850 Professional IC: Anion - 2.850.2010
850 Professional IC: Anion - 2.850.2010
Anion – 2.850.2010
Manual
8.850.8045EN / 2019-10-10
Metrohm AG
CH-9100 Herisau
Switzerland
Phone +41 71 353 85 85
Fax +41 71 353 89 01
[email protected]
www.metrohm.com
850 Professional IC
Anion – 2.850.2010
Manual
8.850.8045EN / 2019-10-10
Technical Communication
Metrohm AG
CH-9100 Herisau
[email protected]
Table of contents
1 Introduction 1
1.1 Instrument description ......................................................... 1
1.2 Intended use ......................................................................... 4
1.3 About the documentation ................................................... 4
1.3.1 Symbols and conventions ........................................................ 5
1.4 Safety instructions ................................................................ 6
1.4.1 General notes on safety ........................................................... 6
1.4.2 Electrical safety ........................................................................ 6
1.4.3 Tubing and capillary connections ............................................. 7
1.4.4 Flammable solvents and chemicals ........................................... 7
1.4.5 Recycling and disposal ............................................................. 7
2 Installation 9
2.1 About this chapter ................................................................ 9
2.2 Initial installation .................................................................. 9
2.3 Flow diagram ...................................................................... 10
2.4 Setting up the instrument .................................................. 12
2.4.1 Packaging .............................................................................. 12
2.4.2 Checks .................................................................................. 12
2.4.3 Location ................................................................................ 12
2.5 Capillary connections in the IC system ............................. 13
2.6 Rear of the instrument ....................................................... 15
2.6.1 Rollers and handle ................................................................. 15
2.6.2 Positioning and connecting the detector ................................ 18
2.6.3 Transport locking screws ........................................................ 18
2.6.4 Leak sensor ........................................................................... 18
2.6.5 Drainage tubings ................................................................... 19
2.7 Capillary and cable feed-throughs .................................... 21
2.8 Eluent ................................................................................... 24
2.8.1 Connecting the eluent bottle ................................................. 24
2.9 Eluent degasser .................................................................. 28
2.10 High pressure pump ........................................................... 30
2.10.1 Capillary connections high pressure pump/purge valve ........... 30
2.10.2 Deaerating the high pressure pump ....................................... 32
2.11 Inline filter ........................................................................... 34
2.12 Pulsation absorber ............................................................. 35
2.13 Sample degasser ................................................................. 36
3 Start-up 59
3.1 Initial start-up ..................................................................... 59
3.2 Conditioning ........................................................................ 60
5 Troubleshooting 91
5.1 Problems and their solutions ............................................. 91
6 Technical specifications 96
6.1 Reference conditions .......................................................... 96
6.2 Device .................................................................................. 96
6.3 Leak sensor ......................................................................... 96
6.4 Ambient conditions ............................................................ 96
6.5 Housing ............................................................................... 97
6.6 Eluent degasser .................................................................. 97
6.7 High pressure pump ........................................................... 97
6.8 Sample degasser ................................................................. 98
6.9 Injection valve ..................................................................... 98
6.10 Column thermostat ............................................................ 99
6.11 Metrohm Suppressor Module (MSM) ............................... 99
6.12 Peristaltic pump .................................................................. 99
6.13 Detector ............................................................................ 100
6.14 Power connection ............................................................. 100
6.15 Interfaces .......................................................................... 100
6.16 Weight ............................................................................... 101
7 Accessories 102
Index 103
Table of figures
Figure 1 Front view of the instrument ............................................................. 2
Figure 2 Flow diagram with chemical suppression ......................................... 11
Figure 3 Connection of capillaries with pressure screws ................................ 13
Figure 4 Rollers and handle ........................................................................... 16
Figure 5 Handle as MPak holder .................................................................... 17
Figure 6 Connection of the leak sensor on the rear of the instrument ............ 19
Figure 7 Drainage tubings ............................................................................. 20
Figure 8 Capillary feed-throughs on the door ................................................ 22
Figure 9 Capillary feed-throughs base tray/flask holder .................................. 23
Figure 10 Installing the eluent bottle cap ........................................................ 25
Figure 11 Mounting the aspiration filter .......................................................... 25
Figure 12 Installing the tubing weighting and aspiration filter .......................... 26
Figure 13 Eluent aspiration tubing fully equipped ............................................ 26
Figure 14 Eluent bottle – connected ............................................................... 27
Figure 15 Eluent degasser ............................................................................... 29
Figure 16 Capillary connections high pressure pump/purge valve ..................... 30
Figure 17 High pressure pump – Connect inlet ................................................ 31
Figure 18 Deaerate the high pressure pump .................................................... 33
Figure 19 Connecting the inline filter .............................................................. 35
Figure 20 Pulsation absorber – Connection ..................................................... 36
Figure 21 Sample degasser ............................................................................. 37
Figure 22 Injection valve – connected ............................................................. 38
Figure 23 Injection valve – Positions ................................................................ 39
Figure 24 Column thermostat ......................................................................... 41
Figure 25 MSM – connections ........................................................................ 44
Figure 26 Peristaltic pump ............................................................................... 46
Figure 27 Installing the pump tubing .............................................................. 47
Figure 28 Install pump tubing connection with filter ....................................... 48
Figure 29 Install pump tubing connection without filter .................................. 49
Figure 30 Front of conductivity detector ......................................................... 51
Figure 31 Rear of conductivity detector ........................................................... 52
Figure 32 Connection detector–MSM ............................................................. 53
Figure 33 Pump head – removing the piston ................................................... 67
Figure 34 Components of the piston cartridge ................................................ 68
Figure 35 Tool for piston seal .......................................................................... 69
Figure 36 Removing the piston seal ................................................................. 70
Figure 37 Inserting the piston seal into the tool ............................................... 70
Figure 38 Inserting the piston seal into the pump head ................................... 71
Figure 39 Removing valves .............................................................................. 72
Figure 40 Dismantling valve ............................................................................ 73
Figure 41 Components of the inlet valve and outlet valve ................................ 74
Figure 42 Change filters (of the inline filter) ..................................................... 76
Figure 43 MSM – Components ....................................................................... 83
Figure 44 Pump tubing connection – Changing the filter ................................. 88
1 Introduction
3
4
5
8 9 10 11
Figure 1 Front view of the instrument
11 Column thermostat
See Chapter 2.15.
Eluent degasser
The eluent degasser removes gas bubbles and dissolved gases from the
eluent. For degassing, the eluent flows into a vacuum chamber through a
special fluoropolymer capillary.
Inline filter
Inline filters protect the separation column securely against possible con-
tamination from the eluent. Inline filters can however also just as well be
used for the purpose of protecting other sensitive components against
contaminations in the solutions used. The filter platelets with a pore size
of 2 µm can be replaced quickly and easily. They remove particles like e. g.
bacteria and algae from the solutions.
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.
Sample degasser
The sample degasser removes gas bubbles and dissolved gases from the
sample. For degassing, the sample flows into a vacuum chamber through
a special fluoropolymer capillary.
Injection valve
The injection valve connects the eluent and sample path through rapid
and precise valve switchover. A precisely measured amount of sample
solution is injected and rinsed with eluent onto the separation column.
Column thermostat
The column thermostat controls the temperature of the column and elu-
ent channel and thus ensures stable measuring conditions. It provides
space for 2 separation columns.
Peristaltic pump
The Peristaltic pump is used for pumping sample and auxiliary solutions. It
can rotate in both directions.
Conductivity detector
The conductivity detector continuously measures the conductivity of the
liquid passing through and outputs these signals in digital form (DSP –
Digital Signal Processing). The conductivity detector exhibits outstanding
thermal stability and thus guarantees reproducible measuring conditions.
Separation column
The intelligent separation column is the heart of the ion chromatographic
analysis. It separates the different components corresponding to their
interactions with the column. Metrohm separation columns are equipped
with a chip on which their technical specifications and their history (first
use / setting up, operating hours, injections, …) are saved.
CAUTION
WARNING
WARNING
WARNING
Supply voltage
WARNING
WARNING
CAUTION
Leaks in tubing and capillary connections are a safety risk. Tighten all
connections well by hand. Avoid applying excessive force to tubing con-
nections. Damaged tubing ends lead to leakage. Appropriate tools can
be used to loosen connections.
Check the connections regularly for leakage. If the instrument is used
mainly in unattended operation, then weekly inspections are manda-
tory.
WARNING
More details about the disposal of your old instrument can be obtained
from your local authorities, from waste disposal companies or from your
local dealer.
2 Installation
NOTICE
3 Place the detectors in the instrument and connect them (see chapter
2.6.2, page 18).
9 Installing the MSM (see chapter 2.16, page 43) – with associated
peristaltic pump (see chapter 2.17, page 46).
11 Mains connection .
14 Install the guard column (if used) (see chapter 2.21, page 55).
Eluent 11
Sample
Sample optional
Rinsing solution
Regeneration solution 10
9
15 8
16 17
18 19
2 12 13
1 14
3
5
4
6
9 MSM 10 Detector
See Chapter 2.16. See Chapter 2.18.
2.4.2 Checks
Immediately after receipt, check whether the shipment has arrived com-
plete and without damage by comparing it with the delivery note.
2.4.3 Location
The instrument has been developed for operation indoors and may not be
used in explosive environments.
Place the instrument in a location of the laboratory which is suitable for
operation and free of vibrations and which provides protection against
corrosive atmosphere and contamination by chemicals.
Pressure screws
4
1 2 3
Figure 3 Connection of capillaries with pressure screws
NOTICE
NOTICE
Connection capillaries
PEEK capillaries and PTFE capillaries are used in the IC system.
PEEK capillaries (poly- PEEK capillaries are temperature-resistant up to 100°C, stable under pres-
etheretherketone) sure up to 400 bar, flexible, chemically inert and exhibit an extremely
smooth surface. They can be readily cut down to the desired length with
the 6.2621.080 capillary cutter.
Usage:
■ PEEK capillaries (6.1831.010) with an internal diameter of 0.25 mm for
the entire high-pressure section.
■ PEEK capillaries (6.1831.030) with an internal diameter of 0.75 mm for
sample handling in the ultratrace range.
CAUTION
For the capillary connections between the injection valve and detector ,
PEEK capillaries with an internal diameter of 0.25 mm must be used.
These are already connected to a newly delivered instrument.
PTFE capillaries (poly- PTFE capillaries are transparent and enable visual tracing of the liquids to
tetrafluoroethylene) be pumped. They are chemically inert, flexible and temperature-resistant
up to 80°C.
Usage:
PTFE capillaries (6.1803.0x0) are used for the low-pressure section.
■ PTFE capillaries with internal diameter of 0.5 mm for sample handling.
■ PTFE capillaries with internal diameter of 0.97 mm for sample handling
as well as for rinsing solutions (they do not have to be in the scope of
delivery of the instrument).
Capillary connections
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 reasons for this:
■ The capillaries do not have exactly cut 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 plane. Therefore we recommend only to cut
PEEK capillaries with the capillary cutter (6.2621.080).
1 Slide the pressure screw over the capillary. Ensure that the capillary
protrudes 1–2 mm from the tip of the pressure screw.
2 Plug the capillary all the way into the connection or coupling until
the stop.
3 Only then start turning the pressure screw, while keeping the capil-
lary pressed in space.
4
Figure 4 Rollers and handle
5 Roller holder
Removing handle
Removing rollers
NOTICE
When extended, the handle (5-2) can also be used for hanging up
MPaks (eluent bags).
1 Move handle (5-2) upwards and screw in the knurled screws (5-1)
again.
WARNING
1 Plug the leak sensor connector plug (6-2) into the leak sensor con-
nection socket (6-1) on the rear of the instrument (see figure 6, page
19).
1 2 3
2
3
4
8 9
Figure 7 Drainage tubings
1 Plug drainage tubing (7-2) into the drainage tubing connector (7-1)
of the flask holder and shorten to required length.
2 Plug drainage tubing (7-4) into the drainage tubing connector (7-3)
of the detector chamber and shorten to required length.
3 Connect drainage tubing (7-2) from the flask holder and drainage
tubing (7-4) from the detector chamber to the Y connector (7-5).
5 Plug drainage tubing (7-7) into the drainage tubing connector (7-8)
of the base tray and guide the other end into a waste container.
1 3
2
1
2
Do not feed capillaries through the Luer connectors (8-1). The capillaries
are fastened with PEEK pressure screws (8-3) from inside to the Luer con-
nector. From outside, liquid can be aspirated or injected with a syringe.
5 6 7 8 8 7 6 5
Rear Front
1 2
3 4
9 10 11 12 12 11 10 9
Figure 9 Capillary feed-throughs base tray/flask holder
2.8 Eluent
2.8.1 Connecting the eluent bottle
The eluent is aspirated out of the eluent bottle via the eluent aspiration
tubing (10-1).
The eluent aspiration tubing is connected to the eluent degasser (see
chapter 2.9, page 28). The tubing must be threaded through a suitable
capillary feed-through (see chapter 2.7, page 21) of the instrument before
the other end can be equipped.
The following accessories are needed for equipping the eluent aspiration
tubing:
■ 6.1602.160 eluent bottle cap GL 45
■ 6.2744.210 tubing adapter for aspiration filter
■ 6.2821.090 aspiration filter
Proceed as follows for equipping the eluent aspiration tubing:
1 Guide the free end of the eluent aspiration tubing (10-1) out of the
instrument through a suitable capillary feed-through.
1 2 3 4
■ Slide the tubing weighting (12-3) onto the eluent aspiration tub-
ing (12-1).
■ Slide the clamping screw (12-4) onto the eluent aspiration tubing
(12-1).
■ Insert eluent aspiration tubing (12-1) into the aspiration filter
(12-5). The end of the tubing should reach approximately to the
center of the aspiration filter.
■ Screw the clamping screw (12-4) to the filter holder (11-1).
■ Tighten the fully equipped bottle cap to the eluent bottle (14-10).
The aspiration filter (14-6) must rest on the base of the eluent
bottle.
■ Close the remaining small opening on the bottle cap with a
threaded stopper (14-14) from the accessory set.
NOTICE
■ First, place a piece of cotton (14-3), then the CO2 adsorber (14-4)
in the large opening of the adsorber tube (14-2) and close with
the plastic cover.
■ Fasten the adsorber tube (14-2) on the bottle cap (14-11) using
the SGJ clip (14-12).
14 1
2
13
3
12
4 11
10
9 8 7 6
Figure 14 Eluent bottle – connected
NOTICE
1
5
3 4
2
6
Figure 15 Eluent degasser
1 CAUTION
■ Insert the eluent aspiration tubing (15-5) into the eluent degasser
input (15-1).
■ Carefully tighten the clamping screw (15-4).
2 ■ Insert connection tubing (15-6) (the end with the longer clamping
screw (15-4)) into the eluent degasser output (15-2).
■ Carefully tighten the clamping screw (15-4).
■ Connect the other end of the connection capillary (15-6) (with
the shorter clamping screw ) to the high-pressure pump (16-9)
(see "Connecting inlet to the high pressure pump", page 31).
NOTICE
All of the capillary connections of the high pressure pump and the
purge valve are already installed in the newly delivered instrument.
2 13
1
2
3
4
12
5
2
6 2
11
2
8 9 10 2 2
Figure 16 Capillary connections high pressure pump/purge valve
13 Connection capillary
Connects the output of the pump head with
the purge valve.
NOTICE
1 2 3 4
Figure 17 High pressure pump – Connect inlet
5 Backup ring
1 Connecting coupling
Fasten the coupling (17-2) with a pressure screw (17-1) on the pump
head inlet capillary (16-7).
CAUTION
■ Plug the eluent aspiration tubing (17-4) into the coupling (17-2).
■ Tighten the clamping screw (17-3).
CAUTION
The high pressure pump must not be deaerated before the initial start-
up (see chapter 3.1, page 59).
Deaerate the high pressure pump as follows (see figure 18, page 33):
5
4 5
6
3 7
2
1 5
5 Aspirating eluent
■ Aspirate with the syringe (18-1) until bubble-free eluent flows into
the syringe.
6 Completing deaerating
■ Switch off high pressure pump.
■ Close rotary knob (18-7).
■ Remove syringe (18-1) from the Luer connector (18-2).
■ Pull the purging needle (18-3) out of the deaerating capillary
(18-4).
NOTICE
CAUTION
Observe the flow direction marked on the filter housing for the connec-
tion of the inline filter.
1 2 3 2 4
Figure 19 Connecting the inline filter
NOTICE
CAUTION
2 3
3
2
4
NOTICE
3 4
1 Remove and keep the threaded stoppers (6.2744.220) from the inlet
and outlet of the sample degasser.
4 Guide the other end of the connection capillary out of the instrument
through a capillary feed-through and connect it with the Sample Pro-
cessor, if applicable.
CAUTION
If the sample degasser is not used, the input and output must be
sealed with the threaded stoppers (6.2744.220).
NOTICE
The capillaries of the eluent path and the sample path and the sample
loop are already installed in the newly delivered instrument.
6 5
7 7
2 1
3 6 2
4 5
7
1
7
3 4
Figure 22 Injection valve – connected
NOTICE
4 3 4 3
2 1 2 1
3 6 3 6
A B
5
4 5 4 5
1 2 1 2
Figure 23 Injection valve – Positions
5 Sample loop
Cation determination 10 µL
Anion determination with suppression 20 µL
Anion determination without suppression 100 µL
3 1
2 2
1
Figure 24 Column thermostat
3 Column holder
For fastening the columns.
With column recognition.
NOTICE
The column input capillary is already threaded into the capillary recesses
of the column thermostat at the time the instrument is first delivered.
The following installation instructions need not be carried out at the
time of initial installation.
Threading capillaries
2 Slide the column input capillary from below into the outer of the two
capillary recesses (24-2). Slide it through under the holder plate until
it emerges again at the top.
3 Carefully bend the column input capillary downward and slide from
from above to below through the inner capillary recess until it
emerges at the lower edge of the holder plate.
4
NOTICE
CAUTION
The three inputs and outputs of the suppressor units numbered 1..3 on
the MSM each have 2 fixed mounted PTFE capillaries (see figure 25, page
44).
8 4
1
2 2
3
7 5
6
Figure 25 MSM – connections
The PTFE capillaries firmly mounted on the MSM are connected to the
other components of the IC system as follows:
CAUTION
As the PTFE capillaries are very soft, the pressure screws should not be
overtightened.
Flattened capillaries must be shortened with the help of a 6.2621.080
capillary cutter.
The rinsing and regeneration solutions are pumped with a peristaltic pump
(see chapter 2.17, page 46).
1 4
3
2
7
7 Snap-action lever
6.2744.180
6.2744.160
9 10 3 6 7 8
Figure 27 Installing the pump tubing
NOTICE
1 2 3
3 Tubing olive
6.1826.310 (orange/green)
6.1826.320 (orange/yellow)
6.1826.330 (orange/white)
6.1826.360 (white/white)
6.1826.380 (gray/gray)
6.1826.390 (yellow/yellow)
1 ■ Fully loosen the contact pressure lever (27-5), i.e. press it all the
way down.
■ Switch on the peristaltic pump.
■ 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 2 ratchet increments.
The contact pressure is now set optimally.
The delivery rate depends not only on the correct contact pressure
but also on the interior diameter of the pump tubing and the rota-
tional speed of the drive.
NOTICE
Pump tubings are consumable material. The service life of the pump
tubings depends on the contact pressure amongst other factors.
1
3
3 Type plate
With serial number.
NOTICE
1 3 2
4
Figure 32 Connection detector–MSM
NOTICE
1 Insert the USB cable into the computer connection socket on the rear
of the instrument labeled PC.
WARNING
NOTICE
NOTICE
CAUTION
New guard columns are filled with solution and are sealed on both
sides with stoppers or caps, respectively. Before using the guard col-
umn, you need to ensure that this solution is miscible with the eluents
used (observe manufacturer's data).
NOTICE
The guard column may only be installed after the initial start-up (see
chapter 3.1, page 59) of the instrument. Until then, use the coupling
(6.2744.040) instead of the guard and separation column.
NOTICE
CAUTION
NOTICE
CAUTION
New separation columns are filled with solution and are sealed on both
sides with stoppers. Before using the column, you need to ensure that
this solution is miscible with the eluents used (observe manufacturer's
data).
You can find the separation columns and guard columns currently avail-
able from Metrohm in the Metrohm IC Column Program, or in the Internet
at http://www.metrohm.com in the product area Ion Chromatography. A
test chromatogram and an leaflet are provided along with each column.
You can request detailed information on special IC applications in the cor-
responding "Application Bulletins" or "Application Notes", available
in the Internet at http://www.metrohm.com in the Applications area or via
the Metrohm agent responsible free of charge.
NOTICE
The separation column may only be installed after the initial start-up
(see chapter 3.1, page 59) of the instrument. Until then, use the cou-
pling (6.2744.040) instead of the guard and separation column.
CAUTION
When inserting the columns, always ensure that these are correctly
inserted corresponding to the flow direction indicated.
NOTICE
The iColumns are equipped with a chip on which their operating data is
saved. The chip has to be hooked into the chip holder provided for this
so that the column recognition can function.
3 Start-up
The chapter Start-up is divided into 2 sections:
Initial start-up The initial start-up is carried out during the ini-
tial installation.
Conditioning Conditioning is carried out as a final installation
step and each time after the system is started.
CAUTION
The separation column and guard column may not be installed for the
initial start-up.
Make sure that the coupling (6.2744.040) is being used instead of the
columns.
3 Starting equilibration
■ In MagIC Net™, start the equilibration.
NOTICE
■ If peristaltic pumps are used, set the contact pressure (see "Set
flow rate", page 50).
The instrument is now ready for the installation of the columns (see chap-
ter 2.21, page 55).
3.2 Conditioning
After the installation and after switching on the instrument, the system
must be conditioned with eluent until a stable baseline is reached.
NOTICE
After a change of eluent (see chapter 4.4.2.3, page 65), the condi-
tioning time can lengthen considerably.
CAUTION
Ensure that the flow set is not higher than the flow permissible for
the corresponding column (see column leaflet and chip data set).
3 Checking leak-tightness
■ In MagIC Net™, start the equilibration.
■ Check all capillaries and their connections from the high pressure
pump to the detector for signs of liquid escaping.
If eluent escapes anywhere, tighten the corresponding pressure
screw or loosen the connection, check the end of the capillary,
shorten it with a capillary cutter if necessary, and restore the con-
nection.
WARNING
CAUTION
On the rear of the instrument, the drainage tubings must be mounted and
the leak sensor must be plugged in and activated as protection against
escaping liquids.
Spillages of chemicals and solvents should be cleaned up immediately. In
particular, the plug connections on the rear panel of the instrument (espe-
cially the mains plug) should be protected from contamination.
4.1.3 Operation
CAUTION
1 Remove the separation column from the eluent path. Connect the
connection capillaries directly with each other using a coupling
(6.2744.040).
Rinse with eluent for at least 15 minutes at starting up again and before
connecting the guard column and separation column.
4.3 Door
CAUTION
CAUTION
4.4 Eluent
4.4.1 Production
Chemicals used for manufacturing eluents must have a purity grade of at
least "p.a.". Only ultrapure water (resistance > 18.2 MΩ*cm) may be used
for dilution (this generally applies for reagents which are used in ion chro-
matography).
Newly manufactured eluents always have to be microfiltered (0.45 µm fil-
ter).
The composition of the eluent plays a critical role in chromatographic ana-
lysis:
Concentration An increase in the concentration generally leads
to shorter retention times and faster separation,
but also to a higher background conductivity sig-
nal.
pH pH changes lead to shifts in dissociation equili-
bria and thus to changes in retention times.
Organic solvents Adding an organic solvent (e.g. methanol, ace-
tone or acetonitrile) to watery eluents generally
speeds up lipophilic ions.
4.4.2 Operation
4.4.2.1 Supply bottle
The supply bottle with the eluent must be connected as indicated in chap-
ter 2.8.1, page 24. This is particularly important for eluents with volatile
solvents (e.g. acetone).
Condensation in the eluent bottle must be avoided. Drop formation can
change the concentration ratio in the eluent.
In the case of very sensitive measurements, we recommend that the elu-
ent be stirred constantly with a magnetic stirrer (e. g. the 2.801.0010 with
6.2070.000).
CAUTION
CAUTION
In order to spare the pump seals, the pump should not be operated dry.
Therefore ensure that the eluent supply is correctly connected and that
there is enough eluent in the eluent bottle each time before switching
on the pump.
4.5.2 Maintenance
CAUTION
Maintenance work on the high pressure pump may not be carried out
unless the instrument is switched off.
1 Switch off high pressure pump and wait until pressure is released.
2 Loosen the pressure screw on the inlet valve holder (16-6) and
unscrew the pump head input capillary (16-7), the coupling (16-9),
and the eluent aspiration tubing from the pump head.
In the process, eluent will spill. Hold the eluent aspiration tubing up
high and allow the eluent to flow back into the eluent bottle.
3 Unscrew the pump head outlet capillary (16-13) from the pump
head.
4 Remove pump head from the pump housing by loosening the 4 fas-
tening screws (16-5) using the hexagon key (6.2621.030). The main
piston is on the left (viewed from the front), and the auxiliary piston
is on the right.
CAUTION
On the inside of the piston cartridge there is a taut spring than can
jump out of the piston cartridge if suddenly loosing tension.
When opening the piston cartridge, hold pressure towards the
spring and unscrew carefully.
■ Remove the backup ring from the pump head and lay to the other
parts.
1 2 3 4 5 6 7 8
The special tool (6.2617.010) (see figure 35, page 69) is necessary to
remove the piston seal from the pump head. It consists of two parts: a tip
for removing the old piston seal and a sleeve for inserting the new piston
seal.
1
2
1 Pin 2 Sleeve
Tip for removing the old piston seal. Sleeve for inserting the new piston seal.
CAUTION
Screwing the special tool for the piston seal (6.2617.010) into the pis-
ton seal destroys this completely!
CAUTION
Avoid touching the sealing surface in the pump head (16-4) with
the tool.
Screw the special tool for the piston seal (35-1) with the narrow side
just as far into the piston seal as the same can be removed.
1 Removing valves
■ Unscrew the connection capillary for the auxiliary piston (16-1)
from the outlet valve holder.
■ Unscrew the holders for the inlet and outlet valves and remove
the valves (39-3) and (39-2).
1
2
NOTICE
Longer lasting ultrasonic baths can damage the ruby ball of the
valve.
3 Dismantling valve
Dismantle every valve separately.
NOTICE
For dismantling the valve the tool for valve cartridges (6.2617.020)
is required.
■ Place the valve with the seal faced downwards above the recess in
the holder.
■ Push the valve components out of the valve housing using the
needle of the tool.
1 Needle 2 valve
For pushing the valve components out of
the valve housing.
3 Recess 4 Holder
For collecting the valve components.
The components of the valve are collected in the recess of the holder.
NOTICE
The components of the valve are very small. In order not to lose
them, put the components into a dish.
■ The inlet valve and the outlet valve consist of the same, just differ-
ently arranged components (see figure 41, page 74).
1 2
3 4
5 5
6 6
7 9
8 8
9 7
10 10
Figure 41 Components of the inlet valve and outlet valve
CAUTION
■ Insert the inlet valve into the inlet valve holder the way the seal is
visible.
■ Screw the inlet valve holder into the bottom of the pump head
and tighten with a wrench (39-4).
■ Insert the outlet valve into the outlet valve holder the way the seal
is visible.
■ Screw the outlet valve holder into the top of the pump head and
tighten with a wrench (39-1).
NOTICE
To prevent the pump head from being positioned the wrong way, it is
provided with different bore hole depths for the fastening bolts, i. e. a
fastening bolt is longer than all others. The bore hole with the greatest
depth must therefore be assigned to the longest bolt. If this is not the
case, the pump will not function perfectly.
1 Mount the pump head on the pump again using the four fastening
screws (16-5). Firmly tighten the screws with the hexagon key
(6.2621.030).
5 1 2 3 4 1 5
Figure 42 Change filters (of the inline filter)
5 Connection capillaries
NOTICE
4.11.2 Operation
NOTICE
The suppressor units must never be regenerated in the same flow direc-
tion in which the eluent is pumped. Therefore always mount the input
and output capillaries according to diagram outlined in Figure 25, Page
44.
The MSM consists of 3 suppressor units, which are used for suppression,
regenerated with sulfuric acid or rinsed with ultra pure water in rotation.
CAUTION
The MSM must never be switched over in a dry state, as there is a risk
of jamming. If the MSM is in a dry state, the MSM must be rinsed for at
least 5 minutes before it may be switched over.
CAUTION
4.11.3 Maintenance
4.11.3.1 Regenerating the MSM
If the suppressor units are loaded for a longer period with certain heavy
metals (e.g. iron) or organic impurities, these can no longer be completely
removed with the regeneration solution (50 mmol/L H2SO4) normally used.
The capacity of the suppressor units is consequently affected, which can
result in reduced phosphate sensitivity in less serious cases and a signifi-
cant rise in the baseline in more serious cases. If such capacity problems
occur at one or more positions, the suppressor units must be regenerated:
CAUTION
The pump tubing made of PVC must not be used for rinsing with
solutions containing organic solvents. In this case, other pump
tubing must be used for rinsing.
NOTICE
The high pressure pump can be used for regeneration. For this,
remove the guard column and separation column and connect the
capillary directly to the MSM (regenerate in opposite direction).
1 2 3 4
5
Figure 43 MSM – Components
CAUTION
■ Insert the MSM rotor A (43-3) into the MSM housing (43-4) in
such a way that the tubing connections on the rear of MSM rotor
A fit into the corresponding recesses inside the MSM housing and
one of the three holes of the MSM rotor A is visible from below in
the slot of the MSM housing (43-5).
■ If the MSM rotor A (43-3) is correctly inserted, its sealing area will
be approx. 4 mm within the MSM housing (43-4). If this is not the
case, MSM rotor A must be moved into the right position from
below using a sharp object (e.g. screwdriver).
Replace parts of the MSM as follows (see figure 43, page 83):
CAUTION
■ Insert the new MSM rotor A (43-3) in the MSM housing (43-4) in
such a way that the tubing connections on the rear of MSM rotor
A fit into the corresponding recesses inside the MSM housing and
one of the three holes of MSM rotor A is visible from below in the
slot (43-5) of the MSM housing.
■ If the MSM rotor A (43-3) is correctly inserted, its sealing area will
be approx. 4 mm within the MSM housing (43-4). If this is not the
case, MSM rotor A must be moved into the right position from
below using a sharp object (e.g. screwdriver).
CAUTION
The service life of the pump tubings also depends on the contact pres-
sure. Therefore fully lift the tubing cartridges by loosening the snap-
action lever (27-10) on the right-hand side if the peristaltic pump is to
be turned off for a longer period. Once set, the contact pressure
remains unaffected.
CAUTION
4.12.2 Maintenance
4.12.2.1 Pump tubings
Pump tubings used for the peristaltic pump are consumables with a lim-
ited lifetime.
LFL pump tubings with three stoppers are inserted into the tubing car-
tridge in such a way that the cartridge is located between two stoppers.
This results in two possible positions for the tubing cartridge. If the pump
tubing was to show pronounced signs of wear, you can insert it a second
time in the other position.
Replace the pump tubings periodically, approx. every four weeks if used
continuously.
3 Filter housing
4.14.2 Protection
To protect the separation column against foreign particles, which can
affect the separating efficiency, we recommend that both the eluent and
the samples undergo a microfiltration (filter 0.45 µm) before being aspira-
ted via the aspiration filter (6.2821.090).
We recommend always to use a guard column (see chapter 2.21, page
55). This protects the separation column and considerably increases its ser-
vice life. 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 agent), the leaflet provided along
with your separation column, the product information on the separation
column at http://www.metrohm.com (product area Ion Chromatography)
or obtained directly from your agent.
The pulsation absorber (see chapter 2.12, page 35) must be installed in
order to protect the column material from pressure concussion caused by
injection.
4.14.3 Storage
Always store the separation columns sealed and filled according to the
data of the column manufacturer when not using them.
4.14.4 Regeneration
NOTICE
5 Troubleshooting
5.1 Problems and their solutions
Problem Cause Remedy
Marked drop in Leak in the system. Check all capillary connections and seal leaks,
pressure. if necessary (see chapter 2.5, page 13).
The baseline has a High pressure pump – con- Clean pump valves (see chapter 4.5.2, page
large amount of taminated pump valves. 66).
noise.
Eluent – Leakage in eluent Check eluent path.
path.
High pressure pump – Replace (see chapter 4.5.2, page 66) piston
defective piston seals. seals .
Pulsation damper not con- Connect the pulsation damper (see Chapter
nected. 2.12, Page 35).
The baseline is drift- Thermal equilibrium not yet Condition instrument with the column thermo-
ing. attained. stat (see Chapter 2.15, Page 40) switched on .
Leak in the system. Check all capillary connections and seal leaks,
if necessary (see chapter 2.5, page 13).
Eluent – Evaporation of ■ Check the eluent bottle cap (see figure 12,
organic solvent in eluent. page 26).
■ Stir the eluent.
The pressure in the Inline filter (6.2821.120) Replace the filter (6.2821.130) (see chapter
system markedly blocked. 4.6, page 76).
increases.
MSM – blocked. ■ Regenerate the MSM (see chapter
4.11.3.1, page 81).
Guard column – blocked. Replace guard column (see chapter 2.21, page
55).
Injection valve – valve Have the valve cleaned (by Metrohm service
blocked. technicians).
The retention times Separation column – ■ Regenerate separation column (see chapter
in the chromato- diminished separating effi- 4.14.4, page 90).
gram have changed ciency. ■ Replace separation column (see "Connect-
unexpectedly. ing and rinsing the separation column",
page 57).
Peak areas are lower Sample – leak in the sam- Check the sample path.
than expected. ple path.
Sample – gas bubbles in Use sample degasser (see chapter 2.13, page
the sample. 36).
The peristaltic pump Peristaltic pump – contact Correctly set contact pressure (see "Set flow
is pumping too little. pressure too weak. rate", page 50).
Data of the separa- Column chip contami- Clean the contact surfaces of the column chip
tion column cannot nated. (with alcohol).
be read.
Column chip defective. 1. Save column configuration in MagIC Net™.
2. Notify Metrohm Service.
Individual peaks are Sample – carry-over of the Rinse system longer between two samples.
greater than samples from previous
expected. measurement.
Peristaltic pump – filter Replace the filter (see "Replacing the filter",
blocked (see figure 28, page 88).
page 48).
MSM – backpressure too Clean the MSM (see chapter 4.11.3.2, page
high. 82) or replace parts (see chapter 4.11.3.3,
page 85).
Peristaltic pump – pump Replace pump tubing (see figure 27, page 47).
tubing defective.
The background MSM – not connected. Connect the MSM (see chapter 2.16, page
conductivity is too 43).
high.
Wrong eluent. Change the eluent (see chapter 4.4.2.3, page
65).
Extreme spread of Capillary connections – Check connections (see chapter 2.5, page 13)
the peaks in the dead volume in the system. (use PEEK capillaries with an internal diameter
chromatogram. of 0.25 mm between the injection valve and
Splitting (dual detector).
peaks)
Guard column – diminished ■ Replace guard column (see chapter 2.21,
performance. page 55).
Greater rise in the MSM – reduced capacity. Regenerate the MSM (see chapter 4.11.3.1,
baseline page 81).
Precision problems - Sample – gas bubbles in Use sample degasser (see chapter 2.13, page
the measured values the sample. 36).
are highly scattered.
Injection valve – sample Check installation of the sample loop (see
loop. chapter 2.14.1, page 38).
Sample – rinsing volume Increase rinsing time (see chapter 4.8, page
too low. 78).
6 Technical specifications
6.2 Device
IC system ■ Metal-free IC system
■ Compact system with modular design
■ Up to two complete chromatographic systems in one housing
Material Painted polyurethane hard foam without CFCs, fire class V0
Operating pres- ■ 0…50 MPa (500 bar) high pressure pump
sure range ■ 0…35 MPa (350 bar) standard-PEEK system
Intelligent com- iPump, iDetector, iColumn, MagIC Net
ponents
Storage
Ambient tem- –20…+70 °C
perature
Transport
Ambient tem- –40…+70 °C
perature
6.5 Housing
Dimensions
Width 365 mm
Height 642 mm
Depth 380 mm
Material of base Polyurethane hard foam (PUR) with flame retardation for fire class V0,
tray, housing and CFC-free, painted
flask holder
Operating ele-
ments
Indicators LED for power display
On/Off switch On the rear of the instrument
Pressure range
Pump 0…50.0 MPa (0…500 bar)
Pump head 0…35.0 MPa (0…350 bar) (applies for the standard PEEK pump head)
Residual pulsa- <1%
tion
Safety shutdown
Function Automatic shutdown upon reaching the pressure limit values
Maximum pres- ■ Adjustable from 0.1…50 MPa (1…500 bar)
sure limit ■ The pump is automatically shut down at the first piston stroke
above the maximum limit value
Minimum pres- ■ Adjustable from 0…49 MPa (0…490 bar)
sure limit ■ The shutdown mechanism is inactive at 0 MPa
■ The shutdown mechanism only becomes active 2 minutes after sys-
tem start
■ The pump is automatically shut down after 3 piston strokes below
the minimum pressure limit
Temperature ± 0.2 °C
reproducibility
Stability < 0.05 °C
Heating up time < 30 minutes from 20 to 50 °C
Cooling time < 40 minutes from 50 to 20 °C
6.13 Detector
You can find the technical specifications for the detector in the manual for
the detector.
6.15 Interfaces
USB
Entry 1 USB upstream, type B (for connection to the PC)
Exit 2 USB downstream, type A
MSB 2 MSB 8-pin Mini DIN (female) (for Dosino, stirrer, remote lines, etc.)
CAUTION
6.16 Weight
1.850.2010 28.3 kg (without accessories)
1.850.9010 (con- 2.3 kg (with accessories)
ductivity detector)
Transport carriage 1.8 kg
(rollers and han-
dle)
7 Accessories
Up-to-date information on the scope of delivery and optional accessories
for your product can be found on the Internet. You can download this
information using the article number as follows:
2 Enter the article number (e.g. 2.850.2010) into the search field.
The search result is displayed.
NOTICE
Index
(6.2821.130) Filter .................... 76 D Flow rate .................................. 97
6.2821.090 aspiration filter ...... 65 Deaerating Frequency .............................. 100
High pressure pump ........... 32
A Purge valve ......................... 30 G
Ambient conditions .................. 96 Degasser Gas .................................... 28, 36
Aspiration filter 6.2821.090 ...... 65 Eluent degasser .................. 28 Guard column
Aspiration tubing for eluent ...... 24 Sample degasser ................. 36 Installation ......................... 55
Degassing Rinsing ............................... 56
B Eluent ................................. 28
Baseline Detector H
Conditioning ...................... 61 Cable connector ................. 18 Handle ..................................... 15
Unstable ............................. 66 Conductivity detector ......... 51 Heating
Blood ....................................... 78 Interface ........................... 100 see also "Column thermostat"
Positioning ......................... 18 ........................................... 40
C Diagram ................................... 10 Heavy metals
Cable feed-throughs ................. 21 Dilution .................................... 78 Contamination of the MSM 81
Capillaries Dimensions .............................. 97 High pressure pump
Installation ......................... 13 Door ........................................ 64 Installation ......................... 30
Capillary feed-throughs ............. 21 Drainage tubings Maintenance ...................... 65
Carry-over ................................ 78 Installation ......................... 19 Protection .................... 18, 65
Cleaning Technical specifications ....... 97
MSM .................................. 83 E Tubing connection .............. 30
Valves of the high pressure Electrostatic charge .................... 7 Valves ................................. 74
pump ................................. 71 Eluent Housing ................................... 97
Column Aspirate .............................. 24 Humidity .................................. 96
see also "Separation column" Change .............................. 65
........................................... 56 Production .......................... 64 I
Column recognition ................ 100 Eluent bottle IC column
Column thermostat Figure ................................. 27 see also "Separation column"
Column thermostat ............ 99 Installation ......................... 24 ........................................... 56
Installation ......................... 40 Operation ........................... 65 Impurity MSM
Computer connection ............... 53 Eluent degasser Organic .............................. 81
Conditioning ............................ 61 Installation ......................... 28 Initial installation ........................ 9
Conductivity detector Technical specifications ....... 97 Inject
Capillary connection ........... 51 Equilibration ....................... 59, 61 Injection valve .................... 40
Connect Injection valve ............................ 3
Power grid .......................... 54 F Fill ...................................... 40
To computer ....................... 53 Feed-throughs Inject .................................. 40
Connection Capillaries ........................... 21 Installation ................... 38, 98
Mains ............................... 100 Fill Maintenance ...................... 80
Connections Injection valve .................... 40 Protection .......................... 80
Installation ......................... 13 Filter Inline filter ................................ 34
Contamination see also "inline filter" .......... 34 Inline sample preparation ......... 78
High pressure pump ........... 65 Filter (6.2821.130) .................... 76 Installation
Valves in the high pressure Filter 6.2821.090 Column thermostat ............ 40
pump ................................. 66 Aspiration filter ................... 65 Conductivity detector ......... 51
Contamination MSM Flow diagram ........................... 10 Connections ....................... 13
Heavy metals ...................... 81 Flow fluctuations ...................... 66 Drainage tubings ................ 19
Crystallization Flow increment ........................ 97 Eluent bottle ....................... 24
High pressure pump ........... 65 Flow range ............................... 97 Eluent degasser .................. 28