted at
these openings. This drainage tubing guides the leaking liquid to the base
tray where the leak sensor is located.
Accessories
For this step you need the following parts from the accessory kit: Vario/
Flex Basic (6.5000.000):
3.4 Connecting the drainage tubing and leak sensor
Connecting the drainage tubing
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Cut a piece of silicone tubing into three pieces using scissors: 2 ×
1
approx. 40 cm and 1 × 20 cm
Attach one end of the 40 cm long piece to the drainage tubing con-
2
nection on the bottle holder.
Attach one end of the 20 cm long piece to the drainage tubing con-
3
nection on the detector chamber.
Attach each of the loose ends of both pieces of silicone tubing to
4
one end of the Y connector.
Attach one end of the second 40 cm long piece to the third end of
5
the Y connector.
Attach the loose end to the right-side drainage tubing connection on
the base tray.
Attach one end of the second piece of silicone tubing to the left-side
6
drainage tubing connection on the base tray.
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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Route the loose end into a waste container.
3.4.2 Connecting the leak sensor
Plugging in the leak sensor connection cable
The leak sensor connection cable is coiled up in the base tray.
3 Installation
Pull the leak sensor connection cable out of the base tray as far as
1
needed.
Plug the plug for the leak sensor connection cable into the leak sen-
2
sor connection socket (labeled Leak Sensor).
3.5 Column oven
The column oven ensures that the separation occurs at a constant temperature. It is firmly sealed by the instrument's smaller door and is well insulated. The capillaries are fed through small recesses on the inner front edge,
so that they do not get pinched when the door is closed. The temperature
of the column oven can be configured in the software.
The column oven is completely connected. No installation work is
required.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3.6 Connecting the eluent bottle
3.6 Connecting the eluent bottle
The eluent is aspirated out of the eluent bottle via the eluent aspiration
tubing . The eluent aspiration tubing is installed on the input for the eluent degasser.
The tubing has to be be fed out of the instrument through a suitable
opening (see "Openings on the back panel", page 11) before the loose
end can be connected to the eluent bottle.
AccessoriesFor this step you need the following accessories:
These parts are part of the accessory kit Vario/Flex ONE (6.5000.010).
■Eluent bottle (6.1608.070)
■The eluent bottle cap GL 45 accessory set (6.1602.160)
This accessory set contains the bottle cap, an M6 tubing nipple, an M8
tubing nipple, two O-rings and an M6 and M8 threaded stopper.
■The tubing adapter for aspiration filter accessory set (6.2744.210)
This accessory set contains a filter holder, a clamping screw and tubing
weighting.
■An aspiration filter (6.2821.090)
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Connecting the eluent aspiration tubing
1
Installing the eluent bottle cap (6.1602.160)
■Start by pushing the M8 tubing nipple onto the loose end of the
eluent aspiration tubing, followed by the O-ring.
■Push the loose end of the eluent aspiration tubing through the
M8 opening of the bottle cap and screw it on for the time being.
Figure 7Installing the eluent bottle cap
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3 Installation
2
Mounting the tubing adapter and the aspiration filter
Install the parts of the tubing adapter for aspiration filter
(6.2744.210) accessory set:
■Start by pushing the tubing weighting onto the loose end of the
eluent aspiration tubing.
■Then push the clamping screw onto the loose end of the eluent
aspiration tubing.
■Lastly, push the filter holder onto the loose end of the eluent aspi-
ration tubing and screw it onto the tubing nipple.
The end of the tubing should extend approximately 1 cm.
Installing the aspiration filter:
NOTE
Only handle the aspiration filter while wearing gloves.
■Place the loose end of the eluent aspiration tubing into the aspira-
tion filter.
The end of the tubing should reach approximately to the center of
the aspiration filter.
■Tighten the aspiration filter to the filter holder.
Figure 8
3
Installing the eluent bottle cap on the eluent bottle
■Insert the eluent aspiration tubing into the eluent bottle
(6.1608.070).
■Tighten the bottle cap on the eluent bottle.
■Adjust the length of the eluent aspiration tubing so that the aspi-
ration filter is at the bottom of the eluent bottle. Then fasten it in
place using the M8 tubing nipple.
■Seal the M6 opening on the bottle cap with the M6 threaded
stopper from the accessory set.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
Installing tubing weighting and aspiration filter
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3.6 Connecting the eluent bottle
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4
Mounting the adsorber tube
NOTE
Depending on the eluent used, the adsorber tube (6.1609.000)
must be filled differently:
■For alkaline eluents or eluents with a low buffer capacity: first a
little cotton, then CO2 adsorber material.
■For all other eluents: only cotton.
■Remove the plastic cover from the large opening of the adsorber
tube. Fill the adsorber tube and close it again using the plastic
cover.
■Insert the adsorber tube into the bottle cap's large opening. Fas-
ten it to the bottle cap using the SGJ clip (6.2023.020).
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3 Installation
3.7 Connecting the eluent degasser
The high-pressure pump cannot generate uniform flow if the eluent contains small gas bubbles or dissolved gas. As a result, the baseline cannot
be stabilized correctly. In order to achieve good measurement results, the
eluent has to be degassed before it goes into the high-pressure pump.
The eluent degasser is completely connected. No installation work is
required.
3.8 Installing the high-pressure pump
The intelligent and low-pulsation high-pressure pump pumps the eluent
through the system. It is equipped with a chip where its technical specifications and "life history" (operating hours, service data, etc.) are saved.
The high-pressure pump consists of:
■The pump head, which pumps the eluent through the system.
■The purge valve used for bleeding the pump head.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3.9 Installing an inline filter
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Figure 9High-pressure pump with purge valve
Pump head
1
The high-pressure pump is completely connected. No installation work is
required.
3.9 Installing an inline filter
Inline filters reliably protect the separation column from potential contamination from the eluent. The small filter plates with 2 µm pore size can be
replaced quickly and easily. They remove particles from the solutions, such
as bacteria and algae.
An inline filter (6.2821.120) is installed between the purge valve and the
pulsation absorber as protection against particles.
Purge valve
2
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3 Installation
Figure 10Inline filter
Input capillary
1
Connected to the purge valve.
Output capillary
2
Connected to the pulsation absorber.
The inline filter is completely connected. No installation work is required.
3.10 Installing the pulsation absorber
The pulsation absorber is installed between the high-pressure pump and
the injection valve. It protects the separation column from damage caused
by pressure fluctuations such as those when switching the injection valve,
and reduces interfering pulsations during highly sensitive measurements.
Figure 11
Connection capillary
1
Connection to inline filter.
Pulsation absorber (6.2620.150)
3
Connection capillary
5
Connection to injection valve.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
Pulsation absorber
2
4
PEEK pressure screws, short
(6.2744.070)
Holder for pulsation absorber
■■■■■■■■
25
3.11 Injection valve
The pulsation absorber is completely connected. No installation work is
required.
3.11 Injection valve
The injection valve connects the eluent path to the sample path. By a
quick and precise switching of the valve a defined quantity of sample solution is injected and flushed to the separation column with the eluent.
The quantity of injected sample solution is determined either by the volume of the sample loop or by an 800 Dosino, if Metrohm's intelligent partial loop injection techniques (MiPT) are being used. For these techniques,
a large sample loop is used, but it is only filled part way.
The choice of sample loop depends on the application. The following
sample loops are normally used:
■■■■■■■■■■■■■■■■■■■■■■
Table 1
Which sample loop do I need?
Cation determination10 µL
Anion determination with suppression20 µL
Anion determination without suppression100 µL
MiPT250 µL
The injection valve is completely connected. No installation work is
required.
Optional: Exchanging the sample loop
The sample loop can be replaced to match the application (see Table 1,
page 26).
NOTE
Only use PEEK pressure screws (6.2744.010) to connect capillaries and
the sample loop to the injection valve.
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26
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
■■■■■■■■■■■■■■■■■■■■■■
3 Installation
Figure 12Exchanging the sample loop
Pressure screw
1
Fastened to Port 6.
Pressure screw
3
Fastened to Port 3.
Sample loop
2
Exchanging the sample loop
1
Removing the existing sample loop
■Unscrew the pressure screws (6.2744.010) at Port 3 and Port 6.
■Remove the sample loop.
2
Installing a new sample loop
■Fasten one end of the sample loop to Port 3 using a PEEK pres-
sure screw (6.2744.010).
■Use the second PEEK pressure screw (6.2744.010) to fasten the
other end of the sample loop to Port 6.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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27
3.12 Suppressor
3.12 Suppressor
The suppressor drive of the 930 Compact IC Flex can hold various rotors.
The large rotors such as the SPM Rotor A (6.2835.000) and the MSM-HC
Rotor A (6.2842.000) can be inserted directly.
Small rotors like the MSM Rotor A (6.2832.000) and the MSM-LC Rotor A
(6.2844.000) must first be fitted into the adapter (6.2842.020) which can
then be inserted into the suppressor housing.
A connecting piece (6.2835.010) is used for all rotors for connecting the
suppressor to the IC system.
■■■■■■■■■■■■■■■■■■■■■■
The instruments are supplied without rotor and without adapter.
The suitable rotor and the adapter, if required, must be ordered separately.
3.12.1 Inserting the rotors
Accessories
For this step you need the following accessories:
■For the suppression: MSM Rotor A (6.2832.000) or MSM-HC Rotor A
Large rotors can be directly inserted into the rotor housing.
NOTE
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28
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3 Installation
CAUTION
The rotor may be destroyed during start-up if not inserted correctly.
Therefore, follow the following instructions exactly.
Inserting large rotors
1
Removing the union nut
Loosen the union nut and remove it.
2
Inserting the rotor
■Clean the sealing surface of the rotor with ethanol using a lint-
free cloth.
■Insert the rotor into the suppressor drive so that the tubing con-
nections on the rear of the rotor fit into the corresponding
recesses inside the suppressor drive and one of the three holes of
the rotor is visible from below in the slot of the suppressor drive.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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29
3.12 Suppressor
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NOTE
The rotor's sealing surface is approximately 4 mm inside the suppressor drive if the rotor is inserted correctly.
If this is not the case, then the rotor has to be moved into the correct position from below using a sharp object (e.g. a screwdriver).
3
Inserting the connecting piece
■Clean the sealing surface of the connecting piece with ethanol
using a lint-free cloth.
■Insert the connecting piece into the suppressor drive so that con-
nector 1 is on top and the three pins of the connecting piece fit
into the corresponding recesses on the suppressor drive.
4
Attaching the union nut
Tighten the union nut on the thread of the suppressor drive by hand
(do not use any tools).
Inserting small rotors
You need the adapter (6.2842.020) in order to insert a small rotor into the
suppressor drive.
1
Inserting the rotor into the adapter
CAUTION
An incorrectly inserted rotor can be destroyed during start-up.
■■■■■■■■
30
■Clean the sealing surface of the rotor with ethanol using a lint-
free cloth.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
■■■■■■■■■■■■■■■■■■■■■■
■Insert the rotor into the adapter so that the tubing connections
on the rear of the rotor fit into the corresponding recesses inside
the adapter and one of the three holes of the rotor is visible in the
slot of the adapter.
2
Inserting the adapter
Insert the adapter into the suppressor drive just like a large rotor (see
"Inserting large rotors", page 29).
3.12.2 Connecting the suppressor
The three inputs and outputs of the suppressor units, numbered with 1, 2
and 3 on the connecting piece, each have 2 fixed mounted PTFE capillaries.
3 Installation
Figure 13
out
1
Output capillary for the eluent.
regenerant
3
Input capillary for the regeneration solution.
waste rins.
5
Output capillary for the rinsing solution; to
the waste container.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
Suppressor – connection capillaries
in
2
Input capillary for the eluent.
waste reg.
4
Output capillary for the regeneration solution; to the waste container.
rinsing solution
6
Input capillary for the rinsing solution.
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31
3.12 Suppressor
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Recommended installation
Alternative installation
Accessories
■■■■■■■■
32
Installing bottles with auxiliary solutions
To connect the bottles of the auxiliary solutions, you will need the following accessories:
■Accessories from the accessory kit: IC Vario/Flex SeS (6.5000.020)
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3.12.2.1 Installing the eluent path
The eluent path is connected with the capillaries
3 Installation
in and out.
Connect the capillary labeled with in with the output of the separa-
1
tion column using a short pressure screw (6.2744.070).
Use a long pressure screw (6.2744.090) to connect the capillary
2
labeled with out to the input of the MCS (see Chapter 3.14.2, page
42).
3.12.2.2 Connecting the regeneration solution
The regeneration solution is connected to the regenerant capillary.
Connecting the regeneration solution to the peristaltic pump
For this step you need the following accessories:
■Accessory kit: Flex/Vario: ChS (6.5000.030)
■Pump tubing (6.1826.420)
■Tubing olive with filter and lock (6.2744.180)
■Tubing olive (6.2744.034)
■Tubing cartridge of the peristaltic pump
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
■■■■■■■■
33
3.12 Suppressor
■■■■■■■■■■■■■■■■■■■■■■
Prepare a tubing cartridge of the peristaltic pump for the regenera-
1
tion solution (see Chapter 3.13.1, page 35).
Fasten the capillary labeled regenerant to the outlet of the pump
2
tubing using a pressure screw (6.2744.070).
Fasten the PTFE capillary from the bottle with the regeneration solu-
3
tion to the inlet of the pump tubing.
3.12.2.3 Connecting the rinsing solution
There are 2 options for rinsing the suppressor:
■Rinsing solution via STREAM (recommended)
Use the eluent from the conductivity detector as a rinsing solution.
■Rinsing solution via peristaltic pump
Prepare the rinsing solution in its own bottle and transport with the
peristaltic pump.
The rinsing solution is connected to the rinsing solution capillary.
Connecting the rinsing solution inlet with STREAM
■■■■■■■■
34
Connect the detector output capillary and the capillary labeled rins-
1
ing solution to each other using a coupling (6.2744.040) and two
pressure screws (6.2744.070).
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
■■■■■■■■■■■■■■■■■■■■■■
3 Installation
Connecting the rinsing solution inlet to the peristaltic pump
For this step you need the following accessories:
■Accessory kit: Flex/Vario: ChS (6.5000.030)
■Pump tubing (6.1826.420)
■Tubing olive with filter and lock (6.2744.180)
■Tubing olive (6.2744.034)
■Tubing cartridge of the peristaltic pump
Prepare a tubing cartridge of the peristaltic pump for the regenera-
1
tion solution (see Chapter 3.13.1, page 35).
Fasten the capillary labeled rinsing solution to the outlet of the pump
2
tubing using a pressure screw (6.2744.070).
Fasten the PTFE capillary from the bottle with the rinsing solution to
3
the inlet of the pump tubing.
3.13 Peristaltic pump
3.13.1 Installing the peristaltic pump
Installing the pump tubing
Pump tubing can differ in terms of material, diameter and thus flow rate.
Different pump tubing is used depending on the application.
Table 2
Order number
6.1826.310Pump tubing LFL (orange/
6.1826.320Pump tubing LFL (orange/
Pump tubing
NameMaterialInner diame-
PVC (Tygon®)0.38 mmPump tubing for bromate deter-
green), 3 stoppers
PVC (Tygon®)0.48 mmFor acceptor solutions for inline
yellow), 3 stoppers
Use
ter
mination using the triiodide
method.
dialysis and for inline ultrafiltration.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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35
3.13 Peristaltic pump
■■■■■■■■■■■■■■■■■■■■■■
Order number
6.1826.330Pump tubing LFL (orange/
6.1826.340Pump tubing LFL (black/
6.1826.360Pump tubing LFL (white/
6.1826.380Pump tubing LFL (gray/
6.1826.390Pump tubing LFL (yellow/
6.1826.420Pump tubing PharMed
6.1826.020Pump tubing (blue/blue), 2
NameMaterialInner diame-
white), 3 stoppers
black), 3 stoppers
white), 3 stoppers
gray), 3 stoppers
yellow), 3 stoppers
(orange/yellow), 3 stoppers
stoppers
Selecting the pump tubing and adapter
Select pump tubing suitable for the application (see Table 2, page
1
35).
Select an adapter suitable for the pump tubing. The adapters are
2
included with the pump tubing connection with safety device and filter (6.2744.180).
Use
ter
PVC (Tygon®)0.64 mmNo special applications.
PVC (Tygon®)0.76 mmFor sample solution in inline dial-
ysis.
PVC (Tygon®)1.02 mmFor sample transfer.
PVC (Tygon®)1.25 mmFor inline sample dilution.
PVC (Tygon®)1.37 mmFor sample solution in inline
ultrafiltration.
®
Ismaprene0.51 mmFor suppressor solutions.
PVC (Tygon
ST)
®
1.65 mmPump tubing for online IC instruments and automation in voltammetry.
■■■■■■■■
36
Table 3Pump tubing and suitable adapters
Pump tubingAdapter
6.1826.310 (orange/green)
6.1826.320 (orange/yellow)
6.1826.330 (orange/white)
6.1826.340 (black/black)
6.1826.360 (white/white)
6.1826.380 (gray/gray)
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
■■■■■■■■■■■■■■■■■■■■■■
3 Installation
Pump tubingAdapter
6.1826.390 (yellow/yellow)
6.1826.420 (orange/yellow)
6.1826.020 (blue/blue)
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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37
3.13 Peristaltic pump
■■■■■■■■■■■■■■■■■■■■■■
Installing the pump tubing
For this step you need the following accessories:
■Tubing cartridge (6.2755.000)
■Pump tubing (6.1826.XXX)
■Coupling Olive/UNF 10/32 (6.2744.034)
■Pump tubing connection with safety device and filter (6.2744.180):
Includes a locknut, 3 adapters and a tubing olive with filter holder.
■2 × pressure screw, short (6.2744.070)
■■■■■■■■
38
1
Connecting the pump tubing
■Attach the Coupling Olive/UNF 10/32 (6.2744.034) to the pump
tubing inlet. Push the end of the pump tubing over at least the
second notch of the olive so that the pump tubing is firmly in
place.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
■■■■■■■■■■■■■■■■■■■■■■
3 Installation
■Install the pump tubing connection with safety device and filter
(6.2744.180) at the pump tubing outlet:
– Push the locknut onto the pump tubing.
– Push the appropriate adapter onto the pump tubing.
– Place the tubing olive with the filter holder into the pump
tubing so that the pump tubing is firmly in place; push the
end of the pump tubing over at least the second notch of
the olive.
– Tighten it using the union nut.
2
Removing the tubing cartridge
■Press in the tubing cartridge's snap-action lever.
■Tilt the tubing cartridge upwards.
■Unhook the tubing cartridge from the mounting bolt.
3
Inserting the pump tubing
■Press the tubing cartridge's contact pressure lever down all the
way.
■Place the pump tubing in the tubing cartridge. Fit the tubing car-
tridge between two stoppers. The stoppers must snap into the
corresponding holder of the tubing cartridge.
4
Inserting the tubing cartridge
■Hang the tubing cartridge in the mounting bolt and press it in the
cartridge holder until you hear the snap-action lever snap in.
Setting the flow rate
The flow rate of the peristaltic pump depends on many factors:
■The inner diameter of the pump tubing
■The rotational speed of the drive
■The contact pressure of the tubing cartridge
NOTE
Pieces of pump tubing are consumables. The lifetime of the pump tubing depends on the contact pressure, among other factors.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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39
3.13 Peristaltic pump
■■■■■■■■■■■■■■■■■■■■■■
Setting the contact pressure correctly
■Fully loosen the contact pressure lever , i.e. press it all the way
1
down.
■Activate the peristaltic pump drive in the software.
■Raise the contact pressure lever one step at a time until liquid
flows.
■When liquid starts flowing, raise the contact pressure lever by an
additional two ratchet increments.
The contact pressure is now set optimally.
3.13.2 Mode of operation for the peristaltic pump
The peristaltic pump is used for pumping sample and auxiliary solutions. It
can rotate in both directions.
The peristaltic pump pumps liquids based on the principle of displacement. The pump tubing is clamped between the rollers (14-5) and the
tubing cartridge (14-2). During operation, the peristaltic pump drive
rotates the roller hub (14-6), so that the rollers (14-5) advance the liquid
in the pump tubing.
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40
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
■■■■■■■■■■■■■■■■■■■■■■
3 Installation
Figure 14Peristaltic pump
Contact pressure lever
1
Cartridge holder
3
Rollers
5
Mounting bolt
7
Tubing cartridges (6.2755.000)
2
Snap-action lever
4
Roller hub
6
3.14 Metrohm CO2 Suppressor (MCS)
3.14.1 General information on MCS
NOTE
The Metrohm CO2 Suppressor (MCS) is used only in conjunction with
conductivity detection with chemical suppression.
The Metrohm CO2 Suppressor (MCS) removes the CO2 from the eluent
stream. This lowers the background conductivity, improves detection sensitivity and minimizes the injection peak and carbonate peak.
CO2 can enter the eluent stream through the sample itself or can develop
due to the suppression reaction in the suppressor. Connecting the MCS
between the suppressor and detector minimizes the CO2 peak in the chromatogram.
The MCS essentially consists of a degassing cell containing a capillary
made from a fluoropolymer membrane. The capillary is permeable to
gases. The degassing cell is connected to the vacuum pump. The eluent is
directed into the degassing cell through the capillary made of a fluoropol-
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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41
3.14 Metrohm CO2 Suppressor (MCS)
ymer membrane. At the same time, the vacuum pump generates a vacuum and draws in the air from the outside. The pressure and concentration difference this creates in the degassing cell relative to inside the capillary causes the CO2 to be diffused out of the eluent stream. The ambient
air is drawn in by a CO2 adsorption cartridge that filters out the CO2.
3.14.2 Connecting the MCS
The MCS is connected between the suppressor and the detector.
Connecting the MCS
■■■■■■■■■■■■■■■■■■■■■■
Figure 15
Air aspiration capillary
1
For drawing in air with low CO2 content (via
the CO2 adsorption cartridge).
Luer coupling (6.2744.120)
3
Mounted on the air aspiration capillary with
a pressure screw (6.2744.070).
1
Removing the threaded stoppers
Remove and keep the two threaded stoppers (6.2744.220) from the
input and output of the MCS.
2
Connection from the suppressor
Use a long pressure screw (6.2744.090) to connect the capillary
labeled out to the input of the of the MCS (labeled In).
Connecting the MCS
2
Pressure screw, short (6.2744.070)
Installed on the air aspiration capillary.
■■■■■■■■
42
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
■■■■■■■■■■■■■■■■■■■■■■
3
Connection to the detector
Connect the detector input capillary with a long pressure screw
(6.2744.090) to the MCS output (labeled Out).
CAUTION
If the MCS is not used, the input and output must be sealed with the
threaded stoppers (6.2744.220).
3.14.3 Installing adsorption cartridges
The suctioned air has to have the lowest CO2 content possible in order for
the CO2 to be removed from the eluent as efficiently as possible. In order
to achieve this, the air is aspirated through a CO2 adsorption cartridge
(6.2837.000).
3 Installation
Accessories
However, the CO2 adsorption cartridge is sensitive to humidity; the CO
2
adsorption cartridge becomes clogged when wet. In order to protect the
CO2 adsorption cartridge, an H2O adsorption cartridge (6.2837.010) is
also installed.
For this step you need the following accessories:
■Adsorption cartridge holder (6.2057.080) with 4 clips, an adapter
(6.1808.190) and a piece of PVC tubing.
■CO
■H
adsorption cartridge (6.2837.000)
2
O adsorption cartridge (6.2837.010)
2
All of the parts are located in one accessory kit: Vario/Flex SeS
(6.5000.020).
Installing the adsorption cartridge
CAUTION
The following preparatory steps absolutely must be carried out for CO
suppression to operate correctly.
2
Preparing the adsorption cartridges:
■Prepare the H
ded leaflet.
■Remove the protective cap on the tip of the CO
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
O adsorption cartridge for use as specified in the provi-
2
adsorption cartridge.
2
■■■■■■■■
43
3.14 Metrohm CO2 Suppressor (MCS)
■■■■■■■■■■■■■■■■■■■■■■
1
Preparing the adsorption cartridge holder
■Push the 4 clips into the slots on the adsorption cartridge holder.
2
Connecting adsorption cartridges
■Attach the PVC tubing to the tip of the H
■Insert the adapter into the other end of the PVC tubing.
■Insert the adapter into the star-shaped cap of the CO
O adsorption cartridge.
2
adsorption
2
cartridge.
■Attach the capillary connected to the MCS's Air in connection to
the tip of the CO2 adsorption cartridge.
3
Inserting the adsorption cartridges into the adsorption cartridge holder
■Clamp the two adsorption cartridges in place using the clips on
the adsorption cartridge holder.
4
Putting the adsorption cartridge holder into the instrument
■Place the adsorption cartridge holder with cartridges into the
instrument's detector chamber.
■■■■■■■■
44
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3.15 Installing the detector
The 930 Compact IC Flex provides enough space for two detectors and
additional accessories in the detector chamber. The detectors are available
as accessories and are supplied with separate manuals.
Placing the detector in the instrument
Follow the instructions in the chapter Inserting the detector in the manual
for the detector.
Connecting the detector to the eluent path
Accessories
For this step you need the following accessories:
■Pressure screw, long (6.2744.090)
3 Installation
Tighten the detector input capillary to the Out output of the MCS
1
using a long pressure screw (6.2744.090).
3.16 Connecting the sample degasser (optional)
Gas bubbles in the sample lead to poor reproducibility, as the quantity of
sample in the sample loop is not always the same. Therefore, we recommend degassing samples that contain gas before injection.
NOTE
The sample degasser does not have to be connected. We recommend
only using the sample degasser if the application requires it.
The rinsing time increases by at least 2 minutes when the sample
degasser is connected.
Accessories
For this step you need the following accessories:
■2 × pressure screw, long (6.2744.090)
■PTFE capillary (6.1803.040)
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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45
3.16 Connecting the sample degasser (optional)
Connecting the sample degasser
■■■■■■■■■■■■■■■■■■■■■■
CAUTION
If the sample degasser is not used, the input and output must be
sealed with threaded stoppers (6.2744.220).
1
Removing the threaded stoppers
Remove and keep the threaded stoppers (6.2744.220) from the input
and output of the sample degasser.
2
Connecting the output capillary
■Push a long pressure screw over the loose end of the capillary
connected to port 1 of the injection valve.
■Tighten the pressure screw at the output of the sample degasser
(labeled Out).
Try to ensure the shortest possible connections.
3
Connecting the input capillary
■Push a long pressure screw over one end of the PTFE capillary
(6.1803.040) and tighten the pressure screw at the input of the
sample degasser (labeled In).
■Guide the other end of the PTFE capillary (6.1803.040) out of the
instrument through a capillary feed-through and connect it to the
Sample Processor, if applicable.
■■■■■■■■
46
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3.17 Connecting the instrument to a computer
NOTE
The instrument must be switched off when being connected to a computer.
AccessoriesFor this step you need the following accessories:
■USB connecting cable (6.2151.020)
■USB connection cable (6.2151.020) from the accessory kit: Vario/Flex
Basic (6.5000.000)
Connecting the USB cable
3 Installation
Insert the USB cable into the computer connection socket on the rear
1
of the instrument.
Insert the other end into a USB port on the computer.
2
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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47
3.18 Connecting the instrument to the power supply
■■■■■■■■■■■■■■■■■■■■■■
3.18 Connecting the instrument to the power supply
WARNING
The power supply unit must not get wet. Protect it from liquids.
The power supply cable is three-core and provided with a plug with
grounding. If another plug has to be mounted, the yellow/green conductor (IEC standard) must be connected to the protective ground (protection
class I).
Accessories
For this step you need the following accessories:
■For Switzerland, …: Power supply cable with IEC 60320 line socket,
type C13, with SEV 1011 plug, type 12 (6.2122.020), 1.5 m
■For Germany, …: Power supply cable with IEC 60320 line socket, type
C13, with CEE 7 plug, type VII (6.2122.040), 1.5 m
■For the USA, …: Power supply cable with IEC 60320 line socket, type
C13, with NEMA 5-15 plug, type 498 (6.2122.070), 1.5 m
Connecting the power supply cable
■■■■■■■■
48
1
Inserting the power supply cable
■Insert the power supply cable into the instrument's power socket.
■Connect the power supply cable to the power supply.
2
Switching on the instrument
Switch on the instrument using the power switch.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
■■■■■■■■■■■■■■■■■■■■■■
After being switched on, the LED on the front of the instrument
flashes. The instrument conducts a system test and establishes a connection to the software. Once the system test is complete and the
connection to the software has been established, the LED lights up
continuously.
3.19 Initial start-up
Even before the guard column and separation column are installed, the
entire system has to be completely rinsed with eluent for the first time.
Rinsing the IC system
The guard column and separation column must not be installed for the
initial start-up.
3 Installation
CAUTION
Make sure that a coupling (6.2744.040) is being used instead of the
columns.
1
Preparing the software
■Start the MagIC Net computer program.
■Open the Equilibration tab in MagIC Net: Work-
place ▶ Run ▶ Equilibration.
■Select (or create) a suitable method.
Also see: MagIC Net tutorial and online help.
2
Preparing the instrument
■Ensure that the eluent aspiration tubing is immersed in the eluent
and there is enough eluent in the eluent bottle.
■STREAM method (recommended): Ensure that the aspiration tub-
ing for the regeneration solution is immersed in the solution and
that there is enough solution; also check that the detector output
capillary is connected to the suppressor's input capillary for rinsing
solution (labeled rinsing solution).
Alternatively, if two bottles are being used for rinsing and regeneration: Ensure that the aspiration tubings for the auxiliary solutions (regeneration solution and rinsing solution) are immersed in
the respective solutions and that there is enough solution in both
bottles.
■Switch on the instrument.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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49
3.19 Initial start-up
■■■■■■■■■■■■■■■■■■■■■■
MagIC Net detects the instrument and all of its modules.
3
Starting equilibration
■Start the equilibration in MagIC Net: Workplace ▶ Run ▶ Equi-
libration ▶ Start HW.
4
Deaerating the high-pressure pump
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50
■Push the end of the purging needle (6.2816.040) over the end of
the deaerating capillary on the purge valve.
■Insert the syringe (6.2816.020) in the Luer connector of the purg-
ing needle.
■Open the purge valve using the rotary knob (approx. ½ turn).
■Switch on the high-pressure pump in MagIC Net.
■Use the syringe to aspirate eluent until there are no more air bub-
bles in the aspirated eluent.
■Switch off the high-pressure pump in MagIC Net.
■Seal the purge valve using the rotary knob.
■Remove the syringe from the purging needle.
■Pull the purging needle out of the deaerating capillary.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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5
Setting the contact pressure of the peristaltic pump
■Set the contact pressure of the peristaltic pump (see "Setting the
contact pressure correctly", page 40).
6
Rinsing the instrument without columns
■Rinse the instrument (without columns) with eluent for 5 minutes.
3.20 Connecting and rinsing the guard column
Guard columns protect the separation column and substantially increase
its service life. Guard columns available from Metrohm are either actual
guard columns or what are known as guard column cartridges that can be
used together with a cartridge holder. The process for installing a guard
column cartridge in the associated holder is described in the leaflet for the
guard column.
NOTE
3 Installation
Metrohm recommends working with guard columns at all times. They
protect the separation column and can be replaced regularly as needed.
NOTE
Information regarding which guard column is suitable for your separation column can be found in the Metrohm IC Column Program
(which is available from your Metrohm representative), the leaflet provided along with your separation column, the product information about
the separation column at http://www.metrohm.com (Ion Chromatography product area), or obtained directly from your representative.
CAUTION
New guard columns are filled with solution and sealed with stoppers or
caps on both sides.
Before inserting the guard column, ensure that this solution can be
mixed with the eluent being used (follow information from the manufacturer).
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3.20 Connecting and rinsing the guard column
NOTE
The guard column may not be connected until after the instrument has
already been put into operation once (see Chapter 3.19, page 49). The
guard column and separation column have to be replaced by a coupling
(6.2744.040) until then.
AccessoriesFor this step you need the following accessories:
■Guard column (suitable for the separation column)
Connecting the guard column
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1
Removing the coupling
Remove the coupling installed between the column input capillary
and the column output capillary for the initial start-up.
2
Preparing the guard column
■Remove the stopper and the sealing cap from the guard column.
3
Connecting the guard column
CAUTION
When inserting the guard column, ensure that it is inserted correctly based on the marked flow direction (if specified).
■Fasten the input of the guard column to the column input capil-
lary using a short pressure screw (6.2744.070).
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3 Installation
■Optional: In case the guard column is connected to the separation
column using a provided a connection capillary, fasten the connection capillary to the guard column's output using the pressure
screw also provided.
Rinsing the guard column
1
Rinsing the guard column
■Place a beaker under the guard column's output.
■Start manual control in MagIC Net and select the high-pressure
pump: Manual ▶ Manual control ▶ Pump
– Flow: in accordance with column leaflet
– On
■Rinse the guard column with eluent for approx. 5 minutes.
■Use manual control in MagIC Net to stop the high-pressure pump
again: Off.
3.21 Connecting the separation column
The intelligent separation column (iColumn) is the heart of the ion chromatographic analysis. It separates different components according to their
interactions with the column. Metrohm separation columns are equipped
with a chip where their technical specifications and history (start-up, operating hours, etc) are stored.
NOTE
Information regarding which separation column is suitable for your
application can be found in the Metrohm IC Column Program, the
product information for your separation column at http://
www.metrohm.com (Ion Chromatography product area) or obtained
directly from your representative.
You can find the separation columns and guard columns currently available from Metrohm in the Metrohm IC Column Program or on the Internet at http://www.metrohm.com in the Ion Chromatography product
area. A test chromatogram and a leaflet are provided along with each column. You can find detailed information on special IC applications in the
corresponding "Application Bulletins" or "Application Notes", which
are available on the Internet at http://www.metrohm.com in the Applications area or free of charge upon request from your responsible Metrohm
representative.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3.21 Connecting the separation column
New separation columns are filled with solution and sealed with stoppers on both sides. Before inserting the column, ensure that this solution can be mixed with the eluent being used (follow information from
the manufacturer).
The separation column may not be connected until after the instrument
has already been put into operation once (see Chapter 3.19, page 49).
The guard column and separation column have to be replaced by a
coupling (6.2744.040) until then.
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CAUTION
NOTE
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3 Installation
Connecting the separation column
1
Removing the stoppers
When inserting the column, ensure that it is inserted correctly
based on the marked flow direction.
■Remove the stoppers from the separation column.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
CAUTION
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55
3.21 Connecting the separation column
2
3
4
5
6
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Installing the input of the separation column
There are 3 possibilities:
■Attaching the bottom end of the separation column directly to
the guard column.
or
■If the guard column is connected to the separation column using
a provided connection capillary, connect the bottom end of the
separation column to the guard column's output capillary using
the provided PEEK pressure screw (6.2744.070).
or
■If no guard column is used (not recommended), connect the col-
umn input capillary to the input of the separation column using a
short pressure screw (6.2744.070).
Rinsing the separation column
■Place a beaker under the separation column's outlet.
■Start manual control in MagIC Net and select the high-pressure
pump: Manual ▶ Manual control ▶ Pump
– Flow: in accordance with column leaflet
– On
■Rinse the separation column with eluent for approximately 10
minutes.
■Use manual control in MagIC Net to stop the high-pressure pump
again: Off.
Removing the coupling
■Remove the coupling (6.2744.040) from the column output capil-
lary.
Installing the output of the separation column
■Fasten the column output capillary to the upper end of the sepa-
ration column using a PEEK pressure screw (6.2744.070).
Inserting the separation column
■Insert the separation column with chip into the column holder
until you hear it snap in place.
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56
The separation column is now detected by MagIC Net.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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3.22 Conditioning
After installation, after each time the instrument is switched on and after
each time the eluent is changed, the system has to be conditioned with
eluent long enough that a stable baseline is attained.
The conditioning time can lengthen considerably after changing the
eluent.
Conditioning the system
1
Preparing the software
3 Installation
NOTE
CAUTION
Ensure that the configured flow is not higher than the flow permitted for the corresponding column (refer to the column leaflet and
the chip data record).
■Start the MagIC Net computer program.
■Open the Equilibration tab in MagIC Net: Work-
place ▶ Run ▶ Equilibration.
■Select (or create) a suitable method.
Also see: MagIC Net tutorial and online help.
2
Preparing the instrument
■Ensure that the column is inserted correctly in relation to the flow
direction marked on the sticker (arrow has to point in the direction of flow).
■Ensure that the eluent aspiration tubing is immersed in the eluent
and there is enough eluent in the eluent bottle.
3
Starting equilibration
■Start the equilibration in MagIC Net: Workplace ▶ Run ▶ Equi-
libration ▶ Start HW.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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57
3.22 Conditioning
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■Visually inspect whether all capillaries and their connections from
the high-pressure pump to the detector are leak-tight. If eluent is
leaking out anywhere, tighten the corresponding pressure screw
further, or loosen the pressure screw, check the end of the capillary and shorten it using the capillary cutter if necessary and
retighten the pressure screw.
4
Conditioning the system
Rinse the system with eluent until the required stability of the baseline is attained (normally 30 minutes).
The instrument is now ready for measuring samples.
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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4 Operation
4 Operation
The 930 Compact IC Flex Oven/SeS/PP/Deg is operated solely using the
MagIC Net software. You can find information on operating the software
in the tutorial for MagIC Net or in the online help.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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5.1 IC system
5 Operation and maintenance
5.1 IC system
5.1.1 Operation
CAUTION
In order to avoid disruptive temperature influences, the entire system
including the eluent bottle must be protected from direct sunlight.
5.1.2 Care
The instrument requires appropriate care. Excess contamination of the
instrument may result in functional disruptions and a reduction in the lifetime of the sturdy mechanical and electronic components.
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The instrument must be cleaned immediately if chemicals or solutions are
spilled on it. In particular, the plug connections (particularly the power
plug) have to be protected from contamination.
CAUTION
The instrument has been designed so that liquid is largely prevented
from being able to get inside the instrument. However, unplug the
power plug immediately if you suspect that corrosive media have gotten inside the instrument. This is the only way to prevent extreme damage to the instrument electronics. Notify Metrohm Service.
WARNING
Untrained personnel may not open the instrument's housing.
5.1.3 Maintenance by Metrohm Service
Maintenance of the instrument is best carried out as part of annual service
performed by specialist personnel from Metrohm. A shorter maintenance
interval is recommended if you are frequently working with caustic and
corrosive chemicals. Metrohm Service offers every form of technical advice
for maintenance and service of all Metrohm instruments.
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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5.1.4 Shutting down and starting back up
If the instrument is not used for a long period, the whole IC system (without separation column) must be rinsed to be free of salts using methanol/
ultrapure water (1:4). This prevents eluent salts from crystallizing and then
causing damage.
Rinsing the IC system to be free of salts
In the software, stop the hardware and wait until the pressure in the
1
high-pressure pump has dissipated.
Remove the guard column and the separation column from the elu-
2
ent path. Connect the connection capillaries directly with each other
using a coupling (6.2744.040).
Rinse the IC system for 15 minutes with methanol/ultrapure water
3
(1:4).
Optional: Only if the IC system is equipped with a ChS plug-in or a
4
SeS plug-in.
5 Operation and maintenance
In the software, switch the suppressor twice during the rinsing process (STEP command).
Optional: Only if the IC system is equipped with a ChS/PP plug-in or a
5
SeS/PP plug-in.
Rinse the two pieces of pump tubing for the peristaltic pump with
water for 5 minutes at level 3. Finish by releasing the peristaltic
pump's contact pressure.
Putting the IC system back into operation
Check that a coupling (6.2744.040) is installed in place of the guard
1
column and the separation column.
Rinse the IC system with eluent for 15 minutes.
2
Remove the coupling and install the guard column and the separa-
3
tion column and(see Chapter 3.21, page 53).
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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61
5.2 Capillary connections
5.2 Capillary connections
All connections between injection valve, separation column and detector
must be as short as possible, have a low dead volume and be completely
leak-tight.
The PEEK capillary downstream of the detector must be free of blockages.
Only use PEEK capillaries with an inner diameter of 0.25 mm in the highpressure section between the high-pressure pump and the detector.
5.3 Servicing the door
CAUTION
The door is made of PMMA (poly(methyl methacrylate)). It must never
be cleaned with abrasive media or solvents.
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CAUTION
Never hold the instrument by the door when lifting it. Only hold the
instrument by the housing.
5.4 Column oven – replacing the capillaries
There are preheating grooves in the inner side wall of the column oven
where the column input capillary has already been inserted and fastened
in place with a holder plate.
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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1
2
2
3
4
5 Operation and maintenance
Figure 16Column oven
Column holder
1
For hanging the separation column (iColumn). With column recognition.
Holder plate
3
For fastening capillaries threaded into the
chamber.
Preheating grooves
2
For threading in capillaries to be temperature-conditioned.
Recesses
4
For routing capillaries into and out of the
column chamber.
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5.5 Handling the eluent
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Replacing the preheating capillaries
In order to make threading the column input capillary into the column
oven's preheating grooves easier, we recommend loosening the screws
for the holder plate a little, but not removing them all the way.
Guide the column input capillary into the column oven via a suitable
1
recess (16-4).
Push the column input capillary into the outermost of the two pre-
2
heating grooves (16-2) from the bottom. Continue pushing it
through under the holder plate until it comes back out the top.
Carefully bend the column input capillary downward and push it
3
through the innermost preheating groove until it comes out at the
bottom edge of the holder plate.
5.5 Handling the eluent
Careful handling of the eluent ensures stable analysis results. Keep the following general measures in mind when handling the eluent:
■The supply bottle with the eluent must be connected as indicated in
chapter 3.6, page 20. This is particularly important for eluents with volatile solvents (such as acetone).
■Avoid condensation in the eluent bottle. Drop formation can change
the concentration ratio in the eluent.
■In the case of very sensitive measurements, we recommend that the
eluent be stirred constantly with a magnetic stirrer (e. g. the
2.801.0010 with 6.2070.000).
■To protect the IC system from foreign particles, we recommend aspi-
rating the eluent via an aspiration filter (see Chapter 3.6, page 20)
(6.2821.090). This aspiration filter has to be replaced as soon as it
turns yellow but at least every 3 months.
5.5.1 Manufacturing eluent
Chemicals used for manufacturing eluents must have a purity grade of at
least "p.a." They may be diluted only by using ultrapure water (resistance
> 18.2 MΩ*cm). (These specifications apply generally for all reagents used
in ion chromatography).
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64
Newly manufactured eluents always have to be microfiltered (0.45 µm filter).
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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The composition of the eluent plays a critical role in chromatographic analysis:
ConcentrationAn increase in the concentration generally leads
pHpH changes lead to shifts in dissociation equili-
Organic solventsAdding organic solvents (such as methanol, ace-
5.5.2 Changing the eluent
Ensure that no precipitates can form when changing the eluent. Immediately successive solutions must be miscible. If the system has to be rinsed
with organic solvents, several solvents with rising or falling lipophilicity
must be used.
5 Operation and maintenance
to shorter retention times and faster separation,
but also to a higher background conductivity signal.
bria and thus to changes in retention times.
tone or acetonitrile) to a watery eluent generally
speeds up lipophilic ions.
NOTE
To change the eluent, remove the separation column and connect the
capillaries using a coupling (6.2744.040) and two pressure screws
(6.2744.070).
5.6 Servicing the eluent degasser
The pieces of connection tubing are connected to the eluent degasser
with clamping screws.
Proceed as follows if you have to loosen and reconnect the connection
tubing at the eluent degasser:
Accessories
For this step you need the following accessories:
You can find these parts in the accessory kit: Vario/Flex Basic (6.5000.000)
■Wrench (6.2621.050)
Loosening the connecting tubing
■Loosen the clamping screws with the wrench.
1
■Unscrew the clamping screws by hand and pull them out of the
connector.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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65
5.7 Notes on operating the high-pressure pump
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Connecting the connecting tubing
■Insert the clamping screws on the connector and screw them in
1
by hand.
■Tighten the clamping screws with the wrench.
5.7 Notes on operating the high-pressure pump
CAUTION
The pump head is filled ex works with methanol/ultrapure water. Ensure
that the eluent used is miscible with this solvent.
Keep the following recommendations in mind in order to protect the
high-pressure pump from damage as much as possible during operation:
■To protect the high-pressure pump from foreign particles, we rec-
ommend filtering the eluent through a filter with a pore size of 0.45
µm and aspirating it via an aspiration filter (6.2821.090).
■Ensure that no precipitates can form when changing the eluent. Salt
crystals between the piston and seal cause abrasive particles that can
find their way into the eluent. These lead to contaminated valves, an
increase in pressure and, in extreme cases, scratched pistons.
Immediately successive solutions must always be miscible. If the system
has to be rinsed with organic solvents, use several solvents with rising
or falling lipophilicity.
■In order to protect the pump seals, ensure that the pump is never
operated dry. Therefore ensure that the eluent supply is correctly connected and that there is enough eluent in the eluent bottle each time
before turning on the pump.
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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5.8 Servicing the high-pressure pump
5 Operation and maintenance
Figure 17High-pressure pump – parts
Pressure screw, short (6.2744.070)
1
Fastened to the outlet valve holder.
Fastening screw
3
Inlet valve holder
5
Eluent aspiration tubing connector
7
Consists of a coupling with a pressure
screw.
Outlet valve holder
2
Pump head
4
Pressure screw, short (6.2744.070)
6
Fastened to the inlet valve holder.
Pressure screw, short (6.2744.070)
8
Fastened to the pump output.
Maintenance intervalThe following parts of the high-pressure pump have to be serviced at least
Maintenance work on the high-pressure pump may not be carried out
unless the instrument is switched off.
Recommended procedure
We recommend the following for the maintenance of the pump head:
1.Service the inlet valve and the outlet valve.
2.Remove the pump head.
3.Service both pistons.
4.Reinstall the pump head.
You can find brief video sequences on the following maintenance steps
on the Internet at http://www.metrohm.com/com/Support/Video/ICGen-
eral.html.
Servicing the outlet valve
Accessories
For this step you need the following accessories:
You can find these parts in the accessory kit: Vario/Flex Basic
(6.5000.000).
■Adjustable wrench (6.2621.000)
Spare partsIf the outlet valve cannot be cleaned, you will need a new outlet valve
(6.2824.160) for this step.
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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Cleaning the outlet valve
1
Removing the outlet valve
5 Operation and maintenance
■Unscrew the connection capillary to the auxiliary piston from the
outlet valve holder (17-2) (1).
■Start by loosening the outlet valve holder with the adjustable
wrench and then unscrew it by hand (2) and remove it.
■Remove the outlet valve from the outlet valve holder (3).
2
Cleaning the outlet valve
■Start by rinsing the outlet valve in the direction of eluent flow
using a wash bottle filled with ultrapure water, RBS™ solution or
acetone. (The direction of eluent flow is marked on the valve by
an arrow.)
The rinsing solution must come out at the valve outlet.
If no more solution comes out, then the valve is blocked.
■Rinse the outlet valve in the direction opposite the eluent flow
using a wash bottle filled with ultrapure water, RBS™ solution or
acetone.
The rinsing solution should only come out at the valve outlet.
■The rinsing effect is further increased through a short treatment in
an ultrasonic bath.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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69
5.8 Servicing the high-pressure pump
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NOTE
The maximum treatment time in an ultrasonic bath is 20 s. Ultrasonic baths that last longer than this can damage the ruby ball
inside the valve.
The outlet valve has to be replaced if it remains clogged after the
ultrasonic bath.
3
Reinserting the outlet valve into the pump head
Accessories
■■■■■■■■
70
■Insert the outlet valve into the outlet valve holder (the seal must
be visible) (1).
■Screw the outlet valve holder up into the pump head (2) and
tighten it in place using the adjustable wrench (3).
■Tighten the connection capillary to the auxiliary piston back onto
the outlet valve holder.
Servicing the inlet valve
For this step you need the following accessories:
You can find these parts in the accessory kit: Vario/Flex Basic
(6.5000.000).
■Adjustable wrench (6.2621.000) from the accessory kit: Vario/Flex
Basic (6.5000.000)
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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5 Operation and maintenance
Spare partsIf the inlet valve cannot be cleaned, you will need a new inlet valve
(6.2824.170) for this step.
Cleaning the inlet valve
1
Removing the inlet valve
■Start by loosening the inlet valve holder with the adjustable
wrench (1) and then unscrew it by hand (2) and remove it.
■Remove the inlet valve from the inlet valve holder (3).
2
Cleaning the inlet valve
■Start by rinsing the inlet valve in the direction of eluent flow using
a wash bottle filled with ultrapure water, RBS™ solution or acetone. (The direction of eluent flow is marked on the valve by an
arrow.)
The rinsing solution must come out at the valve outlet.
If no more solution comes out, then the valve is blocked.
■Rinse the inlet valve in the direction opposite the eluent flow
using a wash bottle filled with ultrapure water, RBS™ solution or
acetone.
The rinsing solution should only come out at the valve outlet.
■The rinsing effect is further increased through a short treatment in
an ultrasonic bath.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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71
5.8 Servicing the high-pressure pump
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NOTE
The maximum treatment time in an ultrasonic bath is 20 s. Ultrasonic baths that last longer than this can damage the ruby ball
inside the valve.
The inlet valve has to be replaced if it remains clogged after the ultrasonic bath.
3
Reinserting the inlet valve into the pump head
Accessories
■■■■■■■■
72
■Insert the inlet valve into the inlet valve holder (the seal must be
visible) (1).
■Screw the inlet valve holder up into the pump head (2) and
tighten it in place using the adjustable wrench (3).
Removing the pump head
For this step you need the following accessories:
You can find these parts in the accessory kit: Vario/Flex Basic
(6.5000.000).
■4 mm hex key (6.2621.030)
Removing the pump head
Prerequisites:
■Is the high-pressure pump switched off?
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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5 Operation and maintenance
■Has the pressure dissipated?
■Is the instrument switched off?
Release the coupling from the pressure screw and seal it with a stop-
1
per.
Unscrew and remove the pressure screw on the pump head's output
2
(17-8).
Unscrew and remove the four fastening screws (17-3) using the hex
3
key.
Remove the pump head (17-4).
4
Replacing the piston seal
Carry out the following work on both pistons in turn.
Servicing a piston consists of the following tasks:
1.Replace the piston seal.
2.Optional: Clean or replace the zirconium oxide piston.
3.Reinstall the piston.
930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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5.8 Servicing the high-pressure pump
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Figure 18High-pressure pump – cross-section
Outlet valve holder
1
Backup ring
3
Pump head
5
Inlet valve holder
7
Piston cartridge
9
Outlet valve (6.2824.160)
2
Piston seal (6.2741.020)
4
Inlet valve (6.2824.170)
6
Zirconium piston (6.2824.070)
8
AccessoriesFor this step you need the following accessories:
You can find these parts in the accessory kit: Vario/Flex Basic
(6.5000.000).
■Adjustable wrench (6.2621.000)
■Tool for piston seals (6.2617.010) consisting of a tip (19-1) for remov-
ing the old piston seal and a sleeve (19-2) for inserting the new piston
seal.
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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2
1
5 Operation and maintenance
Figure 19Tool for piston seal (6.2617.010)
Tip
1
Sleeve
2
Spare partFor this step you need a new piston seal (6.2741.020).
Replacing the piston seal
Piston cartridge
1
Figure 20
1
Removing the piston cartridge
Removing the piston cartridge from the pump head
Backup ring
2
Loosen the piston cartridge (18-9) using the adjustable wrench and
then unscrew it from the pump head by hand. Place it off to the side.
2
Removing the backup ring
Shake the backup ring (18-4) out of the piston opening. Place it off
to the side.
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5.8 Servicing the high-pressure pump
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3
Removing the old piston seal
CAUTION
Screwing the (6.2617.010) special tool for the piston seal into the
piston seal destroys this completely!
CAUTION
Avoid touching the sealing surface in the pump head with the
tool!
Only screw the tip (19-1) of the tool for piston seal far enough into
the piston seal that the seal can be pulled out.
4
Inserting the new piston seal into the tool
Insert the new piston seal into the recess of the sleeve (21-1) of the
tool for piston seal. The sealing spring must be visible from the outside.
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Figure 21Inserting the piston seal into the tool
Tool for piston seal (6.2617.010)
1
Sleeve for inserting the new piston seal.
5
Inserting the new piston seal into the pump head
Guide the sleeve (19-2) of the tool for the piston seal with inserted
piston seal into the pump head. Press the seal into the pump head
recess using the wide end of the tip (19-1) of the tool.
6
Reinserting the piston cartridge
Screw the piston cartridge back into the pump head and tighten, first
by hand, then also by approx. 15° using an adjustable wrench.
Piston seal (6.2741.020)
2
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5 Operation and maintenance
Optional: Cleaning/replacing the zirconium oxide piston
If the baseline still remains unstable after replacing the valves and piston
seal, the zirconium oxide piston in the high-pressure pump may be dirty or
scratched. In that case, the zirconium oxide piston must have to be
cleaned or replaced.
Clean one piston cartridge after the other as follows:
AccessoriesFor this task you need the following accessories:
You can find these parts in the accessory kit: Vario/Flex Basic
(6.5000.000).
■Adjustable wrench (6.2621.000)
Spare partsFor this first step you need a new zirconium oxide piston (6.2824.070).
Optional: Cleaning/replacing the zirconium oxide piston
Prerequisites:
■The pump head has been removed (see "Removing the pump head",
page 72).
■The piston cartridge is removed (see "Replacing the piston seal", page
73).
1
Breaking down the piston cartridge
CAUTION
Inside the piston cartridge there is a taut spring that can launch
out of the piston cartridge if the tension is released suddenly.
When opening the piston cartridge, counteract the pressure from
the spring and carefully unscrew the cartridge.
■Loosen the piston cartridge's screw with an adjustable wrench
and carefully unscrew the screw by hand while counteracting the
pressure from the taut spring.
■Remove the zirconium oxide piston and place it on a paper towel.
■Remove the spring retainer, spring and the inner plastic sleeve
from the piston cartridge and lay them next to the piston.
■Place the backup ring you put aside with the remaining parts.
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5.8 Servicing the high-pressure pump
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Figure 22Components of the piston cartridge
Piston cartridge screw
1
Zirconium oxide piston (6.2824.070)
3
Spring (6.2824.060)
5
Piston cartridge
7
2
3
4
Retaining washer
2
Spring retainer
4
Inner plastic sleeve
6
Protects from metallic abrasion.
Backup ring
8
Cleaning the parts of the piston cartridge
■If the zirconium oxide piston has become contaminated due to
abrasion or deposits, then clean it using a fine abrasive cleaning
powder, rinse it using ultrapure water until it is free of particles
and dry it.
The zirconium oxide piston has to be replaced if it is heavily contaminated or scratched.
■Rinse the other parts of the piston and dry with a lint-free cloth.
Putting the piston cartridge together
■Insert the inner plastic sleeve, the spring and the spring retainer
into the piston cartridge.
■Slide the zirconium oxide piston carefully into the piston cartridge
until its tip emerges from the small opening of the piston cartridge.
■Attach the screw and tighten it by hand.
Reinserting the piston cartridge
Screw the assembled piston cartridge back into the pump head and
tighten, first by hand, then also using an adjustable wrench by
approx. 15°.
Accessories
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Clean the second piston cartridge in the same way.
Mounting the pump head
For this step you need the following accessories:
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5 Operation and maintenance
You can find these parts in the accessory kit: Vario/Flex Basic
(6.5000.000).
■4 mm hex key (6.2621.030)
Mounting the pump head
NOTE
To prevent the pump head from being mounted the wrong way, it has
fastening bolts with different bore hole depths, i.e. one fastening bolt is
longer than all others. The bore hole with the greatest depth must
therefore be assigned to the longest bolt.
■Push the pump head onto the four fastening bolts (1).
1
■Tighten the four fastening screws using the hex key (6.2621.030)
alternating crosswise.
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5.9 Servicing the inline filter
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Connecting the input for the high-pressure pump
■Remove the stopper from the coupling. Tighten the coupling to
1
the pressure screw located on the pump head input capillary (1).
■Reconnect the pump head output capillary to the pump head out-
put (2).
5.9 Servicing the inline filter
NOTE
You can find a video sequence for this task in the Multimedia Guide IC
Maintenance or on the Internet at http://www.metrohm.com/com/
Support/Video/ICGeneral.html?q=14.
Maintenance interval
AccessoriesFor this task you need the following accessories:
The filter has to be replaced at least every 3 months; the filter has to be
replaced more frequently if you are working with high backpressure.
■Adjustable wrench (6.2621.000) from the accessory kit: Vario/Flex
Basic (6.5000.000)
■Tweezers
■A new filter from the packaging (6.2821.130)
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5 Operation and maintenance
Removing the filter
Figure 23Inline filter – removing the filter
Filter housing
1
Inline filter housing. Part of the accessories
(6.2821.120).
Filter (6.2821.130)
3
Packaging contains 10 pieces.
1
Shutting off the flow
Switch off the high-pressure pump in the software.
2
Removing the inline filter
Unscrew the both pressure screws from the inline filter.
3
Unscrewing the filter screw
Use two adjustable wrenches (6.2621.000) to loosen the filter screw
(23-2) from the filter housing (23-1) and unscrew it by hand.
4
Removing the filter
Remove the old filter (23-3) using tweezers.
Filter screw
2
Screw for the inline filter. Part of the accessories (6.2821.120).
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5.9 Servicing the inline filter
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Inserting a new filter
1
Inserting a new filter
■Place the new filter flat in the filter housing (23-1) using tweezers.
2
Mounting the filter screw
■Screw the filter screw (23-2) back into the filter housing (23-1)
and tighten by hand. Then use two adjustable wrenches
(6.2621.000) to tighten it slightly.
3
Remounting the inline filter
■Screw pressure screws back onto the inline filter.
4
Rinsing the inline filter
■Dismantle the guard column (if present) and the separation col-
umn and replace with a coupling (6.2744.040).
■Rinse the instrument with eluent.
■Reinsert the columns after 10 minutes.
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5.10 Servicing the pulsation absorber
CAUTION
The pulsation absorber is maintenance-free and must not be opened.
5.11 Injection valve
Maintenance on the injection valve is best performed by specialist personnel from Metrohm during annual service.
5.12 Suppressor
5.12.1 Notes for operating the suppressor
5 Operation and maintenance
NOTE
The suppressor units must never be regenerated in the same flow direction the eluent is pumped. Therefore, always mount the input and output capillaries according to the diagram outlined in Chapter Connectingthe suppressor, page 31.
The suppressor consists of three suppressor units, which are used in rotation for suppression, regenerated with regeneration solution, and rinsed
with ultrapure water. In order to record every new chromatogram under
comparable conditions, you should normally work with a freshly regenerated suppressor.
CAUTION
The suppressor must never be switched over if liquid is not flowing
through it, since otherwise it may become jammed. If the suppressor is
in a dry state, it must be rinsed for at least five minutes before it may be
switched over.
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5.12 Suppressor
1
2
3
4
5
CAUTION
The suppressor has to be regenerated (see Chapter 5.12.3.2, page
85), cleaned (see Chapter 5.12.3.3, page 86) or replaced (see Chapter 5.12.3.4, page 88) if the capacity of the suppressor is reduced or
if the backpressure is high.
5.12.2 Taking care of the suppressor housing
CAUTION
The transparent suppressor housing can become fogged.
The suppressor housing is made of PMMA (poly(methyl methacrylate)).
It can become scratched and foggy if cleaned improperly. This can
make viewing the rotor difficult or impossible.
■Do not use any scouring agents for cleaning.
■Do not use any solvents for cleaning.
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5.12.3 Servicing the suppressor
5.12.3.1
Figure 24Parts of the suppressor
1
3
5
Parts of the suppressor
Union nut
Rotor
Slot in the housing
Connecting piece (6.2832.010)
2
Housing
4
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5.12.3.2 Regenerating the suppression rotor
If the suppressor units are loaded with certain heavy metals (such as iron)
or organic contamination for long periods, then the standard regeneration
solution may no longer be able to completely remove them. This constantly reduces the capacity of the suppressor units, which results in
reduced phosphate sensitivity in mild cases and a large increase in the
baseline in severe cases.
If such capacity problems occur at one or more positions, all suppressor
units must be regenerated with one of the following solutions:
■Contamination with heavy metals:
1 mol/L H2SO4 + 0.1 mol/L oxalic acid
■Contamination with organic cationic complexing agents:
Pump tubing made of PVC must not be used for solutions containing
organic solvents.
We recommend using the high-pressure pump for regeneration.
Regenerating the suppressor
1
Disconnecting the suppressor from the IC system
■Disconnect the capillaries of the suppressor labeled regenerant
and rinsing solution from the IC system.
2
Regenerating the suppressor
Regenerate the three suppressor units one after the other for approx.
15 minutes using one of the solutions mentioned above.
■Connect the capillary labeled regenerant to the outlet of the
high-pressure pump using a coupling (6.2744.040).
■Set the flow of the high-pressure pump to 0.5 mL/min in the soft-
ware.
■Switch on the high-pressure pump.
If the pressure decreases during regeneration, slowly increase the
flow of the pump to a maximum of 2 mL/min. When doing so,
make sure that the pressure does not exceed 2 MPa!
■After approx. 15 minutes, switch off the high-pressure pump.
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5.12 Suppressor
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■In the software, use the Step command to switch to the next
suppressor unit and regenerate it as described above.
■As soon as all three suppressor units have been regenerated, dis-
connect the capillary labeled regenerant from the coupling.
3
Rinsing the suppressor
After regeneration, each of the three suppressor units must be rinsed
with degassed ultrapure water for about 15 minutes.
■Connect the capillary labeled rinsing solution to the outlet of
the high-pressure pump using a coupling (6.2744.040).
■Set the flow of the high-pressure pump to 0.5 mL/min in the soft-
ware.
■Switch on the high-pressure pump.
If the pressure decreases during rinsing, slowly increase the flow
of the pump to a maximum of 2 mL/min. When doing so, make
sure that the pressure does not exceed 2 MPa!
■After approx. 15 minutes, switch off the high-pressure pump.
■In the software, use the Step command to switch to the next
suppressor unit and rinse it as described above.
■As soon as all three suppressor units have been rinsed, disconnect
the capillary labeled rinsing solution from the coupling.
4
Connecting the suppressor to the IC system
■Reconnect the capillaries of the suppressor labeled regenerant
and rinsing solution to the IC system.
■Reconnect the outlet of the high-pressure pump to the IC system.
5.12.3.3 Cleaning the suppressor
In the following cases, it may be necessary to clean the suppressor:
■Increased backpressure at the suppressor's connection tubing.
■Blockage of the suppressor which cannot be eliminated (solutions can
no longer be pumped through the suppressor).
■Jamming of the suppressor which cannot be eliminated (suppressor
can no longer be switched over).
Cleaning the suppressor
1
Disconnecting the suppressor from the IC system
■Switch off the instrument.
■Disconnect all capillaries of the suppressor from the IC system.
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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5 Operation and maintenance
2
Dismantling the suppressor
■Unscrew union nut (24-1) from the housing (24-4).
■Pull the connecting piece (24-2) out of the housing together with
the the rotor (24-3).
If rotor A gets stuck in the housing, you can knock it loose as follows:
Put a pointed object into the slot in the housing and use it to
knock rotor A loose.
■Detach the connecting piece from the rotor.
3
Rinsing the capillaries
■Connect each of the 6 PTFE capillaries fastened to the connecting
piece (24-2) to the high-pressure pump in order and pump ultrapure water through them.
■Check whether water comes out at the connecting piece.
If one of the capillaries remains blocked, the connecting piece (see
"Replacing parts of the suppressor", page 89) has to be replaced
(order number 6.2835.010).
4
Cleaning the rotor
■Clean the surface of the rotor (24-3) with ethanol using a lint-free
cloth.
5
Inserting the rotor
CAUTION
Rotor A may be destroyed during start-up if not inserted correctly.
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5.12 Suppressor
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■Insert the rotor (24-3) into the housing (24-4) in such a way that
the tubing connections on the rear of rotor fit into the corresponding recesses inside the housing and one of the three holes
of the rotor is visible from below in the slot of the housing (24-5).
■The rotor's sealing surface is approximately 4 mm inside the hous-
ing if the rotor is inserted correctly. If this is not the case, the
rotor must be moved into the right position from below using a
sharp object.
6
Cleaning the connecting piece
■Clean the sealing surface of the connecting piece (24-2) with
ethanol using a lint-free cloth.
7
Inserting the connecting piece
■Insert the connecting piece (24-2) into the housing in such a way
that the connector 1 is on top and the three pins of the connecting piece fit into the corresponding recesses on the housing.
■Reattach the union nut (24-1) onto the housing and tighten by
hand (do not use a tool).
8
Connecting and conditioning the suppressor
■Reconnect the suppressor to the IC system.
■Before switching the suppressor over for the first time, rinse each
of the three suppressor units with solution for 5 minutes.
5.12.3.4 Replacing parts of the suppressor
In the following cases, it might be necessary to replace parts of the suppressor:
■Loss of suppressor capacity which cannot be eliminated (reduced phos-
phate sensitivity and/or significant rise in the baseline).
■Blockage of the suppressor which cannot be eliminated (solutions can
no longer be pumped through the suppressor).
Both the rotor and the connecting piece can be replaced.
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5 Operation and maintenance
Replacing parts of the suppressor
1
Disconnecting the suppressor from the IC system
■Switch off the instrument.
■Disconnect all capillaries of the suppressor from the IC system.
2
Dismantling the suppressor
■Unscrew union nut (24-1) from the housing (24-4).
■Pull the connecting piece (24-2) out of the housing together with
the the rotor (24-3).
If rotor A gets stuck in the housing, you can knock it loose as follows:
Put a pointed object into the slot in the housing and use it to
knock rotor A loose.
■Detach the connecting piece from the rotor.
3
Cleaning the new rotor
■Clean the surface of the new rotor (24-3) with ethanol using a
lint-free cloth.
4
Inserting the new rotor
CAUTION
Rotor A may be destroyed during start-up if not inserted correctly.
Insert the new rotor (24-3) into the housing (24-4) in such a way
■
that the tubing connections on the rear of rotor fit into the corresponding recesses inside the housing and one of the three holes
of the rotor is visible from below in the slot of the housing (24-5).
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5.12 Suppressor
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■The rotor's sealing surface is approximately 4 mm inside the hous-
ing if the rotor is inserted correctly. If this is not the case, the
rotor must be moved into the right position from below using a
sharp object.
5
Cleaning the new connecting piece
■Clean the surface of the new connecting piece (24-2) with etha-
nol using a lint-free cloth.
6
Inserting the new connecting piece
■Insert the connecting piece (24-2) into the housing (24-4) in such
a way that the connector 1 is on top and the three pins of the
connecting piece fit into the corresponding recesses on the housing.
■Reattach the union nut (24-1) and tighten it by hand.
7
Connecting and conditioning the suppressor
■Reconnect all capillaries of the suppressor to the IC system.
■Before switching the suppressor over for the first time, rinse the
three suppressor units with solution for 5 minutes.
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930 Compact IC Flex Oven/SeS/PP/Deg (2.930.2560)
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